Log in

View Full Version : A review of RDX synthesis.


megalomania
April 26th, 2002, 01:54 PM
I am thinking we need to have some better information about RDX synthesis as there seems to be some disagreement as to how it can be most efficiently done. To that end I have rounded up some references on RDX synthesis for the past few decades. If someone who involves themselves in greater detail than I can give in RDX synthesis, please review this list of references and I will get what is asked for. These are from 1993-2002

Bibliographic Information

Nitric acid decomposition of waste composite propellants for recovery of nitramine components. Warner, Kirstin F.; Cannizzo, Louis F.; Hajik, Robert M.; Johnston, Harold E. (Cordant Technologies Inc., USA). U.S. Pat. Appl. Publ. (2002), 9 pp. CODEN: USXXCO US 20020028971 A1 20020307 Patent written in English. Application: US 2001-784475 20010215. Priority: US 2000-188182 20000310. CAN 136:219170 AN 2002:172521 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
US 2002028971 A1 20020307 US 2001-784475 20010215

Priority Application Information
US 2000-188182P 20000310

Abstract

Nitramines are recovered from waste or unwanted composite nitramine aluminized propellants by: (1) treating the waste propellant with aq. nitric acid (below 55 wt.% HNO3), at a 4-6:1 wt. ratio of HNO3 to waste propellant, to digest the binder into soln. while neither solvating nor solvolyzing into soln. all or most of the nitramine, (2) adding a mineral acid other than nitric acid to the soln. and digesting a portion of the aluminum, and (3) recovering the nitramine. Suitable mineral acids other than nitric acid are selected from hydrochloric acid, perchloric acid, sulfuric acid, phosphoric acid, hydrobromic acid, and hydroiodic acid. Suitable nitramines that can be recovered include RDX, HMX, TEX, 4,10-dinitro-4,10-diaza-2,6,8,12-tetraoxatetracyclo[5.5.0.05,9.0.3,11] dodecane, and CL-20 (HNIW). Treatment of the energetic material can be carried out without the use of volatile org. solvents.

Bibliographic Information

Formation of energetic materials using supercritical fluids. Teipel, Ulrich; Krober, Hartmut; Krause, Horst H. Fraunhofer-Institut fur Chemische Technologie (ICT), Pfinztal, Germany. Propellants, Explosives, Pyrotechnics (2001), 26(4), 168-173. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 136:104697 AN 2001:829487 CAPLUS (Copyright 2002 ACS)

Abstract

A new field of applications of compressed gases is the formation of solid particles with well-defined properties, e.g. the particle size, the particle size distribution, the particle shape, the sp. surface area and free of solvent inclusions. It is possible to process moderately solids like energetic materials which are difficult to comminute due to their sensitivity to mech. or thermal stress. The characteristics of compressed gases allow to vary the morphol. of solid particles in a wide range. A pilot plant is presented, which has been built to prep. fine particles by the rapid expansion of supercrit. solns. (RESS process) and pptn. by a compressed fluid antisolvent (PCA process). The micronization of different energetic materials by the RESS and PCA processes is investigated.

Bibliographic Information

Process for co-manufacturing RDX high explosive and TNT-free emulsified explosive. Bao, Guangyi; Bao, Cuoli. (Peop. Rep. China). Faming Zhuanli Shenqing Gongkai Shuomingshu (2001), 4 pp. CODEN: CNXXEV CN 1293177 A 20010502 Patent written in Chinese. Application: CN 2000-131348 20001102. CAN 135:320150 AN 2001:813474 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
CN 1293177 A 20010502 CN 2000-131348 20001102

Abstract

The process comprises reacting of 10-12 wt. parts HNO3 with 1 wt. part hexamine at below 20° to obtain RDX, charging a mixt. contg. ammonium nitrate and ammonium sulfonate in an amt. of 8-12 wt. parts to the reactant, reacting the mixt. at 70-80°, neutralizing the byproduct (nitrate, H2O, etc.) with CaCO3, Ca(OH)2 or CaO to obtain the aq. phase of TNT-free emulsified explosive, and then reacting with oily phase to obtain TNT-free emulsified explosive.

Bibliographic Information

Study on preparation of ultrafine particle of explosive using technology of direct dilution. Sima, Tianlong; Yan, Jisheng. Gansu Yinguang Chemical industrial Complex, Baiyin, Peop. Rep. China. Huozhayao Xuebao (2001), 24(4), 46-47. CODEN: HUXUFP Journal written in Chinese. CAN 136:234276 AN 2001:804744 CAPLUS (Copyright 2002 ACS)

Abstract

Ultrafine particle of explosive is prepd. by using direct diln. technol. The fundamental principle of the method is introduced. The particle size and distribution of size of ultrafine PETN and RDX are tested.

Bibliographic Information

Study on high-energy LOVA propellant. Liao, Xin; Huang, Zhenya; Yang, Wenbao; Wang, Zeshan. Xi'an Modern Chemistry Research Institute, Xi'an, Peop. Rep. China. Huozhayao Xuebao (2001), 24(4), 8-9, 30. CODEN: HUXUFP Journal written in Chinese. CAN 136:249804 AN 2001:804730 CAPLUS (Copyright 2002 ACS)

Abstract

The formulation of a LOVA propellant was detd. by using RDX as the main energetic compn. with inert and energetic complex binders, complex plasticizers and combustion modifiers. The closed bomb tests showed that the designed formula of the LOVA propellant had the characteristic of high energy and low erosion. The solvent-extrusion process was demonstrated practicable for this type of LOVA propellant formula.

Bibliographic Information

Supercritical fluid technology: a new process on formation of energetic materials. Krober, H.; Reinhard, W.; Teipel, U. Fraunhofer Institut fur Chemische Technologie (ICT), Pfinztal, Germany. International Annual Conference of ICT (2001), 32nd(Energetic Materials), 48/1-48/13. CODEN: IACIEQ ISSN: 0722-4087. Journal written in English. CAN 135:346528 AN 2001:605072 CAPLUS (Copyright 2002 ACS)

Abstract

A novel process for purifn. of energetic solids was developed using compressed inert supercrit. gases (esp. CO2), in which the material can be comminuted to solid particles with well-defined properties (e.g., particle size, size distribution, shape, and sp. surface area) and no fluid inclusions. The particle morphol. can be varied by varying the characteristics of the compressed gases. The RESS (Rapid Expansion of Supercrit. Solns.) uses a loaded supercrit. fluid that is expanded through a nozzle to create a high supersatn. in the jet, in which rapid crystal nucleation and growth occurs. Solids which are insol. in a compressed gas can be processed by using the PCA process (pptn. with a compressed antisolvent). In this process, a soln. consisting of an org. solvent that is completely miscible with the compressed gas, and a solid material dissolved in this solvent is sprayed through a nozzle into a high-pressure vessel filled with a compressed gas. A pilot plant was thus built to prep. fine particles of certain solid explosives (e.g., HNS, TNT, RDX, etc.).

Bibliographic Information

Raman spectroscopy investigation of the effects of precipitation of precursor powders by antisolvents. Case study of RDX powders precipitation. Marlange, L.; Begue, G.; Petitet, J. P.; Jacob, G. Laboratoire D'Ingenierie des Materiaux et des Hautes Pressions, Institut Galilee - Universite Paris XIII, Villetaneuse, Fr. Recents Progres en Genie des Procedes (2001), 15(77, Science et Technologie des Poudres), 61-66. CODEN: RPGPEX ISSN: 1166-7478. Journal written in French. CAN 136:8599 AN 2001:599690 CAPLUS (Copyright 2002 ACS)

Abstract

Based on Raman spectroscopic results, the effect of a CO2 antisolvent (at densities 0.01-0.25 g/cm3) on the precursors of the powders obtained by pptn. was discussed for different solvents (e.g., acetone, Et acetate, or toluene) depending on the solvent swelling capacity. Three results were obsd. in the rapid pptn. of RDX from acetone soln. using crit. CO2 antisolvent: (1) the observable appearance of the ppt. is localized just beyond the max. obsd. Raman intensity, (2) the morphol. of the powder is different at a low pressure or under crit. conditions for CO2, and (3) the appearance of the pptd. powder at low pressure is reversible.

Bibliographic Information

Separation of nitramine and nitroaromatic explosives by capillary liquid chromatography. Goodpaster, John V.; McGuffin, Victoria L. Department of Chemistry, Michigan State University, East Lansing, MI, USA. Journal of Liquid Chromatography & Related Technologies (2001), 24(13), 1965-1978. CODEN: JLCTFC ISSN: 1082-6076. Journal written in English. CAN 135:244590 AN 2001:557131 CAPLUS (Copyright 2002 ACS)

Abstract

This study outlines the successful sepn. of nitrated explosives by using high efficiency capillary liq. chromatog. Careful optimization of sepn. conditions such as mobile phase compn. and temp. was performed by using a window diagram, as well as a more global criterion, the chromatog. resoln. statistic. These efforts resulted in complete baseline resoln. of all 14 components of a std. mixt. of explosives, which has not previously been achieved by using conventional liq. chromatog. This method was then applied to the detn. of hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX), octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazine (HMX), and 2,4,6-trinitrotoluene (2,4,6-TNT) in com.-grade and military-grade explosive samples. As a result, the countries of manuf. of two RDX samples were deduced based on the presence or absence of reaction byproducts.

Bibliographic Information

Explosive properties of reactive mixtures formed during manufacturing of explosives. Buczkowski, Daniel; Gucma, Miroslaw; Pagowski, Witold. Institute of Industrial Organic Chemistry, Warsaw, Pol. Editor(s): Zeman, Svatopluk. New Trends in Research of Energetic Materials, Proceedings of the Seminar, 4th, Pardubice, Czech Republic, Apr. 11-12, 2001 (2001), 29-33. Publisher: University of Pardubice, Pardubice, Czech Rep CODEN: 69BKIC Conference written in English. CAN 135:228922 AN 2001:476831 CAPLUS (Copyright 2002 ACS)

Abstract

Explosive properties of mixts. formed in manuf. of PETN and RDX are presented. Deposits of PETN and RDX in nitric acid filling voids between crystals have detonation abilities similar to typical brisant explosives. Such deposits are formed if mixing is stopped. Soln. of RDX and slurry of PETN in nitric acid have weaker explosive properties, but are dangerous from the point of view of explosion. A problem of minimizing the possibility of damage of mixing equipment or electricity loss must be anticipated during designing producing plants for the manuf. of explosives.

Bibliographic Information

The sensitivity of explosives. McCrone, Walter C. McCrone Associates, Inc., Chicago, IL, USA. Microscope (2001), 49(1), 47-48. CODEN: MICRAD ISSN: 0026-282X. Journal written in English. CAN 135:109344 AN 2001:363793 CAPLUS (Copyright 2002 ACS)

Abstract

The sensitivity of HMX (e.g., as a byproduct of the manuf. of RDX) posses 4 known polymorphs, and, in one form (designated HMX 1, in the bipyramidal polymorph) is relatively insensitive. Phys. deformation (e.g., induced by rapid crystn.) results in a marked increase in sensitivity of HMX 1. HMX in general is subject to crystal strain if crystd. rapidly or ground to finer crystals, which can increase sensitivity, make the total batch have variable sensitivity, and can cause occasional unexpected explosions. This effect of crystal strain on sensitivity was also obsd. for TNT and lead azide, although no quant. relationship was examd.

Bibliographic Information

Study on the crystal size control of RDX. Liu, Han-bin; Yeh, Tsao-fa; Hu, Cheng-ching; Shieh, Chow-yang; Wang, Shan-guang. Department of Applied Chemistry, Chung Cheng Institute of Technology, National Defense University, Ta-hsi, Taoyuan, Taiwan. Huoyao Jishu (2001), 17(1), 41-51. CODEN: HJISE2 ISSN: 1013-767X. Journal written in Chinese. CAN 135:7561 AN 2001:312660 CAPLUS (Copyright 2002 ACS)

Abstract

RDX is probably the most important high brisance explosive and has wide applications. The performances of explosive depend on the crystal size distribution of RDX. The crystal size control is studied by using the characteristic of RDX dissoln. in concd. nitric acid. Based on the process flow conditions of RDX prodn. in the 203rd Arsenal Combined Service Force, the temp., concn. and residence time are selected as control parameters to conduct the expts. Thus it provides the better conditions of product and enables to obtain higher yield of target crystal size with the redn. of the quantity of outside target range of RDX.

Bibliographic Information

Study of the optimal reactor design in the manufacture process of RDX. Luo, Kuo-ming; Lin, Sheann-huei; Chang, Jih-guang; Chu, Kuang-shing. Department of Applied Chemistry, Chung Cheng Institute of Technology, National Defense University, Ta-hsi, Taoyuan, Taiwan. Huoyao Jishu (2001), 17(1), 21-32. CODEN: HJISE2 ISSN: 1013-767X. Journal written in Chinese. CAN 135:7560 AN 2001:312659 CAPLUS (Copyright 2002 ACS)

Abstract

The RDX is produced by the chem. reaction of Hexamine and nitric acid in three CSTRs of vol. of 112.5 L. A correlation is given for the calcn. of the reaction rate. To det. the optimal reactor design. The reaction temp. and fractional conversion are added to det. the optimum reactor design. The highest yield of the RDX is obtained at const. feeding ratio and const. reaction temp. range. The results enable to improve the RDX prodn. at optimum reaction temp. and flow rate.

Bibliographic Information

Preparation of nanometer RDX in situ by solvent substitution effect in reverse micelles. Liu, Dabin; Xu, Dong; Zhao, Baochang; Peng, Jinhua; Gao, Yaolin; Fan, Qinwen. Nanjing University Science Technology, Nanjing, Peop. Rep. China. Proceedings of the International Pyrotechnics Seminar (1999), 26th 269-275. CODEN: PPYSD7 ISSN: 0270-1898. Journal written in English. CAN 134:313266 AN 2001:294122 CAPLUS (Copyright 2002 ACS)

Abstract

A new method to prep. ultrafine explosive through solvent substitution effect in reverse micelles was introduced. The max. soly. of DMF, DMSO, and its RDX soln. in NaAOT-isooctane reverse micelles were detd. The cylinder model RDX crystallites with their diam. of 70-100 nm were prepd. in situ in the NaAOT-isooctane reverse micelle system.

Bibliographic Information

Manufacture of finely dispersed explosives by crystallization from supercritical fluids. Teipel, Ulrich; Krause, Horst; Krober, Hartmut; Forter-Barth, Ulrich. (Fraunhofer-Gesellschaft zur Forderung der Angewandten Forschung e.V., Germany). Eur. Pat. Appl. (2001), 13 pp. CODEN: EPXXDW EP 1090894 A1 20010411 Designated States R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO. Patent written in German. Application: EP 2000-121747 20001005. Priority: DE 99-19948133 19991006. CAN 134:282927 AN 2001:261086 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
EP 1090894 A1 20010411 EP 2000-121747 20001005
R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO

Priority Application Information
DE 1999-19948133 19991006

Abstract

An explosive is dissolved in an org. solvent, a supercrit. fluid, which is miscible or partially miscible with the solvent and in which the explosive is insol. or slightly sol., is injected in the form of a jet flow into the soln., the solvent is collected during crystn. of the explosive particles from the supercrit. fluid, and the explosive particles are sepd. after expansion into a subcrit. state. Preferably, the soln. is injected into the supercrit. fluid by means of a complex nozzle or at least 1 nozzle channel of the complex nozzle, and the supercrit. fluid is fed by means of another nozzle channel.

Bibliographic Information

Effect of entropy on the formation of circular nitramine. Fang, Yi; Yongping, Pan. Nanjing, Peop. Rep. China. Proceedings of the International Pyrotechnics Seminar (1999), 26th 578-582. CODEN: PPYSD7 ISSN: 0270-1898. Journal written in English. CAN 134:268397 AN 2001:115917 CAPLUS (Copyright 2002 ACS)

Abstract

Linear nitramines of TDA, BSX and ACAN were used to compose RDX directly in the soln. of ammonium nitrate - nitric acid. The reaction mechanism is discussed. Eight-member ring nitramine was composed difficultly. The effect of entropy was an important factor.

Bibliographic Information

Synthesis and nitration of condensation products of sulfamates with aliphatic amines and formaldehyde. Tartakovsky, V. A.; Ermakov, A. S.; Sigai, N. V.; Vinogradov, D. B. N. D. Zelinsky Institute of Organic Chemistry, Russian Academy of Sciences, Moscow, Russia. Russian Chemical Bulletin (Translation of Izvestiya Akademii Nauk, Seriya Khimicheskaya) (2000), 49(6), 1082-1085. CODEN: RCBUEY ISSN: 1066-5285. Journal written in English. CAN 134:4920 AN 2000:700624 CAPLUS (Copyright 2002 ACS)

Abstract

A method for the synthesis of 5-alkyl-1,3-dinitro-1,3,5-triazacyclohexanes and linear polynitramines was proposed. It includes the reaction of aliph. amines with sulfamates and formaldehyde and nitration of the reaction products. The yield and compn. of nitramino derivs. depend on the conditions of the condensation and nitration.

Bibliographic Information

Crystallization of explosives and high-energy oxidizers in presence of ultrasound. Veltmans, Wilhelmina H. m.; Wierckx, Franciscus J. m. (Aerospace Propulsion Products B.V., Neth.). Eur. Pat. Appl. (2000), 13 pp. CODEN: EPXXDW EP 1033357 A1 20000906 Designated States R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO. Patent written in English. Application: EP 99-200592 19990302. CAN 133:195590 AN 2000:626476 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
EP 1033357 A1 20000906 EP 1999-200592 19990302
R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO
NO 2000001017 A 20000904 NO 2000-1017 20000229

Priority Application Information
EP 1999-200592 19990302

Abstract

Cryst. energetic materials with improved stability and/or decreased sensitivity are prepd. by crystn. with stirring at 15-75° in the presence of ultrasound with frequency 10-100 kHz and amplitudes of 0.4-10 m. The energetic materials that can be prepd. in this manner are explosives and high-energy oxidizers, esp. hydrazinium nitroformate, CL-20, ADN, AP, RDX, HMX, and PETN.

Bibliographic Information

Simple method for labeled conjugate production using N-hydroxysuccinimide and phase changes to control the reaction. Morseman, John P.; Zeng, Xiangfei. (Martek Biosciences Corporation, USA). PCT Int. Appl. (2000), 35 pp. CODEN: PIXXD2 WO 0043784 A1 20000727 Designated States W: AE, AL, AM, AT, AU, AZ, BA, BB, BG, BR, BY, CA, CH, CN, CR, CU, CZ, DE, DK, DM, EE, ES, FI, GB, GD, GE, GH, GM, HR, HU, ID, IL, IN, IS, JP, KE, KG, KP, KR, KZ, LC, LK, LR, LS, LT, LU, LV, MA, MD, MG, MK, MN, MW, MX, NO, NZ, PL, PT, RO, RU, SD, SE, SG, SI, SK, SL, TJ, TM, TR, TT, TZ, UA, UG, US, UZ, VN, YU, ZA, ZW, AM, AZ, BY, KG, KZ, MD, RU, TJ, TM. Designated States RW: AT, BE, CH, CY, DE, DK, ES, FI, FR, GB, GR, IE, IT, LU, MC, NL, PT, SE, BF, BJ, CF, CG, CI, CM, GA, ML, MR, NE, SN, TD, TG. Patent written in English. Application: WO 2000-US1350 20000121. Priority: US 99-116689 19990122. CAN 133:101746 AN 2000:513898 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
WO 2000043784 A1 20000727 WO 2000-US1350 20000121
W: AE, AL, AM, AT, AU, AZ, BA, BB, BG, BR, BY, CA, CH, CN, CR, CU, CZ, DE, DK, DM, EE, ES, FI, GB, GD, GE, GH, GM, HR, HU, ID, IL, IN, IS, JP, KE, KG, KP, KR, KZ, LC, LK, LR, LS, LT, LU, LV, MA, MD, MG, MK, MN, MW, MX, NO, NZ, PL, PT, RO, RU, SD, SE, SG, SI, SK, SL, TJ, TM, TR, TT, TZ, UA, UG, US, UZ, VN, YU, ZA, ZW, AM, AZ, BY, KG, KZ, MD, RU, TJ, TM
RW: GH, GM, KE, LS, MW, SD, SL, SZ, TZ, UG, ZW, AT, BE, CH, CY, DE, DK, ES, FI, FR, GB, GR, IE, IT, LU, MC, NL, PT, SE, BF, BJ, CF, CG, CI, CM, GA, GN, GW, ML, MR, NE, SN, TD, TG
EP 1145007 A1 20011017 EP 2000-903358 20000121
R: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LI, LU, NL, SE, MC, PT, IE, SI, LT, LV, FI, RO

Priority Application Information
US 1999-116689P 19990122
WO 2000-US1350 20000121

Abstract

The present invention relates to methods for coupling labels to particular target moieties. The coupling reactions of the present invention use temporal spacing of the reactants through phase change (i.e. by rapid freezing) to control the initiation and termination of reaction. This process results in a simplified and improved method for linking labels to specific binding moieties using N-hydroxysuccinimide chem. The present invention further relates to kits comprising all necessary components to easily and rapidly make protein conjugates. Phycoerythrin was conjugated to streptavidin via EDAC/sulfo-NHS from a freeze dried reagent where D-(+)-trehalose was used.

Bibliographic Information

Application of solid-phase microextraction to the recovery of explosives and ignitable liquid residues from forensic specimens. Furton, K. G.; Almirall, J. R.; Bi, M.; Wang, J.; Wu, L. Department of Chemistry and International Forensic Research Institute, Florida International University, Miami, FL, USA. Journal of Chromatography, A (2000), 885(1+2), 419-432. CODEN: JCRAEY ISSN: 0021-9673. Journal written in English. CAN 133:203913 AN 2000:436513 CAPLUS (Copyright 2002 ACS)

Abstract

Solid-phase microextn. (SPME) was applied to the anal. of ignitable liqs. and explosive residues and the relative effects of controllable variables were studied. Variables discussed include fiber chem., adsorption and desorption temps., extn. and desorption times, fiber sampling placement (direct, headspace, and partial headspace) and matrix effects, including water content. SPME is shown to be an inexpensive, rapid and sensitive method for the anal. of ignitable liqs. and high explosives residues from solid debris samples and from aq. samples. Explosives are readily detected at parts per trillion concns. and ignitable liqs. are reproducibly detected at levels below those using conventional methods.

Bibliographic Information

Preparation of Grade III RDX by crystallization in nitric acid. Ye, Ling; Wang, Jian-long; Ye, Yu-peng. Capital University of Medical Science, Beijing, Peop. Rep. China. Hanneng Cailiao (2000), 8(1), 46-48. CODEN: HACAFQ ISSN: 1006-9941. Journal written in Chinese. CAN 132:349813 AN 2000:372246 CAPLUS (Copyright 2002 ACS)

Abstract

The prepn. of RDX of grade III is controlled by the nucleation temp., the interval of heat preservation, and the rate of stepwise diln. with water during the crystn. process in nitric acid. The exptl. results show that reducing the acidity and controlling the granularity of the final product are keys to the technol. for crystn. of RDX in strong acid medium.

Bibliographic Information

Recovering nitroamines from energetic pyrotechnic materials and reformulation of by-products. Phillips, Randall S.; Cain, Andrew W.; Schilling, Thomas J.; Miks, Michael W. (TPL, Inc., USA). U.S. (2000), 5 pp. CODEN: USXXAM US 6063960 A 20000516 Patent written in English. Application: US 98-212050 19981215. Priority: US 97-69492 19971215. CAN 132:323300 AN 2000:323256 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
US 6063960 A 20000516 US 1998-212050 19981215

Priority Application Information
US 1997-69492P 19971215

Abstract

A method for recovering nitroamines from energetic pyrotechnic materials yielding usable byproducts and no waste comprises solubilizing an energetic pyrotechnic material (such as surplus energetic material plastic binder) in a nitric acid soln., (b) removing an effluent from the soln. to leave a nitroamine (such as cyclotetramethylene tetranitramine), (c) neutralizing the effluent with a base, (d) removing liq. content from the effluent to yield a compd. salt, (e) rinsing the nitroamine and (f) desensitizing the nitroamine.

Bibliographic Information

Supercritical fluid extraction of triple-base and LOVA gun propellants. Morris, Jeffrey B. U. S. Army Research Laboratory AMSRL-WM-BD, Aberdeen Proving Ground, MD, USA. CPIA Publication (1999), 687(JANNAF 28th Propellant Development & Characterization and 17th Safety & Environmental Protection Subcommittee Joint Meeting, Vol. 1, 1999), 331-340. CODEN: CPPUDT ISSN: 0272-5118. Journal written in English. CAN 132:267179 AN 2000:256920 CAPLUS (Copyright 2002 ACS)

Abstract

Two supercrit. fluid extn. (SFE) studies are carried out on low-vulnerability ammunition (LOVA) and triple-base gun propellants. The extn. of RDX from ground LOVA gun propellant is carried out using dynamic SFE conditions with acetonitrile and dimethylsulfoxide modifiers for carbon dioxide (CO2). The results of this study are compared to the previous work on static SFE of bulk LOVA propellant. The extn. of nitroglycerin (NG) from M30 gun propellant is investigated with unmodified CO2, using both bulk and ground propellant. In addn., the soly. of NG is also measured under isothermal conditions at 40°. For both types of propellants, substantial matrix effects are encountered for the extn. of RDX or NG from the bulk propellant sample.

Bibliographic Information

Preparation of ultra-fine explosive HMX and RDX using high-speed impinging streams. Zhang, Xiaoning; Xu, Gengguang; Wang, Tingzeng. Department of Engineeing Safty, Beijing Institute of Technology, Beijing, Peop. Rep. China. Beijing Ligong Daxue Xuebao (1999), 19(5), 646-650. CODEN: BLXUEV ISSN: 1001-0645. Journal written in Chinese. CAN 132:51962 AN 1999:815237 CAPLUS (Copyright 2002 ACS)

Abstract

A method for prepg. ultra-fine HMX and RDX and their technol. factors affecting the prepn. are described. High-speed impinging streams of suspending liq. were used. The particles of HMX and RDX can be crushed into sub-micron effectively by high-speed impinging streams method. The effective particle diam. is 612.2 nm and the particle size distribution is 236.5.apprx.1286.0 nm. The pressures and times of processing are the main factors that affect the particle sizes and particle size distribution. The most important factor affecting the degree of crush is the pressure. The times of processing affect the mean particle diam. and the particle size distribution, not the crushing lower limit.

Bibliographic Information

Method for the recovery of secondary explosives from 2,4,6-trinitrotoluene-containing explosive compositions. Spencer, Arthur F.; Hartline, David F. (United States Dept. of the Air Force, USA). U.S. (1999), 4 pp. CODEN: USXXAM US 5977354 A 19991102 Patent written in English. Application: US 98-211491 19981215. CAN 131:288483 AN 1999:705051 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
US 5977354 A 19991102 US 1998-211491 19981215

Abstract

Secondary explosive materials, particularly nitramines, are recovered from an explosive compn. contg. a mixt. of 2,4,6-trinitrotoluene (I) and at least one secondary explosive(s) by heating the explosive compn. to melt the I (preferably using steam), sep. collecting and recovering the melted I, treating the sepd. secondary explosive (e.g., octahydro-1,3,5,7-tetranitro-1,3,5,7-Tetrazocine; i.e., HMX) with a material which is a solvent for I and a nonsolvent for the secondary explosive (e.g., toluene) to dissolve the TNT, removing the nonsolvent from the secondary explosive, and recovering the secondary explosive.

Bibliographic Information

A molecular modeling study of the solvent effect on the RDX crystal morphology. ter Horst, J. H.; Geertman, R. M.; van der Heijden, A. E.; van Rosmalen, G. M. Laboratory for Process Equipment, Delft University of Technology, Delft, Neth. International Symposium on Industrial Crystallization, 14th, Cambridge, United Kingdom, Sept. 12-16, 1999 (1999), 1973-1984. Publisher: Institution of Chemical Engineers, Rugby, UK CODEN: 68IRAJ Conference written in English. CAN 132:37699 AN 1999:704681 CAPLUS (Copyright 2002 ACS)

Abstract

The choice of solvent has a large effect on the crystal morphol. of RDX explosive. Mol. dynamics simulations of a solvent layer of g-butyrolactone upon the {200} and {210} RDX crystal surfaces were performed to obtain a better understanding of the behavior of solvent mols. near a crystal surface. The av. potential energy of the solvent mols. near the surfaces was higher than in the solvent bulk. The surface induces a potential energy change in the solvent layer. This surface-induced potential energy change might be an adequate solvent effect parameter to use in the prediction of the morphol. importance of a crystal surface. From the calcd. surface-induced potential energy changes, it follows that the {210} face is morphol. more important than the {200} surface. This agreed well with the obsd. exptl. RDX morphol. grown in the solvent g-butyrolactone.

Bibliographic Information

Antisolvent crystallization of the explosive compound RDX. ter Horst, J. H.; Geertman, R. M.; van der Heijden, A. E.; van Rosmalen, G. M. Laboratory for Process Equipment, Delft University of Technology, Delft, Neth. International Symposium on Industrial Crystallization, 14th, Cambridge, United Kingdom, Sept. 12-16, 1999 (1999), 1960-1972. Publisher: Institution of Chemical Engineers, Rugby, UK CODEN: 68IRAJ Conference written in English. CAN 132:37698 AN 1999:704678 CAPLUS (Copyright 2002 ACS)

Abstract

RDX crystals were produced by antisolvent crystn. with either acetone or g-butyrolactone as the solvent and water as the antisolvent. Prodn. rates up to 38 g/L-h with acetone and 96 g/L-h with g-butyrolactone were achieved at a residence time of .apprx.30 min. The single crystals have a rather large av. size for such an antisolvent crystn. process. Attrition of the larger crystals reduces the quality of the crystals. In addn. to unagglomerated single crystals, the product contained a considerable amt. of agglomerated crystals.

Bibliographic Information

Preparation of ultra-fine nitroamine explosives by using high-speed impinging stream. Zhang, Xiao-Ning; Xu, Geng-Guang; Wang, Ting-Zeng. Beijing Institute of Technology, Beijing, Peop. Rep. China. Hanneng Cailiao (1999), 7(3), 97-99,102. CODEN: HACAFQ ISSN: 1006-9941. Journal written in Chinese. CAN 131:339045 AN 1999:689401 CAPLUS (Copyright 2002 ACS)

Abstract

The sub-micron ultra-fine particles of nitroamine explosives (HMX and RDX) were prepd. by using high-speed impinging stream. The fundamental principle and characteristic of this method were analyzed. The granularity and shape of the ultra-fine explosive particles obtained were tested with laser-sedimentograph and scanning electronic microscope.

Bibliographic Information

Crystallization and characterization of energetic materials. Van der Heijden, A. E. D. M. TNO Prins Maurits Laboratory, Research Group Pyrotechnics and Energetic Materials, Rijswijk, Neth. Current Topics in Crystal Growth Research (1998), 4 99-114. CODEN: CTCRFJ Journal; General Review written in English. CAN 131:259565 AN 1999:646019 CAPLUS (Copyright 2002 ACS)

Abstract

A review, with 85 refs., of the general aspects of crystn. of energetic materials, esp. explosives and oxidizers, driven by the need to develop less-sensitive materials. Topics discussed include soly., nucleation and crystal growth mechanisms, layer growth, rough growth, crystn. techniques (e.g., melt, cooling, evaporative, pptn., drowning out, supercrit., and quasi-emulsion crystn.), prediction of crystal shape, plastic explosives, formation of inclusions and dislocations, examples of crystn. of energetic materials, polymorphism, crystal size distribution, particle shape, crystal perfection, purity, thermal stability, and hazard properties of crystd. explosives. Compds. discussed include ammonium nitrate, TNT, RDX, HMX, hydrazinium nitroformate, hexanitrostilbene, HNIW, and NTO.

Bibliographic Information

Fluid extraction with supercritical carbon dioxide for recovery of TNT from high explosives. Morris, Jeffrey B. (United States Dept. of the Army, USA). U.S. (1999), 10 pp. CODEN: USXXAM US 5953679 A 19990914 Patent written in English. Application: US 97-840779 19970416. CAN 131:186997 AN 1999:582734 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
US 5953679 A 19990914 US 1997-840779 19970416

Abstract

TNT is recovered from high explosives contg. TNT by supercrit. fluid extn. with CO2 at a temp. above the m.p. of TNT, preferably at .apprx.85° and .apprx.37.4 MPa. The TNT can be recovered from such TNT-contg. explosives as Compn. B, Compn. B3, Cyclotol, Octol, Tritonal, and Torpex, in which a warhead to be decommissioned is held in an inverted position, and supercrit. CO2 is led through channels in the warhead. RDX can often be recovered as a CO2-insol. fraction.

Bibliographic Information

Solubility Determination of TNT and Wax and Their Fractionation from an Explosive Material Using a Supercritical Fluid. Ashraf-Khorassani, Mehdi; Taylor, Larry T. Department of Chemistry, Virginia Polytechnic Institute and State University, Blacksburg, VA, USA. Journal of Chemical and Engineering Data (1999), 44(6), 1254-1258. CODEN: JCEAAX ISSN: 0021-9568. Journal written in English. CAN 131:301221 AN 1999:574255 CAPLUS (Copyright 2002 ACS)

Abstract

The solubilities of 2,4,6-trinitrotoluene (TNT) and wax were measured in supercrit. carbon dioxide (CO2) under nine static conditions of pressure (13.8, 25.0, and 37.9 MPa) and temp. (35, 50, and 70°). The concns. of each component were detd. off-line via UV (TNT) and evaporative light scattering (wax) detection. The soly. of TNT was an order of magnitude higher than that of wax. Gas chromatog. assay of the wax ext. revealed that only the lower mol. wt. components dissolved. Fractionation of the TNT and wax from an explosive material (Compn. B, contg. 59.5 wt.% RDX and 39.5 wt.% TNT) was attempted by making incremental increases in CO2 d. Although TNT and wax could be easily isolated from RDX, attempts to sep. TNT from wax were not totally successful. More specifically, the initial fractions contained lower mol. wt. wax components in addn. to major amts. of TNT. Since the percentage of TNT was .apprx.50 times the amt. of wax, later fractions were 100% TNT, although most of the TNT was removed at the lower densities.

Bibliographic Information

Recovery of acetic acid from spent liquor of cyclotetramethylene tetranitramine plant. Rajopadhye, M. V.; Hima, P. R.; Syal, R. K. Materials Research Laboratory, Pune, India. Chemical Engineering World (1999), 34(5), 81-86. CODEN: CEWOF5 Journal written in English. CAN 131:189044 AN 1999:520590 CAPLUS (Copyright 2002 ACS)

Abstract

A technol. for wastewater treatment and recovery of acetic acid from the effluent of the explosive cyclotetramethylene tetranitramine (HMX) plant was developed. At pH 2.8, HNO3, present in the spent liquor, is completely neutralized. The dild. acetic acid is recovered (greater than 85%) in a single-stage distn. under reduced pressure. The residues contg. all impurities including the explosives RDX/HMX are sepd. by cooling and filtration. Diln. of the residues with water enhances the pptn. of the explosives. From the safety point of view and for efficient recovery, spent liquors with higher acid concn. must be dild. to acetic acid concns. of .apprx.25-30% by water addn. prior to distn. A pilot plant with a capacity of 2000 L/day effluent is in operation.

Bibliographic Information

Recycling of nitramines at Bofors Explosives AB. Sjoberg, Per. Bofors Explosives AB, Karlskoga, Swed. Editor(s): Johansson, Stig R. Proceedings of the International Disposal Conference, 1st, Lund, Swed., Nov. 12-13, 1997 (1999), Meeting Date 1997, 133-136. Publisher: Sektionen foer Detonik och Foerbraenning, Combustion Institute, Billdal, Swed CODEN: 67YNAC Conference written in English. CAN 131:161104 AN 1999:502652 CAPLUS (Copyright 2002 ACS)

Abstract

Bofors Explosives has reclaimed 50 tonnes of nitramines from destroyed ammunition. The process was developed and is patented by Bofors Explosives. All worked-up nitramines have been reused in com. applications where otherwise freshly synthesized nitramines would have been used. The work-up process produces nitramine which is pure and chem. and phys. indistinguishable from freshly synthesized ones. The operation could be scaled up considerably if the recycled nitramines are accepted by the military for use in new ammunition. The military require freshly synthesized nitramines.

Bibliographic Information

Study on preparation of ultrafine particle of explosive by high-speed impinging stream technology. Zhang, Xiaoning; Wang, Weimin; Xu, Gengguang. Department of Mechanical and Electronic Engineerig, Beijing Institute of Technology, Beijing, Peop. Rep. China. Huozhayao Xuebao (1999), 22(3), 1-3. CODEN: HUXUFP Journal written in Chinese. CAN 131:172278 AN 1999:464551 CAPLUS (Copyright 2002 ACS)

Abstract

The prepn. of sub-micron ultrafine particle of explosive by high-speed impinging stream technol. was studied. The particle sizes of ultrafine HMX and RDX were detd.

Bibliographic Information

Mannich condensation reactivity of DPT nitrolysis fragments. Zhang, Yuejun; Zhou, Weilian; Wen, Jinquan. School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing, Peop. Rep. China. Proc. Int. Pyrotech. Semin. (1997), 23rd 999-1007. CODEN: PPYSD7 ISSN: 0270-1898. Journal written in English. CAN 130:298956 AN 1999:154372 CAPLUS (Copyright 2002 ACS)

Abstract

The two kinds of different nitrogen atoms of amino groups in DPT (dinitropentamethylenetetramine) mol. had been labeled with 15N atoms, resp., in order to distinguish Mannich reactivity of fragments formed in DPT nitrolysis process. The nitrolysis fragments produced in DPT nitrolysis process could condense with urea or nitrourea to form product Keto-RDX. With the aid of mass spectrum isotope anal., the isotope distribution and abundance of 15N tracer atoms in product Keto-RDX and reactant DPT could be detd. The research results showed: nitrogen atoms of the trimethylene amino groups in DPT mol. appeared 100% in the 4 position in product Keto-RDX mol., but nitrogen atoms of the nitroamino groups in DPT mol. disappeared completely in the product Keto-RDX mol.

Bibliographic Information

Studies on the mechanism of synthesizing Keto-RDX in direct preparation method. Zhang, Yuejun. School of Chemical Engineering, Nanjing University of Science and Technology (NUST), Nanjing, Peop. Rep. China. Proc. Int. Pyrotech. Semin. (1997), 23rd 987-998. CODEN: PPYSD7 ISSN: 0270-1898. Journal; General Review written in English. CAN 130:298931 AN 1999:154371 CAPLUS (Copyright 2002 ACS)

Abstract

A review with 19 refs. of the recent progresses of mechanistic researches of synthesizing Keto-RDX in direct prepn. method using urotropine and urea as reactants were systematically described in this paper. The evidences of reaction forms of urotropine and urea in the reaction to form resultant Keto-RDX were presented in several aspects: the active intermediates, the relationships between intermediate structures and reactivities, and the 15N trace atoms, etc.. The nitrolysis fragments N,N-dimethylolamines and their imine cations formed during the urotropine nitrolysis process were active intermediates from urotropine. And the product of nitrating urea or nitrourea, N,N'-dinitrourea also was an active intermediate. Keto-RDX was synthesized via Mannich condensation of the above active intermediates in strong acidic media.

Bibliographic Information

Missile system reclamation and recycling. Melvin, William S.; Freeman, Charles W.; Wright, Jeffrey S. U.S. Army Aviation and Missile Command (AMCOM) Missile Research, Development, and Engineering Center Propulsion and Structures Directorate, AMSAM-RD-PS-R, Redstone Arsenal, AL, USA. CPIA Publ. (1998), 674(Vol. 1, 1998 JANNAF Propellant Development & Characterization Subcommittee and Safety & Environmental Protection Subcommittee Joint Meeting, Vol. 1), 411-421. CODEN: CPPUDT ISSN: 0272-5118. Journal written in English. CAN 130:200413 AN 1999:80588 CAPLUS (Copyright 2002 ACS)

Abstract

This report describes the implementation, testing, and evaluation of environmentally friendly procedures and processes for complete missile system demilitarization and recycling of recovered ingredients and hardware components. Redstone Arsenal facilities and AMCOM developed technologies to support these efforts. The vast majority of the Army missile systems are full up rounds. The demilitarization approach addresses the entire missile system. Loaded rocket motors and cases are considered a subset of the total missile system. Warheads, rocket motors, guidance and control packages, shipping containers, and launch tubes will all be recycled. In contrast to missile system destruction approaches, where neither products nor assocd. values are recovered, this Army initiative includes both military and com. market reuse options for deriving max. product values of reclaimed ingredients and components. The AMCOM liq. ammonia-based, ingredient extn. and reclamation process for rocket propellant recycling has been integrated into a Missile System Recycling Facility at Redstone Arsenal. This propellant reclamation technol. has successfully completed full scale, class 1.3 MLRS and class 1.1 Hellfire rocket motor recycling demonstrations. The fully operational AMCOM pilot plant validated the closed-loop reclamation process by efficiently extg. and recovering 100% of the ammonium perchlorate (AP) and aluminum/binder from the MLRS propellant. This pilot facility fully achieved its design requirements. Test demonstrations confirmed the operational capability to process greater than 200 lb of AP composite propellant from a full scale MLRS rocket motor in a single batch. Pilot demonstrations have validated its operational capability by the processing of 100 lb batches of nitrate ester plasticized, HMX/RDX nitramine propellant from Hellfire rocket motors. Complete missile system recycling demonstrations using 60 TOW missiles are in progress. Pilot demonstration efforts have confirmed that strategically valuable fuel and oxidizer ingredients (such as HMX, RDX, AP, aluminum/rubber binder) can be safely and efficiently recovered from Army tactical rocket motors. The AMCOM missile system recycling technol. is directly applicable to the vast majority of rocket motors in the Army, other DoD, and foreign missile inventories. With emphasis on reclamation instead of destruction, the liq. ammonia process is a near-optimal soln. for environmentally sound rocket motor disposition.

Bibliographic Information

A fiber optic biosensor for multianalyte detection: importance of preventing fluorophore aggregation. Bakaltcheva, Irina B.; Shriver-Lake, Lisa C.; Ligler, Frances S. Geo-Centers, Incorporated, Rockville, MD, USA. Sens. Actuators, B (1998), B51(1-3), 46-51. CODEN: SABCEB ISSN: 0925-4005. Journal written in English. CAN 130:211443 AN 1998:815678 CAPLUS (Copyright 2002 ACS)

Abstract

Individual assays for the detection of the explosives RDX and TNT with a fiber-optic biosensor were developed. In order to develop an assay for simultaneous detection of RDX and TNT, a mixt. of the fluorescent-labeled analogs Cy5-EDA-RDH (hapten) and Cy5-EDA-TNB used in the individual assays was passed over the sensor that used anti-RDX and anti-TNT fiber probes connected in series. There was an increased total fluorophore concn. in the mixt., which resulted in a significant increase in the normalized signal compared to that produced by a single fluorophore. Aggregation of the amphiphilic fluorophores in the mixt. on the surface of the fiber optic probe was a possible reason for the obsd. effect. The use of nonionic (Tween 20) and ionic detergents (deoxycholic acid) to block aggregate formation and to allow detn. of RDX and TNT was examd. Use of the ionic detergent deoxycholic acid can help prevent fluorophore aggregation.

Bibliographic Information

Recovery/reuse of energetics from military munitions. Burch, Dan; Griggs, John; Johnson, Mike; Sims, Keith. Naval Surface Warfare Center, Crane Division (Code 4073), Crane, IN, USA. Proc. Int. Pyrotech. Semin. (1998), 24th 101-112. CODEN: PPYSD7 ISSN: 0270-1898. Journal; General Review written in English. CAN 129:278152 AN 1998:574325 CAPLUS (Copyright 2002 ACS)

Abstract

A review, with 8 refs., of methods for recovery and reuse of propellants and explosives from military munitions. Disassembly technol. using an abrasive waterjet was developed by the University of Missouri-Rolla (UMR) which can cut through projectiles and other munition items. Testing was performed using an abrasive slurry waterjet to cut the tracers and fuses off of Navy 40mm projectiles in order to reclaim the TNT. In addn., UMR has developed high-pressure water technol. to remove explosives and high-energy propellants from projectiles, warheads, and rocket motors. Other removal technologies being explored are microwave melt out and induction heating. Several projects are underway to process the reclaimed explosive from the waterjet washout process and other removal processes. This includes the mech. reprocessing of the PBXN-106 into two sep. explosive products, a dimensional stone mining explosive, boosters for insensitive blasting agents, high-purity HMX from reclaimed LX-14 and Trident I rocket motor formulations, and RDX from PBXN-106 and Compn. A3. Possible com. products manufd. from recovered military explosives included sporting powder, oil-gas well perforation charges, and fertilizer from reclaimed nitrocellulose-based gun propellants. Other projects currently being explored at the lab/bench scale include catalytic hydrotreating technol. to convert Explosive D (ammonium picrate) contained in Navy projectile to higher value products and the recovery of magnesium from illumination and decoy flares for reuse in the military or for com. applications.

Bibliographic Information

Process safety management on spray system to produce ultrafine RDX powder. Hong, Yaw-Shun; Huang, Chen-Chia; Chang, Fang-Mo; Luo, Shen-Kay; Chen, Sun-I. Department of Applied Chemistry, Chung Cheng Institute of Technology, Taoyuan, Taiwan. Huoyao Jishu (1997), 13(2), 37-47. CODEN: HJISE2 ISSN: 1013-767X. Journal written in Chinese. CAN 129:97364 AN 1998:393643 CAPLUS (Copyright 2002 ACS)

Abstract

Spraying is an useful fabrication technique to obtain ultrafine powd. RDX. A process safety management program for the process involved mech. integrity information, std. operation procedures, safety systems, and maintenance and emergency planning. Following the management procedure, it was possible to reduce manufg. hazards.

Bibliographic Information

Recrystallization technology of powdered RDX. Wang, Jianlong; Xu, Chunyan. North China Institute of Technology, Taiyuan, Peop. Rep. China. Huabei Gongxueyuan Xuebao (1997), 18(3), 262-265. CODEN: HUGXFH ISSN: 1006-5431. Journal written in Chinese. CAN 129:83380 AN 1998:365791 CAPLUS (Copyright 2002 ACS)

Abstract

The technol. of producing powd. RDX by recrystn. was studied, with emphasis on the factors that affect the quality of the product.

Bibliographic Information

Recovery and reuse of rocket propellants. Melvin, William S.; Starling, Jarel P. U.S. Army Missile Command, Research, Development, and Engineering Center, Propulsion Directorate, Redstone Arsenal, AL, USA. NASA Conf. Publ. (1997), 3349(Second Aerospace Environmental Technology Conference, 1996), 193-201. CODEN: NACPDX ISSN: 0191-7811. Journal written in English. CAN 128:296643 AN 1998:300290 CAPLUS (Copyright 2002 ACS)

Abstract

An ongoing process development effort by the U.S. Army Missile Command (MICOM) to support environmentally safe rocket motor demilitarization demonstrations was discussed. This process is used to recover oxidizer and fuel ingredients from tactical and strategic class 1.1 and 1.3 solid propellants for recycle/reuse. The closed-loop demilitarization method uses liq. anhyd. ammonia as the processing solvent for ingredient extn. and recovery. A pilot-plant facility was designed and constructed in Magna, Utah, to demonstrate this technol. using Multiple Launch Rocket System (MLRS) and Chaparral tactical solid rocket motors. In July 1996, the pilot plant successfully completed full-scale MLRS propellant testing in a batch process mode at rates approaching 90 kg/h. Process descriptions of the integrated Class 1.1/1.3 rocket motor demilitarization system involving propellant removal, ingredient extn., binder sepn., oxidizer recovery, and solvent regeneration were provided. Test results demonstrating the ability of energetic products recovered by this process to be recycled into other products, and future work plans in support of this program also, were included.

Bibliographic Information

Recovering of components from plastic bonded propellants. Bohn, Manfred A.; Schweppe, Rainer; Weisweiler, Werner. Fraunhofer-Institut fur Chemische Technologie (ICT), Pfinztal, Germany. Waste Management (Oxford) (1998), Volume Date 1997, 17(2/3), 175-185. CODEN: WAMAE2 ISSN: 0956-053X. Journal written in English. CAN 128:219125 AN 1998:219158 CAPLUS (Copyright 2002 ACS)

Abstract

In order to recover the components of so-called "plastic-bonded propellants" (e.g., cryst. energetic materials bonded in a chem. three-dimensional crosslinked polyurethane matrix), the polyurethane matrix is broken solvolytically with water and alk. water (0.05 N-0.5 N NaOH) at 130-170°. Using a model rocket propellant, consisting of a polyether polyol mixt. (Lupranol 1000/2021) cured with Desmodur T80 and filled with 60 wt.% ammonium perchlorate (AP), 84-90% of the polyether polyol component was recovered, and 98% of the AP content subsequently detd. in the aq. hydrolyzate. The polyether polyols were nearly unchanged at 170° for 2 h, as shown by the molar mass distributions (detd. by gel permeation chromatog.). The solid gun propellant KHP (86 wt.% RDX-14 wt.% GAP-Desmodur N100 binder) was solvolyzed at 130, 150, and 170° with pure water and with 0.05 N NaOH for 10, 30, and 60 min. RDX was recovered in high yields and high purity. Under similar hydrolytic conditions, GAP did not behave in the same way as the Lupranol polyether polyols. The molar mass distribution of GPA was broadened and its azide content reduced, as detd. via IR absorption of the asym. N3 stretching vibration, and by differential scanning calorimetry, in both cases in relation to the azide content of the unreacted GAP. Neither the GAP-N100 binder or GAP were recoverable. Under these conditions, the N3 group decompd., yielding a nitrene functionality which formed solvolytically not scissionable C-N bonds by intermol. insertion reactions. The main gaseous reaction products in the solvolysis of KHP were N2, and N2O, with a little CO2, O2, and CO, and small amts. of NH3 and HCHO. The following ionic decompn. products were obsd.: NO2-, NO3-, HCOO- and NH4+.

Bibliographic Information

Value added products from reclamation of military munitions. Burch, D.; Johnson, M.; Sims, K. Crane Division (Code 4073), Naval Surface Warfare Center, Crane, IN, USA. Waste Management (Oxford) (1998), Volume Date 1997, 17(2/3), 159-163. CODEN: WAMAE2 ISSN: 0956-053X. Journal written in English. CAN 128:219168 AN 1998:219156 CAPLUS (Copyright 2002 ACS)

Abstract

The Department of Defense has a backlog of excess, obsolete and unserviceable munitions for disposal. For many of these munition items the only method of disposal is open burning/open detonation (OB/OD) which destroys valuable resources which can be reclaimed and converted to useful products. The Crane Division, Naval Surface Warfare Center (NAVSURFWARCENDIV Crane) in support of the Navy's Ordnance Reclamation Program and the Joint Service Large Rocket Motor Disposal Program has been developing technol. for the removal and reclamation of the energetics from munitions. The University of Missouri-Rolla has demonstrated the use of high pressure waterjet technol. for removal of PBX explosives from projectiles and warheads. Development work is nearing completion for demonstrating the capability to remove Class 1.1 propellant from strategic rocket motors using high pressure waterjets. Current projects are under way focusing on resource recovery and recycling (R3) of the reclaimed energetics while minimizing disposal. The current reclamation projects include reformulation of the explosives and Class 1.1 propellants into com. blasting agents, reuse of Navy gun propellant for various applications including agriculture and oil-gas well stimulation. Other projects include the recovery of RDX/HMX from Class 1.1 explosives and propellants and the conversion of Explosive D into higher value products. Lab/bench scale testing has been completed on many of these processes, and for some pilot scale demonstrations have been or are scheduled to be completed during 1997.

Bibliographic Information

Solubility and phase behavior of PEP binders in supercritical carbon dioxide. Dinoia, Todd P.; Mchugh, Mark A.; Cocchiaro, James E.; Morris, Jeffrey B. Department of Chemical Engineering, The Johns Hopkins University, Baltimore, MD, USA. Waste Management (Oxford) (1998), Volume Date 1997, 17(2/3), 151-158. CODEN: WAMAE2 ISSN: 0956-053X. Journal written in English. CAN 128:232440 AN 1998:219155 CAPLUS (Copyright 2002 ACS)

Abstract

Soly. and phase behavior data up to 300° and pressures to 3000 bars were presented for various propellant, explosive, and pyrotechnic (PEP) binder polymers in supercrit. CO2 with and without modifiers. The binder polymers investigated were polyethylene (PE), oxidized PE, poly(urethane), cellulose acetate butyrate (CAB), poly(vinylidene fluoride-co-hexafluoropropylene) with .apprx.20 mol% hexafluoropropylene (Fluorel and Viton), and poly(chlorotrifluoroethylene-co-vinylidene fluoride) with 24 mol% (Kel-F 800) and 69 mol% (Kel-F 3700) vinylidene fluoride. CO2 has the characteristics of a weak polar solvent which does not dissolve polyethylene although it is can dissolve low-mol.-wt. nonpolar waxes. However, CO2 is not polar enough to dissolve very polar polymers, such as oxidized PE, polyurethane, Kel-F 3700, and CAB (cellulose acetate butyrate). Moderately polar poly(vinylidene fluoride-co-hexafluoropropylene) and Kel-F 800 are sol. in CO2. The soly. of these two copolymers can be further enhanced using acetone as a modifier with CO2. Addnl., oxidized PE is sol. in CO2 with acetone and ethanol as modifiers, but temps. .gtorsim.200° are needed. The fact that many of these polymers are sol. in neat CO2 suggests the potential for a substantial impact upon environmentally sound processing technologies for polymer-based PEP materials.

Bibliographic Information

A study on the preparation of superfine RDX. Gou, Ruijun; Zhang, Jinglin; Han, Baocheng. North China Institute of Technology, Taiyuan, Peop. Rep. China. Editor(s): Feng, Changgen; Ou, Yuxiang; Zeng, Qingxuan. Theory Pract. Energ. Mater., [Proc. Int. Autumn Semin. Propellants, Explos. Pyrotech.], 2nd (1997), 37-40. Publisher: Publishing House of Ordnance Industry, Beijing, Peop. Rep. China CODEN: 65OYAF Conference written in English. CAN 128:142781 AN 1998:84547 CAPLUS (Copyright 2002 ACS)

Abstract

A process parameter study on prepn. of superfine cyclotrimethylenetrinitramine (RDX) was conducted using solvent-nonsolvent type of recrystn. Change in the process conditions caused significant changes in the particle size distribution, sp. surface area, bulk d. and residual solvent content. The particle size of RDX can be in the range of 2.apprx.0.1 mm by controlling the process conditions.

Bibliographic Information

Demilitarization facility for the environmental and acquisition life cycle analysis of explosives and munitions systems. Jeffers, Scott R.; Corley, John. Energetic Materials Branch (WL/MNME), Eglin AFB, FL, USA. Proceedings - International Symposium on Energetic Materials Technology, Phoenix, 1995 (1995), 337-341. Publisher: American Defense Preparedness Association, Arlington, Va CODEN: 65NDAF Conference written in English. CAN 128:117024 AN 1998:63032 CAPLUS (Copyright 2002 ACS)

Abstract

As part of an environmental life-cycle anal. of the munitions design, manuf., and disposal, an aggressive pilot-scale demilitarization program was developed to recover, recycle, reuse, or dispose of explosives and munitions. Technologies developed at the facility will transition to industry or government agencies tasked to execute demil of prodn. weapons systems. The concurrent development of advanced energetic materials for munitions applications and recovery/treatment/disposal technologies for these materials was essential if they are to be incorporated into inventory systems. The technologies used in this program are: (1) high-pressure water washout for removal of the bulk explosive from the munition containers, (2) high-pressure water maceration for size redn. of bulk material for further processing and for the recovery of water-sol. materials, (3) hydrolysis to remove remaining explosive residues from the sides of the munition allowing for container recovery and reuse, (4) molten salt destruction for an environmentally compatible way to completely destroy and dispose of the unrecoverable materials, (5) and non-thermal discharge plasma processing as a supplement to molten salt destruction for controlling any acid gas formation.

Bibliographic Information

Hazards analysis of an integral Class 1.1/1.3 rocket motor demilitarization and ingredient recovery system using ammonia. Stevens, P. M.; Reed, M. H.; Losee, L. A.; Graul, E. R.; Mitchell, D. H. Global Environmental Solutions (Alliant Techsystems), Magna, UT, USA. Proc. - Int. Symp. Energ. Mater. Technol. (1995), 326-336. Publisher: American Defense Preparedness Association, Arlington, Va CODEN: 65NDAF Conference written in English. CAN 128:117007 AN 1998:63027 CAPLUS (Copyright 2002 ACS)

Abstract

Research efforts conducted at the bench-scale have demonstrated the U.S. Army Missile Command (MICOM) near-crit. fluid technol. (using liq. anhyd. NH3) as a viable method of demilitarizing solid rocket motors for recovery of waste rocket propellants. This method was used to recover valuable ingredients, such as HMX, RDX, ammonium perchlorate, and aluminum/binder crumb from tactical and strategic Class 1.1 and 1.3 solid propellants. Ongoing hazards anal. efforts were reported. Hazards anal. testing has characterized the sensitivity of propellants, process streams, and extd. materials. Hazards anal. techniques, such as logic diagrams, and failure modes and effects anal., have identified credible hazards in the equipment design and pilot plant operations. These potential hazards were tracked by a closed loop system and were mitigated by design features or operating controls. Major hazards identified included: (1) shock initiation of ammonium perchlorate-ammonia solns. and undissolved BTTN, (2) ammonia jet impingement heating, (3) reaction of NH3 with nitroglycerin in Class 1.1 propellants, (4) spills and leaks of ammonia with hazard to operators, (5) instability of byproduct ammonium nitrite, (6) oxygen depletion by N2 displacement, (7) startup-shutdown-sampling-maintenance operation, and (8) abnormal situations and contingency plans.

Bibliographic Information

Crystallization of energetic materials; the effect on stability, sensitivity and processing properties. Meulenbrugge, Jan; van der Steen, Albert; van der Heyden, Antoine. TNO Prins Maurits Lab., Rijswijk, Neth. Proc. - Int. Symp. Energ. Mater. Technol. (1995), 297-302. Publisher: American Defense Preparedness Association, Arlington, Va CODEN: 65NDAF Conference written in English. CAN 128:117022 AN 1998:60343 CAPLUS (Copyright 2002 ACS)

Abstract

Results were presented from expts. on crystn. of HNF (hydrazinium nitroformate) and RDX, and the effect of crystn. on the properties of these materials. Control of the crystn. process for HNF will improve the particle shape, the stability and the processability. Other parameters, like sensitivity, are much more reproducible and the control over the particle size will be improved. For RDX esp., the processability and the sensitivity to shock were improved when the particles are made spherical or treated in another way. Photographs of the crystals were presented as well as the properties of the various batches.

Bibliographic Information

Preparation and characterization of an AN-containing IMX. Zhang, Yian; Zhao, Shengxiang; Wu, Zhixing; Zhang, Chengwei. Xian Modern Chem. Res. Inst., Xian, Peop. Rep. China. Proc. China-Jpn. Semin. Energ. Mater., Saf. Environ. (1996), 75-80. Publisher: Nanjing University of Science and Technology, Nanjing, Peop. Rep. China CODEN: 64ZUAH Conference written in English. CAN 127:265104 AN 1997:588770 CAPLUS (Copyright 2002 ACS)

Abstract

An intermol. explosive (IMX) mixt., XR-30, composed of phase-stabilized ammonium nitrate, ethylenediamine dinitrate, RDX, and a melt-casting agent, was prepd. conventionally, with filling d. greater than 98% theor. max. d. The formulation is a eutectic composite explosive. Its impact sensitivity, H50, is 68.5 cm, with a friction sensitivity 4% probability to reaction. The max. detonation velocity and pressure calcd. with N-M-Q method were 8.22 km/s and 28.9 GPa, resp.

Bibliographic Information

Synthesis of 2,4,6-trinitro-2,4,6-triazacyclohexanone (keto-RDX) from DPT and PHX. Zhang, Yuejun; Xie, Chunping. School Chem. Engineering, Nanjing Univ. Sci. & Technology, Nanjing, Peop. Rep. China. Proc. China-Jpn. Semin. Energ. Mater., Saf. Environ. (1996), 63-69. Publisher: Nanjing University of Science and Technology, Nanjing, Peop. Rep. China CODEN: 64ZUAH Conference written in English. CAN 127:250216 AN 1997:588757 CAPLUS (Copyright 2002 ACS)

Abstract

A method was given for synthesis of 2,4,6-trinitro-2,4,6-triazacyclohexanone (Keto-RDX) from 1,5-methylene-3,7-dinitro-1,3,5,7-tetraazacyclononane (I) [DPT], and urea (or nitrourea) in several kinds of nitrating reagents. Primary investigations were carried out for the reaction forms of nitrolysis fragments I and 1,7-diacetoxy-2,4,6-trinitro-2,4,6-triazacycloheptane (II), and on the mechanism of forming byproduct. The nitrolysis fragments N,N-dihydroxymethylamines [RN(CH2OH)2, N is not NO2] that were not directly substituted by nitro groups condensed with urea or nitrourea to form keto-RDX, whereas N,N-dihydroxymethylnitroamine [O2NN(CH2OH)2] did not. Using I as a reactant, the yield of Keto-RDX was 69% (one mole keto-RDX per mol reactant); the byproducts were HMX, RDX, and smaller mol. fragments. Using II, no keto-RDX product and no cyclonitroamine byproducts were obtained.

Bibliographic Information

Technical research to class 5 RDX crystal in nitric acid system. TianLong, Si Ma; Jie, Zhao Yong. Dep. Technique, Yinguang Chem. Corp., Baiying City, Gansu, Peop. Rep. China. Proc. China-Jpn. Semin. Energ. Mater., Saf. Environ. (1996), 54-62. Publisher: Nanjing University of Science and Technology, Nanjing, Peop. Rep. China CODEN: 64ZUAH Conference written in English. CAN 127:250215 AN 1997:588746 CAPLUS (Copyright 2002 ACS)

Abstract

An improved process for producing RDX by direct oxidn. of hexamethylenetetramine was theor. based on the soln. chem. performance. Using this method, RDX can be made in one step, with a quality that complies with class 5 requirements of USA Military Std. USA-R-398C. By controlling the diln. process, the RDX has a granularity of .gtorsim.85% less than 10 mm.

Bibliographic Information

Evaluation of leaving groups in nitramine synthesis. An experimental and theoretical (AM1) study. Piacenza, G.; Jacob, G.; Girard, A.; Graindorge, H.; Gallo, R. Fac. Sciences Saint-Jerome, Marseille, Fr. Int. Annu. Conf. ICT (1997), 28th(Combustion and Detonation), 124.1-124.12. CODEN: IACIEQ ISSN: 0722-4087. Journal written in English. CAN 127:190355 AN 1997:522194 CAPLUS (Copyright 2002 ACS)

Abstract

An exptl. study of nitrolysis was conducted with 12 selected leaving groups located at the N atoms of hexahydro-s-triazine (a reasonably transposable mol. structure) using 7 nitrating media. Yields and limiting side reactions are given and discussed. A theor. study by semi-empirical quantum mech. calcn. (AM1) is made on this substitution reaction by NO2+ with a series of electrophilic leaving groups, the same as studied exptl. The nature, geometry, and energy of intermediates and of transition states are calcd. These results give a classification of leaving-group ability which is in good agreement with exptl. results. They allow a selection of leaving groups for nitrolysis and design of more efficient synthetic methods for prepg. high energy nitramines.

Bibliographic Information

Crystallization technology of Grade 5 RDX. Wang, Janlong; Ye, Yupeng. North China Inst. Tech., Taiyuan, Peop. Rep. China. Huozhayao (1997), 20(2), 14-15. CODEN: HUOZFT ISSN: 1004-9363. Journal written in Chinese. CAN 127:68122 AN 1997:354693 CAPLUS (Copyright 2002 ACS)

Abstract

A technol. of producing Grade 5 RDX by crystn. was studied.

Bibliographic Information

Study on the nitrolysis of hexamethylenetetramine by NMR spectrometry. Part 2. Some new evidence of the intermediate of HOCH2NHNO2 as a possible precursor to RDX. Fang, Zhi Jie; Chen, Li; Wang, Shao Fang; Chen, Ju; Li, Fu Ping. Institute Chemical Engineering, University Science Technology, Nanjing, Peop. Rep. China. Propellants, Explos., Pyrotech. (1997), 22(2), 78-80. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 127:83507 AN 1997:332267 CAPLUS (Copyright 2002 ACS)

Abstract

The RDX yield from nitrolysis of hexamethylenetetramine (HA) together with methylenedinitramine (MDNA) in 90% HNO3 was greater than 100%. MDNA decompd. completely in 90% HNO3, forming O(CH2ONO2)2, whereas in HNO3-NH4NO3 system, the decompd. fragments of MDNA condensed to form RDX. Based on a comparison of the exptl. results to the 1H-NMR spectra obtained by following the decompn. reaction of MDNA with HNO3, the intermediate, HOCH2NHNO2, was postulated as one of the possible precursors to RDX both in Hale and in K process.

Bibliographic Information

Improvement of combustion property of double base propellant with N,N'-dinitropiperazine. Pan, Wenda; Chang, Jingxiang. Xi'an Modern Chemistry Research Inst., Xi'an, Peop. Rep. China. Guti Huojian Jishu (1997), 20(1), 36-40. CODEN: GHJIFL ISSN: 1006-2793. Journal written in Chinese. CAN 126:253075 AN 1997:244968 CAPLUS (Copyright 2002 ACS)

Abstract

This paper presents the formulation and prepn. method of the double base propellant contg. N,N'-dinitropiperazine (DNP) and investigates the effects of DNP on the energy and combustion properties of the double base propellant. Results show that DNP can decrease burning temp. of double base propellant and increase sp. vol., but its specific impulse is almost const. or has a little decrease. DNP can significantly decrease the burning rate and pressure exponent of the double base propellant.

Bibliographic Information

Preparation of RDX of different particle-size by recrystallization in nitric acid solution. Rui, Jiuhou; Liu, Yuhai; Wu, Siaoqing. North China Inst. Technol., Taiyuan, Peop. Rep. China. Baopo Qicai (1997), 26(1), 10-13. CODEN: BAQIEJ ISSN: 1001-8352. Journal written in Chinese. CAN 126:279788 AN 1997:219443 CAPLUS (Copyright 2002 ACS)

Abstract

A method of prepn. of RDX crystals of different particle size distribution by recrystn. in aq. HNO3 was suggested. The relationship between RDX crystal nucleation, crystal fault formation, and the amt. of included acid in RDX crystals was discussed. Special attention was paid to the process conditions which affected the granularity, shape, and the amt. of included acid in RDX crystals (e.g., the crystn. temp., stirring speed, and the diln. rate). RDX crystals could be prepd. with less than 0.02% included acid.

Bibliographic Information

Supercritical fluid extraction of polar nitrogen containing-substances. Niehaus, M.; Teipel, U.; Bunte, G.; Krause, H.; Weisweiler, W. Fraunhofer Institut fur Chemische Technologie (ICT), Pfinztal, Germany. Process Technol. Proc. (1996), 12(High Pressure Chemical Engineering), 345-350. CODEN: PTPREM ISSN: 0921-8610. Journal written in English. CAN 126:187773 AN 1997:79413 CAPLUS (Copyright 2002 ACS)

Abstract

Dynamic fluid extn. with supercrit. CO2 was investigated for the purifn. and prepn. of fine particles of polar nitrogen-contg. compds. (e.g., typical explosives and energetic compds. such as PETN, nitroguanidine, RDX, and 3-nitro-1,2,4-triazole). The two processes examd. were: (1) rapid expansion of supercrit. solns. (RESS), and (2) the gas-antisolvent (GAS) process. All explosives except nitroguanidine could be extd., although for RDX and 3-nitro-1,2,4-triazole, modifiers were necessary. The results demonstrated the high capacity of modified supercrit. CO2 as a solvent in RESS and GAS processes. Suitable modifiers must be examd. empirically.

Bibliographic Information

New Method for preparation of ultrafine RDX crystals. Rui, Jiuhou; Wang, Zeshan; Liu, Yuhai; Shi, Jie. School of Chemical Engineering, NUST, Nanjing, Peop. Rep. China. Nanjing Ligong Daxue Xuebao (1996), 20(5), 385-388. CODEN: NLIXET ISSN: 1005-9830. Journal written in Chinese. CAN 125:333433 AN 1996:686435 CAPLUS (Copyright 2002 ACS)

Abstract

A new method for the direct prepn. of ultrafine RDX crystals was described, in which RDX is dissolved in 98% HNO3 and then treated with water at 0-50°, during which fine and ultrapure RDX crystals ppt. Using the solvent (98% HNO3)-non-solvent (H2O) pptn. technique, 50 g-scale expts. were conducted. Depending on the crystn. condition chosen, ultrafine RDX crystals of 5 to .apprx.7 mm median particle diam. were prepd. Special emphasis was paid to the study of the process conditions affecting the granularity of the ultrafine RDX crystals (e.g., the crystn. temp., stirring speed, concn. of the soln. and the amt. of diln. water).

Bibliographic Information

New method for preparing submicron explosives - microemulsion method. Liu, Zhijian; Fan, Shijun. Xi'an Modern Chemistry Research Institute, Xi'an, Peop. Rep. China. Huozhayao (1996), 19(4), 12-13. CODEN: HUOZFT ISSN: 1004-9363. Journal written in Chinese. CAN 125:252227 AN 1996:621954 CAPLUS (Copyright 2002 ACS)

Abstract

This paper presents, for the fabrication of ultrafine particle explosives, a novel method, the microemulsion method which yields 1.02-0.42 mm-particle explosives. In this paper, the theor. basis of the method and a physicochem. model for the ultrafine particle formation are elucidated, and also four basic compns. for microemulsion explosives are given.

Bibliographic Information

New method for improving the particle size of RDX. Zhang, Nanjiang. Huahei Inst. Technol., Taiyuan, Peop. Rep. China. Huozhayao (1996), 19(3), 23-24. CODEN: HUOZFT ISSN: 1004-9363. Journal written in Chinese. CAN 125:252221 AN 1996:558168 CAPLUS (Copyright 2002 ACS)

Abstract

In the manufg. of RDX, crystal grain size of RDX is improved (increased) by adding to the crystn. soln. the surfactant dodecyl sodium sulfate.

Bibliographic Information

Extraction of explosives by supercritical fluids. Niehaus, M.; Teipel, U.; Krause, H.; Bunte, G. Fraunhofer Institut Chemische Technologie (ICT), Pfinztal, Germany. Int. Annu. Conf. ICT (1996), 27th(Energetic Materials), 128.1-128.16. CODEN: IACIEQ Journal written in German. CAN 125:200039 AN 1996:514603 CAPLUS (Copyright 2002 ACS)

Abstract

The soly. parameters of explosives in supercrit. carbon dioxide are important for evaluation of novel techniques in manuf. and also in quant. anal. Efforts have been made to use the unique possibilities that supercrit. carbon dioxide offers, such as nontoxicity and therefore redn. of environmental pollution or low-temp. processing resulting in addnl. process safety. Also, the performance of explosives improves because of the minimization of contamination caused by conventional org. solvents with low vapor pressure. Supercrit. fluid extn. of the explosives pentaerythrityl tetranitrate (PETN), nitroguanidine (NIGU), RDX, and 3-Nitro-1,3,4-triazole (NTO) has been done in the dynamic mode with pure and modified carbon dioxide. All explosives except nitroguanidine have been extd., although for RDX and NTO use of modifiers proved to be necessary. Effective modifiers must be chosen empirically. The results show the high potential of supercrit. fluids as substitutes for org. solvents.

Bibliographic Information

Bench-scale cooling crystallization of RDX. ter Horst, J. H.; Geertman, R. M.; van der Heijden, A. E.; van Rosmalen, G. M. Laboratory for Process Equipment, Delft Univ. of Technology, Delft, Neth. Int. Annu. Conf. ICT (1996), 27th(Energetic Materials), 126.1-126.11. CODEN: IACIEQ Journal written in English. CAN 125:225933 AN 1996:514601 CAPLUS (Copyright 2002 ACS)

Abstract

Crystals of the explosive RDX were produced by bench-scale batch cooling crystn. and on the lab. scale using three solvents: (1) cyclohexanone, (2) cyclohexanone satd. (3 wt.%) water, and (3) g-butyrolactone. The morphol. of the RDX crystals was strongly dependent on the solvent and independent of the prodn. scale. Crystn. from cyclohexanone gaves block-like RDX crystals with large macrosteps, indicating blockage of growth. When crystn. takes place from cyclohexanone satd. with water, the macrostep formation seems to be eliminated. Comparison of the crystals growing from stagnant solns. and from the bench-scale expts. showed that the turbulence in the crystallizer, that leads to crystal collisions, has a large neg. influence on the formation of crystal inclusions, esp. at high solid loadings.

Bibliographic Information

Study on the nitrolysis of hexamethylenetetramine by NMR-spectrometry. IV. A novel mechanism of the formation of RDX from HA. Fang, Zhijie; Wang, Shaofang; Li, Fuping. Inst. Chemical Eng., Nanjing Univ. Sci. Technology, Jiangsu, Peop. Rep. China. Int. Annu. Conf. ICT (1996), 27th(Energetic Materials), 89.1-89.7. CODEN: IACIEQ Journal written in English. CAN 125:172518 AN 1996:514567 CAPLUS (Copyright 2002 ACS)

Abstract

The mechanisms of the nitrolysis of hexamethylenetetramine (hexamine or HA) with nitric acid and with the mist. of nitric acid and ammonium nitrate to form 1,3,5-trinitro-1,3,5-triazacyclhexane (hexogen or RDX) were studied by NMR tracing. It was found that HA immediately disappeared, while RDX was formed gradually, which indicates the formation of some intermediates in the HA nitrolysis to give RDX. The chem. shift of the peaks in the 1H and 13C NMR tracing spectra disagreed with the possible cyclic-structure intermediates proposed by G. F. Wright (1969) and co-workers. Comparison of the 13C NMR spectra showed that the nitrolysis fragments in K process can be used to form RDX. Based on the results, structures of intermediates were proposed. All the evidences mentioned above suggested a novel mechanism of the formation of RDX form HA, i.e., the nitrolysis of HA first gives some open-chain methylenenitramine intermediates, and the condensation of the latter gives RDX under certain conditions.

Bibliographic Information

New nitration and nitrolysis procedures in the synthesis of energetic materials. Pagoria, Philip F.; Mitchell, Alexander R.; Schmidt, Robert D.; Coon, Clifford L.; Jessop, Edward S. Energetic mater. Cent., Lawrence Livermore Natl. Lab., Livermore, CA, USA. ACS Symp. Ser. (1996), 623(Nitration), 151-164. CODEN: ACSMC8 ISSN: 0097-6156. Journal written in English. CAN 125:37462 AN 1996:288534 CAPLUS (Copyright 2002 ACS)

Abstract

The development of new nitrolysis and nitration reagents are essential to the research and development of energetic materials. In this paper we describe the development of two new nitrolysis reagents, trifluoromethanesulfonic anhydride/HNO3/N2O5 and trifluoroacetic anhydride/HNO3/N2O5, which were uniquely successful in the nitrolysis of secondary amide groups to yield several new, bicyclic nitramines. An alternative method for the synthesis of secondary nitramines by the mild nitrolysis of N-tert-butoxycarbonyl (N-BOC) derivs. The attempted synthesis of 18O-labeled 2,4,6-trinitroltoluene using trifluoromethanesulfonic acid and NaN18O3 at elevated temps. resulted in incorporation of only two 18O atoms per TNT mol., indicating substantial oxygen exchange.

Bibliographic Information

A facile pressing technique for the preparation of small calibre dual role explosive charge. Kumar, A. S.; Samudre, S. S.; Waghmare, N. G.; Gharia, J. S. Explosives Res. and Development Laboratory, Pune, India. Propellants, Explos., Pyrotech. (1996), 21(2), 106-110. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 124:320938 AN 1996:286536 CAPLUS (Copyright 2002 ACS)

Abstract

Small-caliber shaped charges were prepd. by pressing of RDX-wax compns. The shaped-charge performance was considerably influenced by the d. gradient which is an inherent drawback assocd. with pressing. A new method, double-action pressing, was developed which overcomes this problem and is amenable for large-scale prodn. Properties of the charges prepd. by the different methods, esp. with respect to the d. gradient and performance against targets, were presented and discussed. The penetration performance was increased by 8-10% with explosives prepd. by the double-action pressing technique.

Bibliographic Information

Manufacture of HMX with high yield using byproducts from DPT nitrolysis. Xi, Meihong; Deng, Ning. Nanjing Univ. Sci. and Technol., Nanjing, Peop. Rep. China. Editor(s): Yuxiang, Ou. Proc. Beijing Int. Symp. Pyrotech. Explos., 3rd (1995), 280-283. Publisher: China Ordnance Society, Beijing, Peop. Rep. China CODEN: 62RIAT Conference written in English. CAN 124:347528 AN 1996:285175 CAPLUS (Copyright 2002 ACS)

Abstract

In the step-wise nitrolysis of DPT and hexamine (HA), the condensation of nitrolyzed segments of HA and linear nitramines produced in nitrolysis of DPT can increase in yield of HMX to 60% (counted by DPT) and yield of RDX to 75% (counted by HA). The presence of condensation is conformed in the nitrolysis of HA.

Bibliographic Information

Methods for the production of fine particle explosives. Ji, Liguo; Jiao, Qingjie; Cai, Ruijiao. Beijing Institute Technology, Beijing, Peop. Rep. China. Editor(s): Yuxiang, Ou. Proc. Beijing Int. Symp. Pyrotech. Explos., 3rd (1995), 170-174. Publisher: China Ordnance Society, Beijing, Peop. Rep. China CODEN: 62RIAT Conference written in English. CAN 124:347523 AN 1996:285153 CAPLUS (Copyright 2002 ACS)

Abstract

A ultrasonic generator and a sprayer are used in the prodn. of fine cryst. explosive. The cavity effect of ultrasonic is used to crush explosive particles while substituting stirring app. The recryst. process of explosive is controlled by the sprayer. The mechanism of ultrasonic and spraying jet is discussed. Fine particles of PETN and RDX having medium diams. less than 10 mm are manufd. in the process.

Bibliographic Information

Conformation of intermediate HOCH2NHNO2 from nitrolysis of hexamethylentetramine as possible precursor for RDX formation by NMR spectrometry study. Fang, Zhijie; Chen, Li; Wang, Shaofang; Chen, Ju; Li, Fuping. Institute Chemical Engineering, Nanjing University Science and Technology, Nanjing, Peop. Rep. China. Editor(s): Yuxiang, Ou. Proc. Beijing Int. Symp. Pyrotech. Explos., 3rd (1995), 121-123. Publisher: China Ordnance Society, Beijing, Peop. Rep. China CODEN: 62RIAT Conference written in English. CAN 124:347522 AN 1996:285144 CAPLUS (Copyright 2002 ACS)

Abstract

RDX manufd. from nitrolysis of hexamine together with methylenedinitramine (MDNA) in 90% nitric acid is reported. MDNA decompd. completely in 90% nitric acid, forming O(CH2ONO2)2, while in HNO3-NH4NO3 system the decompd. fragments of MDNA condensed into RDX. On the basis of the comparison of the exptl. results to the 1H NMR spectra obtained by following the decompn. reaction of MDNA with nitric acid, the intermediate, HOCH2NHNO2, was postulated as one of the possible precursors to RDX both in Hale and in K process.

Bibliographic Information

Detecting genotoxic activity in industrial effluents using the SOS Chromotest microplate assay. Legault, Richard; Blaise, C.; Trottier, S.; White, P. A. Cent. Saint-Laurent, Environment Canada, Montreal, Can. Environ. Toxicol. Water Qual. (1996), 11(2), 151-65. CODEN: ETWQEZ ISSN: 1053-4725. Journal written in English. CAN 124:335056 AN 1996:271876 CAPLUS (Copyright 2002 ACS)

Abstract

The SOS Chromotest, a cost-effective short-term bacterial genotoxicity screening assay, was performed to appraise its capacity for detecting the presence of sol. genotoxic activity in industrial effluent samples (org. and inorg. chem. plants, metallurgical plants, pulp and paper mills, municipal wastewater treatment plants). An optimized methodol., based on criteria taking into account b-galactosidase activity (the indicator of SOS gene induction), alk. phosphatase activity (the indicator of cytotoxicity), and two genotoxicity measurement end points (min. genotoxic concn. and max. induction factor), was employed to generate reliable results that overcame the potential interferences inherent to complex wastewaters. Of 48 effluent samples tested, 37 (77%) elicited a significant induction of the Escherichia coli PQ37 SOS response. Effluents from inorg. chem. plants and pulp and paper mills displayed the most potent responses, with and without metabolizing enzymes (S9 mix). In general, chem. data available for some wastewaters supported SOS Chromotest pos. responses. The genotoxic activity of whole effluents subjected to a 5-day aeration treatment was as high as that of native (un-aerated) samples, suggesting that sol. genotoxicants are relatively recalcitrant to oxidn., although redns. in genotoxic activity did occur. This study indicates that the SOS Chromotest is sufficiently sensitive to screen for the presence of sol. DNA-damaging agents in a wide variety of un-concd. wastewater samples.

Bibliographic Information

Relationship between crystallization and acidity for RDX. Lu, Yuexian; Chang, Zhihong. North China Inst. Technol., Taiyuan, Peop. Rep. China. Huozhayao (1996), 19(1), 15-18. CODEN: HUOZFT Journal written in Chinese. CAN 124:293627 AN 1996:254833 CAPLUS (Copyright 2002 ACS)

Abstract

Based on the technol. of RDX prepn. by nitrolysis of hexamethylenetetramine (HA), the effect of each factor in crystn. on the acidity of the product was investigated. By controlling the crystn. point and each factor in crystn., the acidity of large-grain product can be reduced such that the RDX product conforms to the appropriate American Military stds.

Bibliographic Information

Crystal growth of energetic materials during high acceleration. Lanzerotti, M. Y. D.; Autera, J.; Borne, L.; Sharma, J. ARDEC, U.S. Army, Picatinny Arsenal, NJ, USA. Mater. Res. Soc. Symp. Proc. (1996), 418(Decomposition, Combustion, and Detonation Chemistry of Energetic Materials), 73-8. CODEN: MRSPDH ISSN: 0272-9172. Journal written in English. CAN 124:206434 AN 1996:176813 CAPLUS (Copyright 2002 ACS)

Abstract

Studies of the growth of crystals of energetic materials under conditions of high acceleration in an ultracentrifuge were reported. When a satd. soln. is accelerated in an ultracentrifuge, the solute mols. move individually through the solvent mols. to form a crystal at the outer edge of the tube if the solute is more dense than the solvent. Since there is no evapn. or temp. variation, convection currents caused by simultaneous movement of solvent and solute are minimized and crystal defects are potentially minimized. Crystal growth is thus controlled by the g-level of the acceleration. In addn., soln. inclusions and bubbles migrate out of the satd. soln. as a result of the pressure gradient induced by the g-force. Results were presented for TNT, RDX, and TNAZ grown at high g from various solns.

Bibliographic Information

Granularity and spheroidization of RDX. Rui, Jiuhou; Ye, Yupeng; Liu, Yuhai; Gu, Jianliang. Sch. Chem. Eng., NUST, Nanjing, Peop. Rep. China. Nanjing Ligong Daxue Xuebao (1995), 19(6), 497-500. CODEN: NLIXET ISSN: 1005-9830. Journal written in Chinese. CAN 124:150101 AN 1996:63600 CAPLUS (Copyright 2002 ACS)

Abstract

A method was described for the direct prepn. of ball-grain RDX that afforded different particle size distributions. HNO3(98%) was reacted with a second acid to form a soln. of RDX in HNO3; the ball-grain RDX with different particle size distributions were then prepd. directly by making use of the technique of solvent/nonsolvent pptn. Expts. with scales of 50 g yield were carried out in the lab. The six classes of ball-grain RDX prepd. directly the acids met the American military specification qualities of the products. Special attention was paid to factors which affect the granularity and spheroidization of RDX (e.g., crystn. temp., stirer speed, and diln. rate).

Bibliographic Information

Recovery of ingredients from plastic-bonded propellants. Bohn, M. A.; Schweppe, R.; Weisweiler, W. Fraunhofer-Institut fur Chemische Technologie (ICT), Pfinztal, Germany. Int. Annu. Conf. ICT (1995), 26th(Pyrotechnics), 44/1-44/32. CODEN: IACIEQ Journal written in German. CAN 124:33073 AN 1995:866216 CAPLUS (Copyright 2002 ACS)

Abstract

The possibility of recovery of energetic ingredients and binders from urethane-bonded propellants was examd. in a process based on high-temp. hydrolysis/solvolysis at 130-170° in pure water and alk. (0.05-0.5 N NaOH) medium. Ammonium perchlorate could be 98% recovered from the aq. soln. from hydrolysis of a 40:60 polyetherdiol-based urethane (prepd. from Lupranol 1000, Lupranol 2021, and TDI); the polyetherpolyol component was 84-90% recoverable and did not show any structural or mol. wt. changes after hydrolysis at 170° for 2 h. Treatment of a second propellant (contg. 86 wt.% RDX and 14 wt.% glycidyl azide-Desmodur N100 copolymer) at 130, 150, and 179° in pure water and 0.05 N NaOH for 10, 30, and 60 min resulted in high recovery of RDX but the GAP-derived urethane was recovered with a significant loss of azide groups. In this case, the azide group reacted to form N2 and nitrenes which formed non-reactive carbon-nitrogen bonds through intermol. insertion reactions, in addn. to nitrogen-contg. gaseous products and aq. ions.

Bibliographic Information

Process and apparatus for producing ultrafine explosive particles. (du Pont de Nemours, E. I., and Co., USA). Israeli (1995), 24 pp. CODEN: ISXXAQ IL 100231 A1 19950124 Patent written in English. Application: IL 91-100231 19911203. CAN 123:117652 AN 1995:743038 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
IL 100231 A1 19950124 IL 1991-100231 19911203

Abstract

An app. for producing ultrafine explosive particles comprises (1) means for injecting a soln. of a crystallizable explosive compns. and a nonsolvent soln. for mixing with the explosive compn. soln., (2) nozzles being adapted for moving the explosive compn. and nonsolvent solns., (3) venturi means communicating with nozzle means, and (4) explosive particle collection means connected with venturi means. The app. further comprises an auxiliary inlet means coaxial with and surrounding the explosive compns. and the nonsolvent soln. inlet means. The nozzle means include first and second continuous orifices. The ultrafine granular explosives which when incorporated into a binder system have the ability to propagate in thin sheets and have very low impact and very high propagation sensitivities.

Bibliographic Information

Method for making explosive charges by filtering liquid explosive. Vlassov, D. A. St. Petersburg Technological Inst., Russia. Hanneng Cailiao (1993), 1(1), 27-30. CODEN: HACAFQ Journal written in English. CAN 123:117600 AN 1995:695221 CAPLUS (Copyright 2002 ACS)

Abstract

A relatively safe method was developed for manuf. of explosive charges contg. a solid cryst. explosive and a liq. thermoplastic or thermosetting (i.e., polymg.) material (typically cryst. RDX and molten TNT). The technique involved filling of shells; calcns. were presented to calc. the porosity of RDX and the vol. of molten TNT that is necessary to fill the pores. The method was esp suitable for manuf. of rocket fuel compns. contg. solid oxidizer, metals, and liq. polymeric binder.

Bibliographic Information

Study on the nitrolysis of hexamethylenetetramine by NMR spectrometry. Fang, Zhijie; Chen, Li; Wang, Shaofang; Chen, Ju; Li, Fuping. Inst. Chemical Engineering, Nanjing Univ. Science and Technol., Nanjing, Jiangsu, Peop. Rep. China. Propellants, Explos., Pyrotech. (1995), 20(2), 83-6. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 122:294747 AN 1995:550727 CAPLUS (Copyright 2002 ACS)

Abstract

The nitrolysis of hexamethylenetetramine (HA) and 1,3,5-trioxane was studied by NMR spectrometry. The structure of the nitrolysis products of the trioxane could be monomethylenedinitrate, dioxymethylenenitronitrate and trioxymethylenenitronitrate, of structures O2N(OCH2)nONO2 (n = 1,2,3). A comparison of the 1H and 13C spectra of the nitrolysis mixt. of HA with the nitrolysis products of trioxane proved that in the nitrolysis mixt. of HA, the methylene group which cannot be used to form 1,3,5-triazacyclohexane (RDX) appears in O2N(OCH2)ONO2 and not in CH2(ONO2)2.

Bibliographic Information

Separation of RDX and HMX by recrystallization using supercritical fluids as anti-solvent. Gallagher, Paula M.; Krukonis, Val J.; Coffey, Michael P. (Phasex Corp., USA). U.S. (1995), 20 pp. CODEN: USXXAM US 5389263 A 19950214 Patent written in English. Application: US 92-886603 19920520. CAN 122:269545 AN 1995:420719 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
US 5389263 A 19950214 US 1992-886603 19920520

Abstract

Materials that are ordinarily difficult-to-comminute such as a mixt. of RDX and HMX are sepd. by dissolving in a common liq. solvent to form a soln., adding to the soln. a supercrit. fluid to induce pptn. of one component of the components of the solid mixt. resulting in a pptd. component, and collecting the pptd. component. The process shows effective at sepg. HMX and RDX to obtain a ppt. of RDX which is essentially free of HMX.

Bibliographic Information

Recrystallization process of RDX and cobalt chloride using anti-solvent methods. Krukonis, Val J.; Gallagher, P. M.; Coffey, M. P. (Phasex Corp., USA). U.S. (1994), 21 pp. Cont.-in-part of U.S. Ser. No. 421,978, abandoned. CODEN: USXXAM US 5360478 A 19941101 Patent written in English. Application: US 91-723245 19910628. Priority: US 89-421978 19891016. CAN 122:34594 AN 1995:229370 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
US 5360478 A 19941101 US 1991-723245 19910628

Priority Application Information
US 1989-421978 19891016

Abstract

In recrystg. solid RDX from systems comprising a solute which is the eventual material recrystd. and a liq. which is a suitable solvent for the solute, a gaseous component which is sol. within the solvent is added into the system to cause the solvent to approach or attain a supersatd. state and solute material to ppt. By control of process parameters such as pressure, temp., time, and rate, rate of injection of gas, the properties of the material recrystd. can be influenced.

Bibliographic Information

Rapid near-IR measurements of explosives. Eisenreich, N.; Kull, H.; Hertz, J. Fraunhofer-Institut fur Chemische Technologie, Pfinztal, Germany. Int. Annu. Conf. ICT (1994), 25TH(ENERGETIC MATERIALS-ANALYSIS, CHARACTERIZATION AND TEST TECHNIQUES), 86/1-86/7. CODEN: IACIEQ Journal; General Review written in German. CAN 122:13139 AN 1995:192723 CAPLUS (Copyright 2002 ACS)

Abstract

A review, with 6 refs., of the use of rapid near-IR (NIR) spectroscopy for online evaluation of explosives (esp. during manuf. and processing). Topics discussed include rapid NIR spectrometry with acoustooptical filters and the NIR spectra of energetic materials. Spectra given were nitromethane, GAP, TAGN (triaminoguanidine nitrate), TNT, RDX, HMX, ammonium nitrate, and ammonium perchlorate.

Bibliographic Information

Explosive property and mechanical characteristics of the trial PBX consisting of RDX and HTPB. Sato, Junichi; Shinkai, Masanori; Ito, Takeshi. Dep. Chem., Natl. Def. Acad., Yokosuka, Japan. Kayaku Gakkaishi (1994), 55(3), 89-95. CODEN: KAGAEA Journal written in English. CAN 121:160342 AN 1994:560342 CAPLUS (Copyright 2002 ACS)

Abstract

The prepn. of PBX (plastic-bonded explosive), consisting of RDX and hydroxy-terminated polybutadiene (HTPB) binder, was attempted. Various tests of explosive properties and mech. characteristics were carried out on the RDX-HTPB compn. as a trial PBX.

Bibliographic Information

Extraction of nitramine propellants using supercritical fluids. Morris, J.B.; McNesby, K.L.; Pesce-Rodriguez, R.A.; Schroeder, M.A.; Fifer, R.A. WT, U.S. Army Res. Lab., Aberdeen Proving Ground, MD, USA. Int. Annu. Conf. ICT (1993), 24th(Energetic Materials: Insensitivity and Environmental Awareness), 37-1/37-12. CODEN: IACIEQ Journal written in English. CAN 120:326901 AN 1994:326901 CAPLUS (Copyright 2002 ACS)

Abstract

The addn. of org. modifiers (co-solvents) for CO2-based supercrit. fluid extn. of an RDX-based LOVA composite gun propellant was examd. for the purpose of maximizing RDX recovery. Under supercrit. fluid extn. conditions (32° and 55 MPa for 45 min), MeCN displayed the greatest soly., or dissoln. rate enhancement, for RDX, with nitromethane a close second. When extg. solid gun propellant, solvent-modified CO2 fluid caused significant swelling of the propellant relative to the use of heat CO2. In addn. to RDX, the gun propellant contained cellulose acetate butyrate, nitrocellulose, plasticizer, and other additives.

Bibliographic Information

Design and calibration of pulsed vapor generators for TNT, RDX and PETN. Davies, J. P.; Blackwood, L. G.; Davis, S. G.; Goodrich, L. D.; Larson, R. A. Idaho Nat. Eng. Lab., Idaho Falls, ID, USA. Editor(s): Yinon, Jehuda. Adv. Anal. Detect. Explos., Proc. Int. Symp., 4th (1993), Meeting Date 1992, 513-32. Publisher: Kluwer, Dordrecht, Neth CODEN: 59MKAE Conference written in English. CAN 120:221786 AN 1994:221786 CAPLUS (Copyright 2002 ACS)

Abstract

Computer-controlled explosive vapor generators for TNT, RDX, and PETN were built and calibrated to support an independent validation and verification facility for Explosive detection systems for the Federal Aviation Administration (FAA). The generators were constructed using pure explosive suspended on quartz beads which were then loaded into a coiled stainless steel tube. A carrier gas (ultra-pure air) was passed through the coil to carry the explosive mols. The generators were capable of delivering a pulse of varying explosive mass through the control of coil temp., air flow rate, and pulse width. Preliminary calibrations were completed in the picogram-to-nanogram range using an ion mobility spectrometer as the calibrating instrument. The explosive vapor generators can be used as quant. vapor stds. to establish the lower detection limits for explosive detection systems systems.

Bibliographic Information

Process for preparation of RDX. Lukasavage, William J.; Nicolich, Steven; Slagg, Norman. (United States Dept. of the Army, USA). U.S. (1993), 4 pp. CODEN: USXXAM US 5250687 A 19931005 Patent written in English. Application: US 92-936375 19920828. CAN 119:271209 AN 1993:671209 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
US 5250687 A 19931005 US 1992-936375 19920828

Abstract

The title process comprises repeated sequential addn. of NH4NO3/HNO3 and Ac2O to DAPT. This method, with continuous addn. of quantities of DAPT, provides near-quant. yields of RDX.

Bibliographic Information

Synthesis of carbon-14 labeled hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX). Horvath, Karoly; Alworth, William L. Dep. Chem., Tulane Univ., New Orleans, LA, USA. J. Labelled Compd. Radiopharm. (1993), 33(6), 467-71. CODEN: JLCRD4 ISSN: 0362-4803. Journal written in English. CAN 119:271112 AN 1993:671112 CAPLUS (Copyright 2002 ACS)

Abstract

14C-labeled hexahydro-1,3,5-trinitro-1,3,5-triazine was prepd by nitrolysis of hexahydro-1,3,5-tripropionyl-1,3,5-triazine (1) for bioenvironmental studies. 1 Was synthesized from paraformaldehyde and propionitrile by a modified method reported earlier.

Bibliographic Information

On the use of AM1 and PM3 methods on energetic compounds. De Paz, Jose Luis G.; Ciller, Juan. Dep. I+D, Union Espanola Explosivos, Madrid, Spain. Propellants, Explos., Pyrotech. (1993), 18(1), 33-40. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 118:237100 AN 1993:237100 CAPLUS (Copyright 2002 ACS)

Abstract

Stewart's new semi-empirical method MNDO-PM3 (PM3) was compared with the well-known Dewar's AM1 method in the study of the heats of formation and dipole moments of nitro-substituted compds., esp. for some energetic materials. The PM3 method had better performance than the AM1 method. Adjacent lone pair-lone pair repulsions were better described at the PM3 level; the known systematic correction of .apprx.-9 kcal/mol for each C-NO2 group of the AM1 method became +3.5 kcal/mol at the PM3 level. PM3 results for N-NO2 contg. compds. were directly comparable to exptl. gas phase data.

Bibliographic Information

Process and apparatus for producing ultrafine explosives. McGowan, Michael James. (du Pont de Nemours, E. I., and Co., USA). PCT Int. Appl. (1993), 26 pp. CODEN: PIXXD2 WO 9304018 A1 19930304 Designated States W: CA, NO. Designated States RW: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LU, NL, SE. Patent written in English. Application: WO 91-US5900 19910827. CAN 118:172045 AN 1993:172045 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
WO 9304018 A1 19930304 WO 1991-US5900 19910827
W: CA, NO
RW: AT, BE, CH, DE, DK, ES, FR, GB, GR, IT, LU, NL, SE
EP 600881 A1 19940615 EP 1991-916893 19910827
EP 600881 B1 19960424
R: CH, DE, FR, GB, LI
WO 9304019 A1 19930304 WO 1991-US6748 19910924
W: CS, SU

Priority Application Information
WO 1991-US5900 19910827

Abstract

The process comprises prepg. a stream of a soln. of the explosive dissolved in a solvent and a stream of an inert nonsolvent, injecting the two streams through concentric orifices of a nozzle into a mixing chamber by injecting nonsolvent stream through the central orifice and explosive stream through the outer orifice, converging the streams in a mixing zone under turbulent conditions to entrap the explosive compn. in droplets of nonsolvent and to rapidly ppt. the explosive compn. as spheroidal particles, and recovering the particles from the solvent and nonsolvent materials.

Bibliographic Information

Explosive biodegradation in soil slurry batch reactors amended with exogenous microorganisms. Shen C F; Hawari J A; Paquet L; Ampleman G; Thiboutot S; Guiot S R Environmental Bioengineering Group, Biotechnology Research Institute, National Research Council, 6100 Royalmount Avenue, Montreal, Quebec H4P 2R2, Canada WATER SCIENCE AND TECHNOLOGY (2001), 43(3), 291-8. Journal code: DV8. ISSN:0273-1223. Journal; Article; (JOURNAL ARTICLE) written in English. DN 21274696 PubMed ID 11381919 AN 2001295394 MEDLINE (Copyright 2002 U.S. National Library of Medicine)

Abstract

The present study explores the feasibility of biotreatment of 2,4,6-trinitrotoluene (TNT) and hexahydro-1,3,5-trinitro- 1,3,5-triazine (RDX)-contaminated soils in slurry batch reactors. Radiorespirometric assays showed that anaerobic sludge was able to mineralize 59% RDX to CO2 although significant mineralization of TNT was not observed in all cases. TNT and RDX at concentrations higher than 50 and 100 mg/L respectively were inhibitory to methanogenesis (used as a bioindicator), however, methanogenesis recovered after TNT was transformed into less toxic triaminotoluene. Bioslurry batch reactors containing 40% of contaminated soil (2000 mg RDX and 1000 mg TNT/kg dry soil) were operated under various conditions. Both TNT and RDX were persistent to soil indigenous microbes. Degradation of both TNT and RDX was enhanced by the municipal sludge amendment, although degradation of RDX was only achieved under anaerobic conditions.

Bibliographic Information

Type I nitroreductases in soil enterobacteria reduce TNT (2,4,6,-trinitrotoluene) and RDX (hexahydro-1,3,5-trinitro-1,3,5-triazine). Kitts C L; Green C E; Otley R A; Alvarez M A; Unkefer P J Environmental Biotechnology Institute, California Polytechnic State University, San Luis Obispo 93407, USA. ckitts@calpoly.edu CANADIAN JOURNAL OF MICROBIOLOGY (2000 Mar), 46(3), 278-82. Journal code: CJ3. ISSN:0008-4166. Journal; Article; (JOURNAL ARTICLE) written in English. DN 20211112 PubMed ID 10749541 AN 2000211112 MEDLINE (Copyright 2002 U.S. National Library of Medicine)

Abstract

Many enteric bacteria express a type I oxygen-insensitive nitroreductase, which reduces nitro groups on many different nitroaromatic compounds under aerobic conditions. Enzymatic reduction of nitramines was also documented in enteric bacteria under anaerobic conditions. This study indicates that nitramine reduction in enteric bacteria is carried out by the type I, or oxygen-insensitive nitroreductase, rather than a type II enzyme. The enteric bacterium Morganella morganii strain B2 with documented hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) nitroreductase activity, and Enterobacter cloacae strain 96-3 with documented 2,4,6-trinitrotoluene (TNT) nitroreductase activity, were used here to show that the explosives TNT and RDX were both reduced by a type I nitroreductase. Morganella morganii and E. cloacae exhibited RDX and TNT nitroreductase activities in whole cell assays. Type I nitroreductase, purified from E. cloacae, oxidized NADPH with TNT or RDX as substrate. When expression of the E. cloacae type I nitroreductase gene was induced in an Escherichia coli strain carrying a plasmid, a simultaneous increase in TNT and RDX nitroreductase activities was observed. In addition, neither TNT nor RDX nitroreductase activity was detected in nitrofurazone-resistant mutants of M. morganii. We conclude that a type I nitroreductase present in these two enteric bacteria was responsible for the nitroreduction of both types of explosive.

Bibliographic Information

Degradation of hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) by Stenotrophomonas maltophilia PB1. Binks P R; Nicklin S; Bruce N C Institute of Biotechnology, University of Cambridge, United Kingdom APPLIED AND ENVIRONMENTAL MICROBIOLOGY (1995 Apr), 61(4), 1318-22. Journal code: 6K6. ISSN:0099-2240. Journal; Article; (JOURNAL ARTICLE) written in English. DN 95266812 PubMed ID 7747953 AN 95266812 MEDLINE (Copyright 2002 U.S. National Library of Medicine)

Abstract

A mixed microbial culture capable of metabolizing the explosive RDX (hexahydro-1,3,5-trinitro-1,3,5-triazine) was obtained from soil enrichments under aerobic and nitrogen-limiting conditions. A bacterium, Stenotrophomonas maltophilia PB1, isolated from the culture used RDX as a sole source of nitrogen for growth. Three moles of nitrogen was used per mole of RDX, yielding a metabolite identified by mass spectroscopy and 1H nuclear magnetic resonance analysis as methylene-N-(hydroxymethyl)-hydroxylamine-N'-(hydroxymethyl)nitroamin e. The bacterium also used s-triazine as a sole source of nitrogen but not the structurally similar compounds octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine, cyanuric acid, and melamine. An inducible RDX-degrading activity was present in crude cell extracts.

Bibliographic Information

Isolation of three hexahydro-1,3,5-trinitro-1,3,5-triazine-degrading species of the family Enterobacteriaceae from nitramine explosive-contaminated soil. Kitts C L; Cunningham D P; Unkefer P J Los Alamos National Laboratory, New Mexico 87545 APPLIED AND ENVIRONMENTAL MICROBIOLOGY (1994 Dec), 60(12), 4608-11. Journal code: 6K6. ISSN:0099-2240. Journal; Article; (JOURNAL ARTICLE) written in English. DN 95110151 PubMed ID 7811097 AN 95110151 MEDLINE (Copyright 2002 U.S. National Library of Medicine)

Abstract

Three species of the family Enterobacteriaceae that biochemically reduced hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX) and octahydro-1,3,5,7-tetranitro-1,3,5,7-tetrazocine (HMX) were isolated from nitramine explosive-contaminated soil. Two isolates, identified as Morganella morganii and Providencia rettgeri, completely transformed both RDX and the nitroso-RDX reduction intermediates. The third isolate, identified as Citrobacter freundii, partially transformed RDX and generated high concentrations of nitroso-RDX intermediates. All three isolates produced 14CO2 from labeled RDX under O2-depleted culture conditions. While all three isolates transformed HMX, only M. morganii transformed HMX in the presence of RDX.

megalomania
April 26th, 2002, 01:59 PM
This is everything up to 1992...

Bibliographic Information

Method and device for the production of fine-grained explosive substances. (Nobel Kemi AB, Swed.). Israeli (1992), 12 pp. CODEN: ISXXAQ IL 90108 A1 19920906 Patent written in English. Application: IL 89-90108 19890427. Priority: SE 88-1619 19880429. CAN 118:257713 AN 1993:257713 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
IL 90108 A1 19920906 IL 1989-90108 19890427

Priority Application Information
SE 1988-1619 19880429

Abstract

Explosive raw materials are dissolved in a vaporizable solvent and the soln. is supplied to a stream-driven ejector equipped with a diffuser connected to a cyclone. The fine explosive pptd. in ejector and having a diam. £20 mm are sepd. using a cyclone and vaporized solvent is recovered from cyclone for re-use.

Bibliographic Information

Study of the state of the methylene group in reaction mixtures for nitration of hexamethylenetetramine by NMR spectrometry. Fang, Zhijie; Wang, Shaofang; Chen, Ju; Chen, Li; Li, Fuping. Inst. Chem. Technol., East China Tech. Univ., Nanjing, Peop. Rep. China. Int. Annu. Conf. ICT (1992), 23rd(Waste Manage. Energ. Mater. Polym.), 61/1-61/7. CODEN: IACIEQ Journal written in German. CAN 118:172038 AN 1993:172038 CAPLUS (Copyright 2002 ACS)

Abstract

The nitration of hexamethylenetetramine (I) and trioxane was examd. by NMR spectroscopy in ref. to the manuf. of RDX. The structures of the nitration products of trioxane were O2N(OCH2)nONO2 (II, n = 1-3). According to the comparison of NMR spectra of the nitration of I and trioxane, the methylene group in I which is not used to form RDX was present as II (n = 2), not when n = 1. It was suggested that the nitration of I does not follow the same mechanism as the acetolysis of I.

Bibliographic Information

Safety guidelines for processing aged obsolete munitions. Chen, Tung Ho; Campbell, C.; Ark, W. F. U. S. Army Armament Res. Dev. Eng. Cent., Picatinny Arsenal, NJ, USA. Int. Annu. Conf. ICT (1992), 23rd(Waste Manage. Energ. Mater. Polym.), 18/1-18/12. CODEN: IACIEQ Journal written in English. CAN 118:153656 AN 1993:153656 CAPLUS (Copyright 2002 ACS)

Abstract

The exptl. approach, rationale, and results (including safety guidelines established) for operation of demilitarization facilities to process aged, obsolete munitions is described.

Bibliographic Information

Clean up methods of explosives using Amberlite XAD resin and Norit-A. Park, Sung Woo; Lee, Jung Pil; Hong, Sung Wook; Cha, Ki Won; Kim, Il Kwang; Kim, Taek Jae. Forensic Sci. Div. II, Natl. Inst. Sci. Invest., Seoul, S. Korea. Anal. Sci. Technol. (1991), 4(1), 61-8. CODEN: ASCTET Journal written in Korean. CAN 117:236727 AN 1992:636727 CAPLUS (Copyright 2002 ACS)

Abstract

Five explosives (DNT, TNT, RDX, PETN, and Tetryl) were purified by adsorption on Amberlite XAD 2, Amberlite XAD 7, and Norit A. From distribution coeffs. of each explosive for the XAD resins in pentane, the XAD 7 resin, which has CO groups, adsorbed the 5 explosives (which have NO groups) more strongly than for the nonpolar Amberlite XAD 2 resin. The arom. explosives and oils were adsorbed in MeCN. Recoveries of the 5 explosives (e.g., from oil) using the XAD 7 resin were ³90%. PETN and RDX could be effectively purified with Norit A.

Bibliographic Information

George Clyde Hale, Hoosier chemist and pioneer in ordnance research and the chemistry of the explosive, RDX. Carmack, Marvin. Dep. Chem., Indiana Univ., Bloomington, IN, USA. Proc. Indiana Acad. Sci. (1992), Volume Date 1991, 100(3-4), 173-8. CODEN: PIACAP ISSN: 0073-6767. Journal written in English. CAN 117:232999 AN 1992:632999 CAPLUS (Copyright 2002 ACS)

Abstract

During the 1920's, Dr. George C. Hale, a native of Indiana, developed and published a procedure for the prepn. of a powerful new explosive which he named cyclonite, subsequently known as RDX. Although his research was carried out and published just after World War I, practical industrial processes for the manuf. of this explosive, as well as necessary experience with its use, did not follow until many years later. During World War II, intensive collaborative research effects in several countries made possible large-scale and efficient prodn. in the US in time to have an important influence on the outcome of World War II.

Bibliographic Information

Composite explosives and their manufacture. Rego Lopez, Jose Manuel; Renedo Arenas, Jose Antonio. (Union Espanola de Explosivos S.A., Spain). Eur. Pat. Appl. (1992), 11 pp. CODEN: EPXXDW EP 493638 A1 19920708 Designated States R: DE, ES, FR, GB, IT. Patent written in English. Application: EP 90-500130 19901231. CAN 117:134007 AN 1992:534007 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
EP 493638 A1 19920708 EP 1990-500130 19901231
R: DE, ES, FR, GB, IT

Abstract

The composite explosives comprise a mol. explosive, e.g., TNT, and oxidizer, e.g., NH4NO3 and are prepd. by injecting both molten phases through a static mixer. The final products show good rheol. properties and can be applicable as boosters for industrial use.

Bibliographic Information

A study on condensation of ammonium nitrate in the process of hexamine nitrolysis. Yao, Qizheng; Zhang, Yujian. Dep. Chem. Eng., East China Inst. Technol., Nanjing, Peop. Rep. China. Proc. Int. Pyrotech. Semin. (1991), 17th(Vol. 1), 244-8. CODEN: PPYSD7 ISSN: 0270-1898. Journal written in English. CAN 116:177204 AN 1992:177204 CAPLUS (Copyright 2002 ACS)

Abstract

In the manuf. of ROX by nitrolysis-nitration of hexamine, results reported by G. F. Wright (Can J. Res., 1949, 27B, 520-594), that a 2nd mole of RDX forms by condensation of NH4NO3 with HCHO (from nitrolysis fragments), are unconvincing, in view of the ability of ammonium salts to condense with nitramines and HCHO under similar conditions. Instead, it is proposed that NH4NO3 takes part in condensation reactions via its dehydrated intermediate (or analog), nitroamide, which then reacts with HCHO and methylenenitramine to form RDX. A possible mechanism for the formation of nitroamide involves reaction of NH4NO3 with N oxides (specifically, NO, N2O3, or NO2), formed under nitration conditions in the presence of a dehydrating agent.

Bibliographic Information

Technological studies on K-process for production of RDX. Ye, Yupeng; Chen, Shushen; Jia, Suyun; Guo, Fumin. Taiyuan Inst. Mach., Taiyuan, Peop. Rep. China. Proc. Int. Pyrotech. Semin. (1991), 17th(Vol. 1), 249-53. CODEN: PPYSD7 ISSN: 0270-1898. Journal written in English. CAN 116:154975 AN 1992:154975 CAPLUS (Copyright 2002 ACS)

Abstract

In an improved K-process (Knoffler, 1936) of RDX prepn., involving the reaction of hexamine and NH4NO3 with concd. HNO3, the waste acid is oxidized at a proper concn., and the size grading of RDX is done by dilg. the acid with water. The dil. acid obtained is neutralized with NH3, and the yellow material filtered. Evapn. gives NH4NO3 for recycle, after drying.

Bibliographic Information

Studies on HMX synthesis from paraformaldehyde and ammonium nitrate. Ren, Tesheng; Yan, Hong. Dep. Chem. Eng., Beijing Inst. Technol., Beijing, Peop. Rep. China. Proc. Int. Pyrotech. Semin. (1991), 17th(Vol. 1), 220-3. CODEN: PPYSD7 ISSN: 0270-1898. Journal written in English. CAN 116:154973 AN 1992:154973 CAPLUS (Copyright 2002 ACS)

Abstract

An HMX-RDX mixt. was prepd. from the reaction of paraformaldehyde with NH4NO3 in Ac2O-AcOH. The HMX content of the mixt. approached ³30%. Adding Na2SO3 (1-2 wt. % of the nitrate amt.) raised the HMX content to 40%; the total yield of cyclonitramines amounted to 53.6%.

Bibliographic Information

A transient explosive vapor generator based on capillary gas chromatography. Reiner, George A.; Heisey, Cheryl L.; McNair, Harold M. Dep. Chem., Virginia Polytech. Inst. and State Univ., Blacksburg, VA, USA. J. Energ. Mater. (1991), 9(3), 173-89. CODEN: JOEMDK ISSN: 0737-0652. Journal written in English. CAN 115:283064 AN 1991:683064 CAPLUS (Copyright 2002 ACS)

Abstract

A vapor generator, based on a com. capillary gas chromatog., was developed which produces transient clouds of high-purity explosive vapor. The chem. compn. of the vapor generator was confirmed by both gas chromatog.-mass spectrometry and by ion mobility spectrometry. Clouds of dinitrotoluene, trinitrotoluene, and RDX were prepd.

Bibliographic Information

Evaluation of adhesives for adherence of aluminum to copper. Osterndorf, John F.; Bonk, Robert B. USA. Int. SAMPE Tech. Conf. (1990), 22(Adv. Mater.), 404-17. CODEN: ISTCEF ISSN: 0892-2624. Journal written in English. CAN 115:160730 AN 1991:560730 CAPLUS (Copyright 2002 ACS)

Abstract

In the prodn. of the M-509 load-cup assembly ammuniation, a series of adhesives were evaluated for bonding the copper shape charge to the aluminum alloy housing in the load cup assembly. Both Permabond HHO40 (an aerobic adhesive) and Laminac 4116 (styrene unsatd. polyester resin)/MR511 (styrene unsatd. polyester resin)/methyl ethyl ketone peroxide combinations gave satisfactory durable and compatible structures when evaluated by compression testing (breaking strength) at 3 temps., temp. and humidity aging, temp. cycling and compatibility testing with an energetic material (i.e., an explosive mixt. of RDX, TNT, and wax).

Bibliographic Information

Manufacture of nitrocellulose microcapsules as sensitizer for oil-in-water or water-in-oil explosive emulsions. Lima Filho, Abelardo Vieira de Araujo; Lopes, Joao Egydio. (Vasconcelos, Maria Cristina, Brazil). Braz. Pedido PI (1991), 9 pp. CODEN: BPXXDX BR 9004405 A 19910115 Patent written in Portuguese. Application: BR 90-4405 19900831. CAN 115:74704 AN 1991:474704 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
BR 9004405 A 19910115 BR 1990-4405 19900831

Abstract

Nitrocellulose is dissolved in a water-immiscible solvent to give a thick lacquer; a stabilizer for the nitrocellulose, water, and a colloid are added with sufficient stirring to transform the lacquer into globules suspended in the aq. phase; an antistatic substance is added and gas injected or generated to be enveloped in the globules and simultaneously the solvent is extd. to give nitrocellulose microcapsules with occluded gases; and the microcapsules are filtered out, washed and dried. The nitrocellulose may be completely or partially replaced by cellulose and a nitro compd. added. Al2O3 may also be added. Microcapsules with d. 0.15 g/cm3 and diam. 10-70 mm were obtained by dissolving nitrocellulose and N in Et acetate and acetone, adding stabilizers, anti-static agents, and a colloid, adding water and stirring, distg. the solvent, filtering, washing, and drying. Addn. of the microcapsules to an emulsion matrix gave an explosive with greater detonation velocity, force, and energy than the same matrix with the same amt. of known types of gasifiers or microcapsules.

Bibliographic Information

Biological treatment of an explosives production wastewater. Burrows, W. Dickinson. U. S. Army Biomed. Res. Dev. Lab., Frederick, MD, USA. Hazard. Ind. Wastes (1990), 22nd 339-54. CODEN: HIWAEB ISSN: 1044-0631. Journal written in English. CAN 114:170455 AN 1991:170455 CAPLUS (Copyright 2002 ACS)

Abstract

The operation of a biol. wastewater treatment facility for waste streams from explosive prodn. at the Halston Army Ammunition Plant was evaluated from Jan. 1985 through August 1986. The facility is a conventional design, built to accommodate half the av. wastewater flow of 0.56 m3/s projected for full mobilization and now receiving an av. of 0.22 m3/s, or 80% of capacity, at 15% of mobilization. The activated sludge system has consistently achieved nearly complete removal of biodegradable orgs. using less than the available aeration capacity; and clarifiers, dual media filters, and sludge handling facilities have performed satisfactorily. The upflow, fixed-film anoxic filters are the least satisfactory part of the system. Designed to provide 95% NO3- removal, they have achieved £50% removal during a 20 mo observation period, and the filters are subject to frequent biomass plugging.

Bibliographic Information

Technological preparation procedure and basic characteristics of cast composite explosives based on polyurethane as a binder. Blagojevic, Milorad; Antic, Gordana. Yugoslavia. Naucno-Teh. Pregl. (1989), 39(7), 35-9. CODEN: NPGLA7 ISSN: 0350-0667. Journal written in SerboCroatian. CAN 112:219919 AN 1990:219919 CAPLUS (Copyright 2002 ACS)

Abstract

A procedure is developed for making cast composite explosives by using hexogen of various granularities and polyurethane binders. Composites having porosity less than 1% and detonation rate greater than 7900 m/s are obtained. According to their mech. properties, these composites are classed as elastic materials, and some of them have rubberlike elasticity. Their sensitivity to shock-wave initiation is equiv. to that of Hexolite 60/40.

Bibliographic Information

Exploratory development on a new process to produce improved RDX (cyclotrimethylenetrinitramine) crystals: supercritical fluid anti-solvent recrystallization. Krukonis, V. J.; Coffey, M. P.; Gallagher, P. M. Army Ballistic Res. Lab., Aberdeen Proving Ground, MD, USA. Avail. NTIS. Report (1988), (BRL-CR-606; Order No. AD-A207760), 74 pp. From: Gov. Rep. Announce. Index (U. S.) 1989, 89(18), Abstr. No. 949,990. Report written in English. CAN 112:121706 AN 1990:121706 CAPLUS (Copyright 2002 ACS)

Abstract

To prep. intragranular-cavity-free RDX crystals (100-150m), supercrit. fluids are used as antisolvents in recrystn. from org. solvents. The concept is based on the phenomenon of absorption of gas near its crit. point by an org. solvent. The absorption of the gas lowers the dissolving power of the org. solvent for RDX resulting in nucleation of RDX. Process parameters such as RDX concn., org. solvent, gas pressure and temp., rate of introduction of gas, and similar factors can be controlled.

Bibliographic Information

N-nitration using ammonium nitrate-trifluoroacetic anhydride. Suri, S. C. Res. Inst., Dayton Univ., Dayton, OH, USA. Avail. NTIS. Report (1988), (UDR-TR-88-62, AFAL-TR-88-079; Order No. AD-A202294), 33 pp. From: Gov. Rep. Announce. Index (U. S.) 1989, 89(9), Abstr. No. 921,531. Report written in English. CAN 112:121693 AN 1990:121693 CAPLUS (Copyright 2002 ACS)

Abstract

In relation to the synthesis of advanced propellant ingredients of a propulsion system, esp. the synthesis of known nitramines and nitramides by existing and new methodol., 1-nitropyrrolidine (I), 1-nitrosuccinimide (II), 1,3-dinitro-2-imidazolidone (I), and 1-nitrohydantoin (IV) were prepd. according to literature and modified procedures by using 100% HNO3 and (CF3CO)2O mixt. Similarly, NH4NO3-(CF3CO)2O can be used for N-nitration and the syntheses of I, II, III, IV, 1-nitro-2-pyrrolidone, and 1-acetyl-3,4-dinitrohexahydro-1,3,5-triazine (V) were so done. In V synthesis from 1,3,5-triacetoxyhexahydrotriazine, a small quantity of RDX was obtained. 1-Acetylsuccinimide and parabanic acid did not undergo nitration under these conditions. This method provides N-nitrated products comparable to those from conventional, but less convenient or safe, nitrating reagents.

Bibliographic Information

Kinetic studies of the pH dependence of the decomposition of 3,7-dinitro-1,3,5,7-tetraazabicyclo[3.3.1]nonane (DPT) and related compounds. Cooney, Aidan P.; Crampton, Michael R.; Scranage, John K.; Golding, Peter. Chem. Dep., Durham Univ., Durham, UK. J. Chem. Soc., Perkin Trans. 2 (1989), (1), 77-81. CODEN: JCPKBH ISSN: 0300-9580. Journal written in English. CAN 111:6745 AN 1989:406745 CAPLUS (Copyright 2002 ACS)

Abstract

Kinetic studies are reported of the pH-dependence of the decompn. of the title compd. I in aq. media. For comparison, data were also obtained for reaction of methylenedinitroamine (MDNA) and nitramide (NH2NO2) which are potential intermediates on the reaction path of I. The results, while not providing a complete description of the decompn. of I, show that at all acidities two stages are obsd. The first stage, K1, involves catalysis by protons and hydroxide ions and it is suggested that reaction occurs via a low-concn., ring-opened structure which is in equil. with I. In acidic soln. an intermediate is obsd. which is identified as nitramide; in basic soln. a different intermediate is formed. MDNA is not an intermediate in the I reaction since its rate of decompn. is too slow.


Bibliographic Information

A convenient method for N-nitration using ammonium nitrate-trifluoroacetic anhydride. Suri, Suresh Chander; Chapman, Robert D. Res. Inst., Univ. Dayton, Edwards Air Force Base, CA, USA. Synthesis (1988), (9), 743-5. CODEN: SYNTBF ISSN: 0039-7881. Journal written in English. CAN 110:192709 AN 1989:192709 CAPLUS (Copyright 2002 ACS)

Abstract

Nitramines, nitramides, and nitrimides are prepd. by reaction of the appropriate heterocyclic precursors with NH4NO3-(CF3CO)2O. Yields are comparable to those from conventional but less safe nitrating agents. Thus, reaction of 2-imidazolidone with NH4NO3-(CF3CO)2O gives 41% 1,3-dinitro-2-oxotetrahydroimidazole. Hydantoin gives 20% 1-nitrohydantoin.

Bibliographic Information

Nitramine explosive manufacture as large crystals. Svensson, Leif; Ericsson, Per; Olsson, Nils Ingvar; Bergstroem, Bertil. (Nobel Kemi AB, Swed.). Eur. Pat. Appl. (1988), 8 pp. CODEN: EPXXDW EP 288122 A2 19881026 Designated States R: AT, BE, CH, DE, ES, FR, GB, GR, IT, LI, NL, SE. Patent written in English. Application: EP 88-200732 19880415. Priority: SE 87-1643 19870422; SE 87-1644 19870422. CAN 110:60614 AN 1989:60614 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
EP 288122 A2 19881026 EP 1988-200732 19880415
EP 288122 A3 19890315
EP 288122 B1 19930224
R: AT, BE, CH, DE, ES, FR, GB, GR, IT, LI, NL, SE
SE 8701643 A 19881023 SE 1987-1643 19870422
SE 462715 B 19900820
SE 462715 C 19911031
SE 8701644 A 19881023 SE 1987-1644 19870422
SE 460416 B 19891009
SE 460416 C 19900208
AT 85970 E 19930315 AT 1988-200732 19880415
ES 2053705 T3 19940801 ES 1988-200732 19880415
US 4900819 A 19900213 US 1988-184131 19880421
CA 1296723 A1 19920303 CA 1988-564652 19880421

Priority Application Information
SE 1987-1643 19870422
SE 1987-1644 19870422
EP 1988-200732 19880415

Abstract

RDX and HMX prepd. by hexamethylenetetramine (I) nitration with NH4NO3, Ac2O, and AcOH by the Backmann process are obtained as large crystals by subjecting the explosive crystal-contg. AcOH acidic mother liquor, after completion of the reaction but before filtering, to a controlled heat and pressure schedule in a closed vessel. First, the mother liquor is heated to 90-200°, e.g., £170° and preferably 110-130°, under £5 bar for 15 min-2 h, then the temp. is decreased to 60-110° and the pressure to normal atm. pressure, the resulting crystals, almost entirely HMX, are sepd. by thermal filtering, the temp. is reduced to room temp., and the resulting HMX and RDX are filtered. The large crystals are easily filtered, and their considerably small surface area leads to decreased contamination of the working liqs. and recrystn. agents. In the conventional HMX synthesis starting with 16 g I, following completion of the reaction and a 2-h after-reaction, 50 mL water was added, the temp. was increased to 120° and held for 1 h during which the pressure increased to 2.4 atm, the mixt. was filtered, the product was washed with water, and the mother liquor was cooled to room temp. and filtered again. The 1st fraction 21.5 g consisted of 0.3% RDX and balance HMX. The 2nd fraction 8.4 g consisted of 48 HMX and 52% RDX.

Bibliographic Information

Preparation of 1,3,5-trinitro-1,3,5-triazacyclohexane. Dimun, Milan; Truchlik, Stefan; Kabatova, Viera; Zeman, Svatopluk. (Czech.). Czech. (1987), 3 pp. CODEN: CZXXA9 CS 235559 B1 19870215 Patent written in Slovak. Application: CS 83-4167 19830609. CAN 109:190456 AN 1988:590456 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
CS 235559 B1 19850515 CS 1983-4167 19830609

Abstract

The yield of the title compd. (I), produced by nitrolysis of hexamethylenetetramine (II), and the safety of the process, increased significantly in the presence of urea nitrate (III). Thus, treating 710 parts 96.1% HNO3 at 15-17° with 100 parts II contg. 0.7-1% III, stirring the mixt. 20 min at 18-19°, pouring it into 3000 parts H2O at 55-60°, and filtering the sepd. product gave 74.2-74.8% I, vs. 70.2% obtained in the absence of III.

Bibliographic Information

Synthesis of 1,3,5-trinitro-1,3,5-triazacyclohexane. Fischer, John W.; Atkins, Ronald L. (United States Dept. of the Navy, USA). Statutory Invent. Regist. (1988), 2 pp. CODEN: SRXXEV US 447 H1 19880301 Patent written in English. Application: US 87-24437 19870311. CAN 109:110459 AN 1988:510459 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
US 447 H1 19880301 US 1987-24437 19870311

Abstract

The title compd. (I) was prepd. by treatment of hexamethylenetetramine (II) with N2O5 (preferably .apprx.25% by wt.) in 100% HNO3, preferably at -20° under a sep. CCl4 phase. Thus, 0.5 g II was added over 5 min to 36 mL of 25% N2O5 in 100% HNO3 at -20°. The mixt. was stirred 30 min to give 57% I, free of 1,3,5,7-tetraaza-1,3,5,7-tetranitrocyclooctane.

Bibliographic Information

Examples of the application of titration techniques in the process industry. Asplund, Jan. Nobel Chem. AB, Karlskoga, Swed. Anal. Chim. Acta (1988), 206(1-2), 137-52. CODEN: ACACAM ISSN: 0003-2670. Journal written in English. CAN 109:85468 AN 1988:485468 CAPLUS (Copyright 2002 ACS)

Abstract

Different titrn. techniques are used for analyses of the nitrating acids in three different industrial processes, namely in the prodn. of glycerol trinitrate (nitrate ester, CONO2), trinitrotoluene (nitro groups, CNO2) and trimethylene trinitramine (nitramine, NNO2). The detn. of the compn. of the process acids, which consist mainly of water, nitric acid, sulfuric acid, acetic acid and hexamethylenetetramine with minor amts. of nitrous acid and ammonium nitrate, are complicated by the ability of the process acids to dissolve the product to various extents. Acid-base titrns. as well as oxidn.-redn. titrns. and voltammetry are used to provide a rapid system for analyzing the process acids.

Bibliographic Information

Process for RDX manufacture. Zeman, Svatopluk; Dimun, Milan; Truchlik, Stefan; Kabatova, Viera. (Czech.). Czech. (1987), 3 pp. CODEN: CZXXA9 CS 235560 B1 19870215 Patent written in Slovak. Application: CS 83-4168 19830609. CAN 108:78258 AN 1988:78258 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
CS 235560 B1 19850515 CS 1983-4168 19830609

Abstract

Nitrolysis of hexamethylenetetramine (I) in the presence of 0.7-1% dicyan diamide (II) gives RDX in 72.5-72.8% yield and increased purity. A mixt. of I and II was added with stirring to a .apprx.7-fold excess of 96.1% HNO3 at 9-17°, kept 25 min, poured into water at 55-60°, stirred, filtered, and dried for 3 h at 90°.

Bibliographic Information

Solvent-free preparation of gun propellant formulations. Kristofferson, Clifford E.; Fisher, Donald G.; Bell, Frank H.; Wagner, William F. (Morton Thiokol, Inc., USA). U.S. (1987), 5 pp. CODEN: USXXAM US 4650617 A 19870317 Patent written in English. Application: US 85-748889 19850626. CAN 107:61572 AN 1987:461572 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
US 4650617 A 19870317 US 1985-748889 19850626

Abstract

A solventless method for the prepn. and storage of uncured low vulnerability ammunition propellant (LOVA) includes blending about 60-80 wt.% of either HMX or RDX oxidizer having a wt. mean diam. of 1.0-14 m with a polyurethane binder. A cure-effecting amt. of cure catalyst may also be included. These ingredients are blended at a .ltorsim.110° F., deaired, and optionally stored at low temps. at a pre-cured condition, extruded, and subsequently cured. The products produced thereby have uniquely low burning rates as well as uniquely low burning rate exponents. Thus, Pluronic L-35 11.7, trimethylolpropane 3.13, isophorone diisocyanate 10.10, HMX (wt. mean diam. 2.3-2.8 m or 2.8 m ratio by blending) 75.00, and titanyl acetylacetonate 0.0125 wt.% were blended by a detailed process to give an uncured propellant mixt. which was packaged in polyethylene film bags and stored 2 mo at -50°F. The mixts. were thawed, extruded, and cured to give LOVA with d. 0.064 lb/in.3, burning rate 0.652 in./s at 10,000 psi and 70°F, and burning rate exponent 1.014. When the temp. of the frozen mixts. was elevated just sufficiently to allow extrusion the resp. properties of the cured LOVA were 0.0615 lb/in.3, 0.714 in./s, and 0.939.

Bibliographic Information

Direct preparation of 1,3,5-triaza-1,3,5-trinitrocyclohexane from hexamethylenetetramine. Fischer, John W.; Atkins, Ronald L. Res. Dep., Nav. Weapons Cent., China Lake, CA, USA. Org. Prep. Proced. Int. (1986), 18(4), 281-3. CODEN: OPPIAK ISSN: 0030-4948. Journal written in English. CAN 106:196402 AN 1987:196402 CAPLUS (Copyright 2002 ACS)

Abstract

Title compd. (I) was prepd. in 57% yield by the nitration of hexamethylenetetramine with N2O5 in HNO3.


Bibliographic Information

1,3,5-Trinitro-1,3,5-triazacyclohexane. Zeman, Svatopluk; Dimun, Milan; Fedak, Jan. (Czech.). Czech. (1986), 5 pp. CODEN: CZXXA9 CS 227905 B 19860515 Patent written in Slovak. Application: CS 80-3304 19800513. CAN 106:35610 AN 1987:35610 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
CS 227905 B 19840514 CS 1980-3304 19800513
CS 227905 B1 19840416

Abstract

The yield and safety of nitration cleavage of hexamethylenetetramine (I) to the title compd. (II), increased significantly in the presence of a polymethylene-urea condensate. Thus, a soln. of I 14 in 98.9% AcOH 23 and a soln. of NH4NO3 25 in 99.19% HNO3 25 were simultaneously fed at 50-55° in 10-12 min into Ac2O contg. a foamed urea-formaldehyde condensate 0.5 parts. The mixt. was stirred 30 min at 70-75°, dild. with 250 parts hot water, refluxed 30 min, cooled, filtered, the cake was washed with water, 5% NH4OH, and water, and dried to give 69.7% II contg. 10.7% 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane. The comparative yield of tech. grade II of approx. the same compn. was 46% in the absence of the condensate.

Bibliographic Information

1,3,5-Trinitro-1,3,5-triazacyclohexane by nitrolysis of hexamethylentetramine. Zeman, Svatopluk; Dimun, Milan. (Czech.). Czech. (1986), 4 pp. CODEN: CZXXA9 CS 227915 B 19860515 Patent written in Slovak. Application: CS 81-6007 19810810. CAN 106:35609 AN 1987:35609 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
CS 227915 B 19840514 CS 1981-6007 19810810

Abstract

The yield and safety of the title process is increased significantly in the presence of tetrahydroimidazo(4,5-d)imidazole-2,5(1H,3H)-dione (I). Thus, 71 mL 97% HNO3 was stirred at 18-20° with addn. of 10 g hexamethylenetetramine contg. 1% I, the mixt. was kept addnl. 30 min at 22-24°, poured into 300 mL hot water, the suspension was filtered, and the product was washed and dried at 80° to give 75.16% 1,3,5-trinitro-1,3,5-triazacyclohexane vs. 72.56% obtained in the absence of I.

Bibliographic Information

Preparation of monocyclic nitramines. Zeman, Svatopluk; Dimun, Milan. (Czech.). Czech. (1986), 8 pp. CODEN: CZXXA9 CS 227911 B 19860515 Patent written in Slovak. Application: CS 80-5905 19800829. CAN 106:35607 AN 1987:35607 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
CS 227911 B 19840514 CS 1980-5905 19800829

Abstract

A mixt. of octogen (I) and hexogen (II, prevailing component) is prepd. by nitrolysis of hexamethylenetetramine (III) in AcOH in the presence of a urea-formaldehyde condensate (UFC) which increases the safety of the process. Thus, a mixt. of 75 mL AcOH, 1.5 mL Ac2O, and 1.7 g paraformaldehyde was treated at 41-44° in 15-17 min simultaneously with a soln. of 8.7 g NH4NO3 in 6.3 mL HNO3 and a soln. of 10.1 g III in 16 mL AcOH contg. (A) 0.38% UFC, (B) 1.06% UFC (based on III), and (c) no UFC. The mixt. was stirred 15 min at 45-47° with addn. of 6 mL Ac2O, treated with addnl. 44.5 mL Ac2O and 13.2 g NH4NO3 in 9.6 mL HNO3, kept 60 min, dild. with 35 mL hot water, refluxed 30 min, and dild. with cold water. The product was filtered and washed with aq. NH4OH and water. The I content in the dry product and the yields of I and II, based on III, were: 72.38, 25.91, and 13.19 for A, 75.04, 29.17, and 12.97 for B, and 71.9%, 24.31%, and 12.64% for C.

Bibliographic Information

1,3,5-Trinitro-1,3,5-triazacyclohexane by nitrolysis of hexamethylenetetramine. Zeman, Svatopluk; Dimun, Milan. (Czech.). Czech. (1986), 6 pp. CODEN: CZXXA9 CS 227906 B 19860515 Patent written in Slovak. Application: CS 80-3632 19800523. CAN 106:35606 AN 1987:35606 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
CS 227906 B 19840514 CS 1980-3632 19800523

Abstract

The yield and safety of the title process increases significantly in the presence of urea, guanidine, or a fatty acid amide. Thus, treating Ac2O 60 at 50-55° simultaneously with a soln. of hexamethylenetetramine (I) 14 in AcOH 23 and a soln. of NH4NO3 25 in HNO3 18, heating the mixt. 30 min at 70-75°, dilg. with water 250 parts, refluxing 30 min, washing and drying as usual gave 46% tech. grade 1,3,5-trinitro-1,3,5-triazacyclohexane (II), based on I. The II yields increased to 56.8% and 59.5% in parallel runs in which the Ac2O batch contained 0.5 and 1 part urea, resp.

Bibliographic Information

1,3,5-Trinitro-1,3,5-triazacyclohexane. Zeman, Svatopluk; Dimun, Milan. (Czech.). Czech. (1986), 10 pp. CODEN: CZXXA9 CS 227903 B 19860515 Patent written in Slovak. Application: CS 79-7398 19791031. CAN 106:20709 AN 1987:20709 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
CS 227903 B 19840514 CS 1979-7398 19791031

Abstract

Nitrolysis of hexamethylenetetramine (I) yielding the title compd. (II), was facilitated and the safety of the process was increased when I was stabilized with an insol. urea-formaldehyde condensation product (III). Thus, treating 115 parts 96.9% HNO3 at 25-28° with 15 parts I contg. 5% III, stirring the mixt. 40 min, and pouring into excess H2O gave 75.66% II, vs. 74.02% obtained in the absence of III.

Bibliographic Information

Composite explosives. Jessop, Harvey A.; Abegg, Taylor M.; Peterson, John A.; Butler, Jay W.; McCormick, Ronald F. (Megabar Explosives Corp., USA). Eur. Pat. Appl. (1985), 26 pp. CODEN: EPXXDW EP 152060 A1 19850821 Designated States R: AT, BE, CH, DE, FR, GB, IT, LI, LU, NL, SE. Patent written in English. Application: EP 85-101262 19850207. Priority: US 84-578177 19840208. CAN 104:21509 AN 1986:21509 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
EP 152060 A1 19850821 EP 1985-101262 19850207
R: AT, BE, CH, DE, FR, GB, IT, LI, LU, NL, SE
US 4600450 A 19860715 US 1984-578177 19840208
AU 8537667 A1 19850815 AU 1985-37667 19850115
AU 569601 B2 19880211
IN 162619 A 19880618 IN 1985-CA51 19850128
IL 74178 A1 19900712 IL 1985-74178 19850128
ZA 8500766 A 19851030 ZA 1985-766 19850131
JP 60200886 A2 19851011 JP 1985-16725 19850201
ES 540136 A1 19870716 ES 1985-540136 19850205
NO 8500445 A 19850809 NO 1985-445 19850206
NO 162611 B 19891016
NO 162611 C 19900124
BR 8500528 A 19850924 BR 1985-528 19850206
CA 1230489 A1 19871222 CA 1985-473660 19850206
DK 8500571 A 19850809 DK 1985-571 19850207
FI 8500515 A 19850809 FI 1985-515 19850207

Priority Application Information
US 1984-578177 19840208

Abstract

Microknit explosive (MCX) compns. with microcryst. property, capable of being machined, and useful as explosives, propellants, and gas generators are prepd. by (1) dissolving surfactants, crystal-habit modifiers, and/or thickeners into a molten oxidizer in a manner which permits supercooling with subsequent solidification, (2) forming an unstable oil-continuous emulsion followed by controlled disruption of the oil-phase continuum which causes solidification after the supercooling, or (3) retarding crystal nucleation in salt-continuous emulsions by introducing surfactants, thickeners, and/or crystal-habit modifiers, along with fuels, resulting in supercooling and solidification to hard compns. These compns. are water-resistant, have excellent explosive and phys. properties, permit a wide range of useful components, and permit const. processing, cooling, optional admixing of additives, loading, and packaging before solidification. Thus, 8 parts Na dodecylbenzenesulfonate and 4 parts Na dimethylnaphthalenesulfonic acid were dissolved at 140° into an oxidizer comprising NH4NO3 68.4, NaNO3 9.8, and KClO4 9.8 parts. This mixt. supercooled before solidification, allowing the addn. of 50.1 parts RDX at temps. typical of military explosives manuf. The compn. had d. 1.65 g/cm3 and, as a 5.0 cm-diam. charge, it failed to detonate at 5° with a no. 8 cap but was detonated by a 15 g tetryl booster. The compns. and detonation results are given for 31 addnl. MCX compns. covering the 3 prepn. procedures cited above.

Bibliographic Information

Reversed-phase gradient high-performance liquid chromatography of nitramine munitions and characterization of munitions process samples by gas chromatography-mass spectrometry. Burrows, Elizabeth P.; Brueggemann, Ernst E. U.S. Army Med. Bioeng. Res. Dev. Lab., Frederick, MD, USA. J. Chromatogr. (1985), 329(2), 285-9. CODEN: JOCRAM ISSN: 0021-9673. Journal written in English. CAN 103:180352 AN 1985:580352 CAPLUS (Copyright 2002 ACS)

Abstract

A reversed-phase, gradient-elution method is presented for the quant. detn. of RDX [121-82-4], HMX [2691-41-0], TAX [14168-42-4], and SEX [13980-00-2] in samples from the DMSO [67-68-5] munitions recrystn. process. The samples also were extd. and analyzed qual. by gas chromatog. and mass spectroscopy. The nitramines were eluted by a linear gradient produced from 1:4 (A) and 4:1 (B) MeOH-H2O and the compn. was changed from A:B 95:5 to A:B 50:50 in 25 min at a flow rate of 1.2 mL/min. The samples were composites from the RDX and HMX processes obtained at several stages in the munitions recrystn. and DMSO recovery. Typical results are tabulated and given graphically for the munitions and trace orgs. Water of the Holston River at Kingsport, Tenn., was analyzed for trace orgs.

Bibliographic Information

Determination of the explosive charge structure by metallographic methods. Rosendorfer, T. MBB, Schrobenhausen, Fed. Rep. Ger. Int. Jahrestag. - Fraunhofer-Inst. Treib- Explosivst. (1984), (Technol. Treib-Sprengm.), 671-82. CODEN: IFTEDV ISSN: 0722-4087. Journal written in German. CAN 103:89874 AN 1985:489874 CAPLUS (Copyright 2002 ACS)

Abstract

Metallog. methods are proposed for the deformation-free prepn. of polished microsections of explosive charges with an ultramilling machine and detn. of the structure or explosive charges. The methods were applied for cast TNT [118-96-7]-hexogen [121-82-4] charges and for pressed charges of hexogen 94, wax 5, and graphite 1%. The effect of compacting pressure on the d., structure, and crystal grain fracture is shown. Conclusions are made for safety limits in the prepn. of pressed explosive charges.

Bibliographic Information

Microcolumn clean-up and recovery techniques for organic explosives compounds and for propellants traces in firearms discharge residues. Lloyd, J. B. F. Home Off. Forensic Sci. Lab., Birmingham, UK. J. Chromatogr. (1985), 330(1), 121-9. CODEN: JOCRAM ISSN: 0021-9673. Journal written in English. CAN 103:82867 AN 1985:482867 CAPLUS (Copyright 2002 ACS)

Abstract

Microcolumn recovery and clean-up procedures suitable for use with a variety of adsorbents of explosive compds. are described. The procedures employ 1 mm I.D. columns that are charged and eluted by the use of the sample loop of a valve injector as a solvent reservoir. Some examples are given of the recovery of nitroglycerin [55-63-0] from firearms discharge residues in clothing exts. and from explosion debris.

Bibliographic Information

Mixtures of cyclic nitramines mostly composed of 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane. Zeman, Svatopluk; Dimun, Milan. (Czech.). Czech. (1984), 4 pp. CODEN: CZXXA9 CS 213509 B 19840301 Patent written in Slovak. Application: CS 80-6163 19800911. CAN 101:211192 AN 1984:611192 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
CS 213509 B 19820409 CS 1980-6163 19800911

Abstract

Nitrolysis of hexamethylenetetramine with a soln. of NH4NO3 in HNO3 in a medium contg. AcOH, Ac2O, and paraformaldehyde gave in the presence of urea a product contg. 80.22% of the title compd. (I). The yields of I and 1,3,5-trinitro-1,3,5-triazacyclohexane were 57.75% and 18.99%, resp. Comparative values obtained in the absence of urea were 73.06, 47.87, and 23.54%, resp.

Bibliographic Information

Cyclic nitramines mixture with majority content of 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane. Zeman, Svatopluk; Dimun, Milan. (Czech.). Czech. (1984), 4 pp. CODEN: CZXXA9 CS 214311 B 19840601 Patent written in Slovak. Application: CS 80-7389 19801103. CAN 101:191980 AN 1984:591980 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
CS 214311 B 19820409 CS 1980-7389 19801103

Abstract

Nitration cleavage of hexamethylenetetramine (I) gives in the presence of urea and a urea-formaldehyde condensate an increased utilization of I in favor of the title compd. [II; X = CH2N(NO2)CH2] which is the explosive octogen. Thus, treating I in AcOH at 43-7° with a soln. of NH4NO3 in HNO3 in the presence of Ac2O and the above additives gave 52.35% octogen and 22.58% hexogen (II, R = CH2). Utilization of I was 48.05% vs. 45.43% obtained in the absence of urea and the urea formaldehyde condensate.


Bibliographic Information

Low burning rate aluminized propellants in acceleration fields. Brundige, Winston N.; Caveny, Leonard H. Morton Thiokol/Elkton, MD, USA. AIAA J. (1984), 22(5), 638-46. CODEN: AIAJAH ISSN: 0001-1452. Journal written in English. CAN 101:75282 AN 1984:475282 CAPLUS (Copyright 2002 ACS)

Abstract

To reduce slag formation and burning rate increases, the effects of radial acceleration (up to 20 g) and low pressure (2-7 MPa) on the combustion of low-burning rate aluminized propellants (87 formulations) were investigated. Expts. were performed to obtain agglomerate size distribution, slag formation, and burning rate data. Data sources included photographs under cross flow and acceleration conditions, scanning electron probe (Cl and Al) images, particle collection combustors, and rocket motors. The tendency to form slag increases as the agglomeration size at the burning surface increases. A lower burning rate increases acceleration effects. However, residue formation is more sensitive to formulation than is burning rate; for example, bimodal vs. trimodal NH4ClO4 can cause significant changes in residue in the absence of burn rate changes; RDX [121-82-4] produces larger agglomerates than HMX [2691-41-0]. Through understanding obtained from this research, redn. in agglomeration, slag formation, and burning rate augmentation are directly attributable to systematic changes in formulation ingredient levels and sizes.

Bibliographic Information

Organometallics in high energy chemistry. Laine, R. M.; Levins, D. A.; Bedford, C. D. SRI Int., Menlo Park, CA, USA. Avail. NTIS. Report (1983), (ARO-18084.5-CH; Order No. AD-A135715), 109 pp. From: Gov. Rep. Announce. Index (U. S.) 1984, 84(6), 160. Report written in English. CAN 101:57280 AN 1984:457280 CAPLUS (Copyright 2002 ACS)

Abstract

New synthetic strategies were developed for the synthesis of polymethyleneimine precursors to RDX [121-82-4] and HMX [2691-41-0] through the use of homogeneous catalysts based on Ru and Ru-Fe mixts. These catalysts have proved effective for the oligomerization and cyclization of tertiary diaminoalkanes at temps. and rates superior to the heterogeneous Pd black-catalyzed reactions previously reported. Under somewhat different conditions, these same catalysts will cleave reform Si-N bonds. Activation of Si-N bonds is useful in several org. syntheses. In an effort to understand why Pd black is less effective than the homogeneous catalysts, an understanding of how Lindlar catalysts function was developed. In addn., a comprehensive picture of how other heterogeneous catalysts esp. hydrodenitrogenation catalysts interact with N-contg. orgs. was developed. In unrelated studies, synthetic methods for prepg. nitro-alkoxyaluminates with the objective of developing air and moisture stable high energy organometallics were explored. For b-nitro alkoxy aluminates, air and moisture sensitivity decreases significantly with increasing nos. of b-nitro groups.

Bibliographic Information

A hexahydro-1,3,5-trinitro-1,3,5-triazine (RDX): e-caprolactone adduct. Selig, W.; Bruenner, R. S.; Price, H. A. Lawrence Livermore Natl. Lab., Univ. California, Livermore, CA, USA. Propellants, Explos., Pyrotech. (1983), 8(3), 83-4. CODEN: PEPYD5 ISSN: 0721-3115. Journal written in English. CAN 99:139909 AN 1983:539909 CAPLUS (Copyright 2002 ACS)

Abstract

An unstable equimol. adduct of hexahydro-1,3,5-trinitro-S-triazine (RDX) was prepd. from caprolactone I by dissolving 100 mg of RDX in a min. amt. of I.


Bibliographic Information

Polymer binding of explosives via radiation curing. Iyer, S. U. S. Army Armament Res. Dev. Command, Dover, NJ, USA. Int. Jahrestag. - Fraunhofer-Inst. Treib- Explosivst. (1981), (Chem. Mech. Technol. Treib-Explosivst.), 321-31. CODEN: IFTEDV Journal written in English. CAN 97:130022 AN 1982:530022 CAPLUS (Copyright 2002 ACS)

Abstract

RDX [121-82-4]-Contg. compns. bonded by poly(Me methacrylate) [9011-14-7] and poly(trimethylolpropane trimethacrylate) [26426-04-0] were prepd. by in-situ polymn. by irradn. with x-rays or g-rays and were characterized. Microscopic study of the cured RDX-poly(Me methacrylate) composite showed that the freshly cut surface was free from macroscopic defects. Significant potential exists for this method to be applied to direct in-situ curing of cast charges of complex shapes in military hardware.

Bibliographic Information

Complex formation in RDX, HMX, TNT, and some related compounds: a bibliography. Abel, J. E.; Marinkas, P. L.; Bulusu, S. Large Caliber Weapon Syst. Lab., U.S. Army Armaments Res. Dev. Command, Dover, NJ, USA. J. Ballist. (1981), 5(3), 1195-216. CODEN: BALLD2 ISSN: 0146-4140. Journal; General Review written in English. CAN 96:165013 AN 1982:165013 CAPLUS (Copyright 2002 ACS)

Abstract

A review, with 35 refs., of complex synthesis and complexing of RDX, HMX, TNT, and related nitramines and nitroaroms. used in formulating explosives and propellants.

Bibliographic Information

Rotating biological contractors for munitions wastewater treatment. Chesler, P. Gail; Eskelund, Gerald R. Army Mobility Equipment Res. Dev. Command, Fort Belvoir, VA, USA. Avail. NTIS. Report (1981), (MERADCOM-2319; Order No. AD-A100437), 45 pp. From: Gov. Rep. Announce. Index (U. S.) 1981, 81(21), 4599. Report written in English. CAN 96:148371 AN 1982:148371 CAPLUS (Copyright 2002 ACS)

Abstract

The applicability of aerobic rotating biol. contactor (RBC) technol. for secondary treatment of the wastestream of a facility manufg. the explosives RDX [121-82-4] and HMX [2691-41-0] was studied. The synthesized wastestream contained high levels of HCHO [50-00-0] and HCO2H [64-18-6] as well as the explosives RDX, HMX, and TNT [118-96-7]. Several other org. contaminants were also present in lesser concns. The RBC was capable of removing 82% of the COD from the wastestream at loading rates of 2.3 lb of COD/1000 ft2 of disk surface area-day.

Bibliographic Information

Hazards of inadvertent mixing of chemicals used in the Bachmann processes for manufacturing the military explosives RDX and HMX. Leach, James T.; Staples, John M. Holston Def. Corp., Kingsport, TN, USA. J. Hazard. Mater. (1981), 4(3), 271-81. CODEN: JHMAD9 Journal written in English. CAN 96:22013 AN 1982:22013 CAPLUS (Copyright 2002 ACS)

Abstract

A CHETAH diagram and results of reactivity tests performed with both open and closed reactor vessels have contributed significantly to understanding the hazards of inadvertent mixing of Bachmann chem. used in the manuf. of RDX [121-82-4] and HMX [2691-41-0]. When mixed in an unconfined, insulated vessel, certain combinations of Bachmann chem., initially at ambient temps., generate fires spontaneously. Other combinations spontaneously generate explosions when mixed in a closed vessel. The types of test app. and techniques used in this work can be of considerable value throughout the chem. processing industries, particularly when potentially hazardous new processes are being scaled up from bench levels to prodn. levels.

Bibliographic Information

Degradable binder explosives. Lee, Benjamin Y. S.; Reed, Russell, Jr.; Miller, Roger L. (United States Dept. of the Navy, USA). U.S. (1981), 3 pp. CODEN: USXXAM US 4293352 19811006 Patent written in English. Application: US 79-69215 19790823. CAN 95:206333 AN 1981:606333 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
US 4293352 A 19811006 US 1979-69215 19790823

Abstract

Explosives with binders which are easily degraded by dil. mineral acids or aq. NH3 for recovery of the explosive components are prepd. from .apprx.82 explosive solids and .apprx.18 wt.% polyurethane binder prepd. from 16.56 polyester and 1.44 wt.% lysine diisocyanate Me ester (I) [4460-02-0] curative. Thus, an explosive was prepd. from RDX [121-82-4](Classes 1, 3, 4, and 5) 82.00, Witco YA 23-4 polyester 16.56, I 1.44, and Ph3Bi catalyst 0.02 wt.%. The binder does not degrade in contact with water but is degraded by dil. H2SO4 or NH4OH for RDX recovery when the compn. has become obsolete.

Bibliographic Information

Nitration of products of the condensation of monoethanolamine and formaldehyde in the presence of ammonium nitrate. Gafarov, A. N.; Punegova, L. N.; Marchenko, G. A.; Novikov, S. S. USSR. Zh. Org. Khim. (1981), 17(4), 716-18. CODEN: ZORKAE ISSN: 0514-7492. Journal written in Russian. CAN 95:203889 AN 1981:603889 CAPLUS (Copyright 2002 ACS)

Abstract

Nitration of H2NCH2CH2OH-CH2O condensation products, e.g., I (R = CH2CH2OH), II, and urotropine, by HNO3-Ac2O in presence of NH4NO3 gave mixts. of 3 identical products, viz., I (R = NO2), AcOCH2CH2N(NO2)CH2CH2ONO2, and AcOCH2N(NO2)CH2N(NO2)CH2N(NO2)CH2CH2ONO2.


Bibliographic Information

A study on the synthesis of 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane. Kang, J. B.; Koo, B. T.; Lee, S. K.; Lee, K. H.; Oh, D. Y. Hongneung Mach. Ind. Corp., Seoul, S. Korea. Taehan Hwahakhoe Chi (1980), 24(4), 322-8. CODEN: DHWHAB ISSN: 0418-2472. Journal written in Korean. CAN 95:97755 AN 1981:497755 CAPLUS (Copyright 2002 ACS)

Abstract

In nitration of hexamethylenetetramine (I) to prep. homocyclonite (II) and cyclonite (III), the dinitro compd. IV was the intermediate.


Bibliographic Information

Biological treatment for waste streams from propellants and explosives manufacturing. Smith, L. L.; Carrazza, J.; Wong, K. Radford Army Ammunition Plant, Hercules Inc., Radford, VA, USA. Editor(s): Bartron, Lester R. Pap. Jt. Symp. Compat. Plast./Mater. Explos. Process. Explos. (1980), 29-48. Publisher: Am. Def. Prep. Assoc., Arlington, Va CODEN: 45LGAQ Conference written in English. CAN 95:67359 AN 1981:467359 CAPLUS (Copyright 2002 ACS)

Abstract

Three pilot studies were conducted on each of the streams from army ammunition plants at Holston and Radford, and a simulated stream for a new facility being considered for the prodn. of RDX [121-82-4]/HMX [2691-41-0]. Both the activated sludge system and the rotating biol. contactor system were investigated. Both systems show a high degree of BOD removal. Each exhibited certain advantages. In both systems carbon columns are needed to remove the nonbiodegradable contaminates from the streams. An optimum treatment approach may be a hybrid system.

Bibliographic Information

Preparation and purification of HMX and RDX intermediates (TAX and SEX). Bedford, Clifford D.; Staats, Steven J.; Geigel, Maria A.; Ross, Donald L. Org. Chem. Dep., SRI Int., Menlo Park, CA, USA. Avail. NTIS. Report (1980), (Order No. AD-A089613), 34 pp. From: Gov. Rep. Announce. Index (U. S.) 1981, 81(2), 280. Report written in English. CAN 95:7242 AN 1981:407242 CAPLUS (Copyright 2002 ACS)

Abstract

1-Acetylhexahydro-3,5-dinitro-1,3,5-triazine (TAX) and 1-acetyloctahydro-3,5,7-trinitro-1,3,5,7-tetrazocine (SEX) were prepd. TAX was prepd. by nitration of 1,3,5-triacetylhexahydro-1,3,5-triazine by (F3CCO)2O and 100% HNO3 followed by column chromatog. on silica gel. SEX was prepd. similarly from 1,5-diacetyloctahydro-3,7-dinitro-1,3,5,7-tetrazoxine (DADN), but was contaminated by 20% DADN.

Bibliographic Information

Pilot-scale evaluation of the treatability of RDX/HMX site 'X' facility wastewaters. Kitchens, Judith F.; Hyde, Raymond G.; Price, Debra A.; Hyde, Kenneth S.; Jones, William E., III. At. Res. Corp., Alexandria, VA, USA. Avail. NTIS. Report (1980), (ARC-49-5766-1, ARCSL-CR-80028, AD-E410 256; Order No. AD-A084 657), 185 pp. From: Gov. Rep. Announce. Index (U. S.) 1980, 80(18), 3682. Report written in English. CAN 94:162134 AN 1981:162134 CAPLUS (Copyright 2002 ACS)

Abstract

In this program, the feasibility of treating the wastewaters from the Site X RDX [121-82-4]/HMX [2691-41-0] manufg. facilities in aerobic rotating biol. contactors (RBC) was evaluated. These wastewaters contain explosives such as RDX, HMX, and TNT [118-96-7]; HCHO [50-00-0]; HCO2H [64-18-6]; AcOH [64-19-7]; and solvents such as cyclohexanone [108-94-1] and Me2CO [67-64-1]. A pilot scale RBC was used in this investigation. The results from the pilot-scale evaluation indicate that 95-100% sol. BOD removal can be achieved and maintained at sol. BOD loading rates of less than 2.5 lb/1000 ft3-day.

Bibliographic Information

Gelled slurry explosive. Irwin, William J.; Reed, Russell, Jr.; Silver, Wallace E. (United States Dept. of the Navy, USA). U. S. Pat. Appl. (1980), 9 pp. Avail. NTIS Order No. PAT-APPL-144 483. CODEN: XAXXAV US 144483 19800926 Patent written in English. Application: US 80-144483 19800428. CAN 94:124135 AN 1981:124135 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
US 144483 A0 19800926 US 1980-144483 19800428
US 4324599 A 19820413

Abstract

Explosive gelled slurries consisting entirely of explosives manufg. wastes and obsolete propellants are obtained from red water (from TNT [118-96-7] manuf.) .apprx.35, oxidizers .apprx.10, ground JPN rocket propellant .apprx.46, and passivated or powd. Al flakes .apprx.8.5 by mixing with .apprx.0.5 wt.% thickening agent and gelling as desired with TDI. NaNO3 oxidizer is obtained as a byproduct in RDX [121-82-4] manuf. and the Al is recovered from obsolete explosives. The compns. can be detonated with conventional blasting caps.

Bibliographic Information

Unusual behavior of 1-acetoxy-2,4,6-trinitro-2,4,6-triaza-8-nitroxyoctane in the presence of sulfuric acid. Gafarov, A. N.; Punegova, L. N.; Marchenko, G. A.; Novikov, S. S. USSR. Zh. Org. Khim. (1980), 16(8), 1774-5. CODEN: ZORKAE ISSN: 0514-7492. Journal written in Russian. CAN 94:65633 AN 1981:65633 CAPLUS (Copyright 2002 ACS)

Abstract

Treatment of the title compd. with 88% H2SO4 at 0° for 30 min gave 73% trinitrotriazacyclohexane I; increasing the temp. to 5° increased the yield of I to 86%.


Bibliographic Information

Be cautious with nitric acid. Bedford, Clifford D. Org. Chem. Dep., SRI Int., Menlo Park, CA, USA. Chem. Eng. News (1980), 58(35), 33, 43. CODEN: CENEAR ISSN: 0009-2347. Journal written in English. CAN 94:52115 AN 1981:52115 CAPLUS (Copyright 2002 ACS)

Abstract

During the prepn. of 1-acetylhexahydro-3,5-dinitro-1,3,5-triazine [14168-42-4], a contaminate formed during the manuf. of RDX [121-82-4], a mixt. consisting of a 3:1 molar ratio of HNO3:1,3-triacetylhexahydro-1,3,5-triazine [26028-46-6] in trifluoroacetic anhydride (5 Mequiv) detonated without warning.

Bibliographic Information

Calorimetry studies of ammonia, nitric acid, and ammonium nitrate. Rewick, R. T.; Gikis, B. J.; Weisman, I. SRI Int., Menlo Park, CA, USA. Avail. NTIS. Report (1979), (ARLCD-CR-79017, AD-E400371; Order No. AD-A078229), 24 pp. From: Gov. Rep. Announce. Index (U. S.) 1980, 80(7), 1214. Report written in English. CAN 93:116720 AN 1980:516720 CAPLUS (Copyright 2002 ACS)

Abstract

Based on calorimetry studies, basic thermochem. data were obtained for the design of the HNO3-NH4NO3 reaction process to be used fo the RDX [121-82-4]-HMX [2691-41-0] X Facility.

Bibliographic Information

New adducts of 1,3,5-trinitro-1,3,5-triazacyclohexane and 1,3,5,7-tetranitro-1,3,5,7-tetrazacyclooctane. Selig, W. Lawrence Livermore Lab., Univ. California, Livermore, CA, USA. Avail. NTIS. Report (1979), (UCRL-82678, CONF-790644-1), 9 pp. From: Energy Res. Abstr. 1979, 4(18), Abstr. No. 47115. Report written in English. CAN 92:198375 AN 1980:198375 CAPLUS (Copyright 2002 ACS)

Abstract

Adducts of the title compds. with hydroxy-1-butanesulfonic acid d-sultone and 2,6-lutidine N-oxide and other pyrimidine N-oxides were prepd.

Bibliographic Information

Phytotoxicity of air pollutants formed by high explosive production. Thompson, C. Ray; Kats, Gerrit; Lennox, Robert W. Statewide Air Pollut. Res. Cent., Univ. California, Riverside, CA, USA. Environ. Sci. Technol. (1979), 13(10), 1263-8. CODEN: ESTHAG ISSN: 0013-936X. Journal written in English. CAN 91:187596 AN 1979:587596 CAPLUS (Copyright 2002 ACS)

Abstract

Six compds. emitted in the manuf. of the explosives TNT (I) [118-96-7] and RDX [121-82-4] were tested for phytotoxicity on 7 species of plants. These compds. were: mixed nitrotoluenes (NT), tetranitromethane (TNM) [509-14-8], nitromethane (NM) [75-52-5], methyl nitrate (MN) [598-58-3], AcOH [64-19-7] and SO2. The plant species tested were wheat, alfalfa, soybean, tobacco, corn, white oak, and scotch pine. The max. dosages used were 10.6-50 mg/m3. White oak and scotch pine showed minimal injury, but wheat, alfalfa, tobacco, soybean, and corn were injured sufficiently with TNM, AcOH, or SO2 to warrant further studies. Minimal or no injury was obsd. on any of the plant species with NM, NT, or MN. TNM was much more toxic than SO2. SO2 was somewhat more toxic than AcOH. The combined effects of SO2 + TNM and SO2 + AcOH were detd. on wheat and alfalfa to find out whether interactions occur.


Bibliographic Information

Recycle of spent acid in nitrolysis of hexamine to RDX. Brumley, Charles D.; Staples, John M. (United States Dept. of the Army, USA). U.S. (1979), 6 pp. CODEN: USXXAM US 4163845 19790807 Patent written in English. Application: US 78-900212 19780426. CAN 91:177536 AN 1979:577536 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
US 4163845 A 19790807 US 1978-900212 19780426

Abstract

The spent acid from hexamine [100-97-0] nitrolysis to RDX [121-82-4] is recycled under conditions which avoid or minimize the need for costly recovery steps and result in little or no decrease in RDX yield. Thus, a hexamine soln. in AcOH and NH4NO3 soln. in HNO3 are combined with excess Ac2O and heated under anhyd. conditions for nitrolysis and formation of RDX and spent acid consisting of AcOH, Ac2O, and HNO3. Water is added to the RDX-acid mixt. to eliminate the Ac2O and give a water content of 0-2%, the RDX is sepd. from the spent acid, and at least part of that acid, contg., HNO3 and 0-2% water, is recycled to dissolve the hexamine.

Bibliographic Information

Application possibilities of molded plastic explosives. Part 1: Composite explosives. Roche, G. Soc. Natl. Poudres Explos., Paris, Fr. Int. Jahrestag. - Inst. Chem. Treib- Explosivst. (1978), (Mod. Technol. Treib- Explosivst.), 235-42. CODEN: IJITDF Journal written in French. CAN 91:93837 AN 1979:493837 CAPLUS (Copyright 2002 ACS)

Abstract

Cast composite explosives, while retaining their excellent detonation properties compared with conventional formulas, offer a no. of obvious advantages: better thermal behavior and phys. and mech. properties, new possibilities in casting techniques, and clearly higher safety. A no. of formulas are now used in industrial developments.

Bibliographic Information

Specific air pollutants from munitions processing and their atmospheric behavior. Volume 1. Executive summary and general appendices. Carpenter, Ben H.; Liepins, Raimond; Sickles, Joseph, II; Hamilton, Harry L.; VanOsdell, Douglas W. Research Triangle Inst., Research Triangle Park, NC, USA. Avail. NTIS. Report (1978), (RTI/1342/0001F; Order No. AD-A060354), 141 pp. From: Gov. Rep. Announce. Index (U. S.) 1979, 79(5), 162. Report written in English. CAN 91:61831 AN 1979:461831 CAPLUS (Copyright 2002 ACS)

Abstract

Definition of the specific air pollutants generated from the prodn. of RDX [121-82-4], HMX [2691-41-0], and TNT [118-96-7], together with their attendant raw material manuf. and recovery processes is discussed, as well as the incineration of offgrade and used materials. Plant visits were made to discuss operations and acquire available data, which, together with survey reports by the USAEHA and technol. reports from the arsenals, were used to develop a state-of-knowledge emissions inventory projected to mobilization prodn. rates. Individual emission sources were characterized to the extent possible. The considerable data gaps were identified and flagged for further investigation. A methodol. was applied to develop ests. of concns. of the various compds. that might arise in the air over the plant. The chem. and toxicolog. characteristics of known emitted compds. were used, and their relevant chem. reactivity under photochem. conditions and at ground state was reviewed by literature search. The various possible transformation processes were catalogued..

Bibliographic Information

Pollution abatement in the military explosives industry. Patterson, J. W.; Shapira, N. I.; Brown, J. Illinois Inst. Technol., Chicago, Ill., USA. Proc. Ind. Waste Conf. (1977), Volume Date 1976, 31 385-94. CODEN: PIWCAX Journal written in English. CAN 88:65586 AN 1978:65586 CAPLUS (Copyright 2002 ACS)

Abstract

Conditions and procedures were studied at army, navy, and air force facilities where explosives are manufd., assembled, and packed. The study defines and characterizes wastewater effluents from the military explosive and propellant prodn. industry, and identifies and assesses water-pollution abatement procedures, manufg. changes, water-management programs, and water-treatment technols. Only H2SO4 and HNO3 acids; the explosives TNT [118-96-7], RDX [121-82-4], and HMX [2691-41-0]; and the propellant nitrocellulose [9004-70-0] are considered.

Bibliographic Information

Toxicological investigations of pilot treatment plant wastewaters at Holston Army Ammunition Plant. Stilwell, J. M.; Eischen, M. A.; Margard, W. L.; Matthews, M. C.; Stanford, T. B. Battelle Columbus Lab., Columbus, Ohio, USA. Avail. NTIS. U. S. NTIS, AD Rep. (1977), (AD-A042601), 56 pp. From: Gov. Rep. Announce. Index (U. S.) 1977, 77(21), 106. CODEN: XADRCH Report written in English. CAN 88:41245 AN 1978:41245 CAPLUS (Copyright 2002 ACS)

Abstract

The toxicity of wastewaters from a pilot biol. treatment plant was detd. Manufg. wastewaters from both Area A and Area B were mixed in a ratio of 1:9 by vol., resp. This mixt. was then treated by 2 biol. systems, the 3A system which consisted of an activated-sludge chamber and the 6A system which contained both a trickling filter and an activated-sludge chamber. The 96-h static acute LC50 toxicities of Area A wastes, Area B wastes, the A + B mixt., the 3A system effluent and the 6A system effluent were detd. using fathead minnows. Quant. analyses of RDX [121-82-4], HMX [2691-41-0], TNT [118-96-7], and COD in the test waters were also conducted in conjunction with each test. Other water quality parameters correlated with munitions constituents and fish mortality. In-house Ames Spot tests were conducted on all wastewaters from the pilot plant. The overall results of the on-site bioassay tests indicate that biol. treatment, either activated sludge or the combination trickling-filter-activated sludge, does reduce the toxicity of the wastewaters.

Bibliographic Information

Absence of health hazards associated with RDX manufacture and use. Hathaway, James A.; Buck, Charles R. Occup. Environ. Med. Div., U. S. Army Environ. Hyg. Agency, Aberdeen Proving Ground, Md., USA. J. Occup. Med. (1977), 19(4), 269-72. CODEN: JOCMA7 Journal written in English. CAN 87:72661 AN 1977:472661 CAPLUS (Copyright 2002 ACS)

Abstract

A cross-sectional epidemiol. study was conducted to investigate cases of systemic lupus erythematosus at one munitions plant. The study demonstrated no excess of autoimmune disease and also failed to identify any abnormalities of the hematol., hepatic, or renal systems in employees with 8 h time-weighted exposures to cyclotrimethylene trinitramine (RDX) [121-82-4] of £1.57 mg/m3 (av. exposure was 0.28 mg/m3).

Bibliographic Information

State-of-the-art: military explosives and propellants production industry. Volume III. Wastewater treatment. Patterson, James; Shapira, Norman I.; Brown, John; Duckert, William; Polson, Jack. Am. Def. Prep. Assoc., Washington, D. C., USA. U. S. Environ. Prot. Agency, Off. Res. Dev., [Rep.] EPA (1976), (EPA-600/2-76-213c), 169 pp. CODEN: XPARD6 Report written in English. CAN 87:11084 AN 1977:411084 CAPLUS (Copyright 2002 ACS)

Abstract

Wastewater treatment in the manuf. of TNT [118-96-7], HOAc [64-19-7], Ac2O [108-24-7], HNO3, H2SO4, nitrocellulose [9004-70-0], RDX [121-82-4], HMX [2691-41-0], nitroglycerin [55-63-0], sellite (Na2SO3), cast, solvent, and solventless propellants, and pressed and plastic-bonded explosives is discussed.

Bibliographic Information

State-of-the-art Military Explosives and Propellants Production Industry. Volume I. The military explosives and propellants industry. Patterson, James; Shapira, Norman I.; Brown, John; Duckert, William; Polson, Jack. Am. Def. Prep. Assoc., Washington, D. C., USA. U. S. Environ. Prot. Agency, Off. Res. Dev., [Rep.] EPA (1976), (EPA-600/2-76-213a), 96 pp. CODEN: XPARD6 Report written in English. CAN 86:192060 AN 1977:192060 CAPLUS (Copyright 2002 ACS)

Abstract

The manufg. technol. for explosives and propellants and their intermediates and problems and handling of wastewaters are discussed.

Bibliographic Information

RDX. Meredith, Joseph A. (United States Dept. of the Army, USA). U.S. (1976), 2 pp. CODEN: USXXAM US 3937703 19760210 Patent written in English. Application: US 74-522153 19741108. CAN 85:7960 AN 1976:407960 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
US 3937703 A 19760210 US 1974-522153 19741108

Abstract

RDX [121-82-4] is prepd. by reacting HCHO [50-00-0] and a C1-3 alkyl nitrile, in the absence of solvents to form 1,3,5-triacylhexahydro-s-triazine and then reacting with concd. HNO3. Thus, 13.8 g propionitrile (I) [107-12-0] and 0.65 g H2SO4 were refluxed and a soln. of 15 g HCHO as trioxane in 13.8 g I was added during about 30 mins. The slurry that formed was added slowly to 10 vols. of 99% HNO3 in a glass flask cooled in an ice bath. The mixt. was held 15 mins with ice bath cooling, allowed to warm to room temp. for 15 mins and then heated to 60° for 60 mins. The mixt. was cooled and drowed into 5 vols. ice water. The yield was 21% based on the propionitrile.

Bibliographic Information

Wabash-RDX manufacture: a laboratory examination of the ammonium nitrate process. Warman, Maurice. Picatinny Arsenal, Dover, N. J., USA. Avail. NTIS. U. S. NTIS, AD Rep. (1975), (AD-A016863), 13 pp. From: Gov. Rep. Announce. Index (U. S.) 1975, 75(26), 56. CODEN: XADRCH Report written in English. CAN 85:7919 AN 1976:407919 CAPLUS (Copyright 2002 ACS)

Abstract

The optimized NH4NO3 process for prepg. RDX [121-82-4], developed at Wabash River Ordnance Works on a lab. scale, has been checked and verified. Items considered included yield and quality of RDX, recovery and recycle of excess NH4NO3, recovery of excess HNO3, and its stabilization by controlled fume-off. The process is considered ready for study on a large scale.

Bibliographic Information

Reclaiming and recycling plastic-bonded energetic material. Falterman, Charles W.; Menz, Fred; Silver, Wallace E.; Wiggins, Pearsie S. (United States Dept. of the Navy, USA). U. S. Pat. Appl. (1975), 8 pp. Avail. NTIS. CODEN: XAXXAV US 554358 19750303 Patent written in English. Application: US 75-554358 19750303. CAN 84:152904 AN 1976:152904 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
US 554358 19750303 US 1975-554358 19750303

Abstract

Solid, plastic-bonded, explosive charges in obsolete or otherwise rejected warheads may be safely removed therefrom for recycling by insertion of detonating cord into the warhead's safe and arm (or other) cavity, filling such cavity with water, and detonating the cord. Normally a portion of the charge is recovered as particles suitable for immediate reuse while the remainder must be broken down to a smaller size. For reuse with a different binder, the original may be removed with solvents or by mech. means. Care must be exercised to avoid use of sufficient detonating cord to initiate sensitive charges. Thus, .apprx.30 g of 50-60 gr/ft Primacord under water in the safe and arm cavity of an MK 38 Mod O warhead (charge 20.1 lbs pressed DATB/nylon) was detonated from the aft end to split the warhead skin and shock out the charge: about 50% was broken into granules resembling the original molding powder and the large pieces were broken down to similar sized particles on soaking 5-30 min in water or other aq. wetting agent.

Bibliographic Information

The preparation of RDX from 1,3,5-triacylhexahydro-s-triazines. Gilbert, E. E.; Leccacorvi, J. R.; Warman, M. Explos. Div., Picatinny Arsenal, Dover, N. J., USA. ACS Symp. Ser. (1976), 22(Ind. Lab. Nitrations, Symp., 1975), 327-40. CODEN: ACSMC8 Journal written in English. CAN 84:138022 AN 1976:138022 CAPLUS (Copyright 2002 ACS)

Abstract

Nitrolysis of N-substituted hexahydro-s-triazine to produce RDX [121-82-4] was achieved in good yields only when the substituent was a lower alkanoyl, being limited by steric and inductive factors in the sidechains. A 4.8-to-1 mol. ratio of HNO3-trifluoroacetic anhydride gave best yields of RDX (98%, for the tripropoxy deriv.), followed by HNO3-P2O5, and finally HNO3 alone. Reaction of the triacetyl deriv. with an equimolar mixt. of HNO3-trifluoroacetic anhydride proved to be a new and superior method for prepg. 1-acetyl-3,5-dinitrohexahydro-s-triazine (TAX) [14168-42-4].

Bibliographic Information

HMX and RDX synthesis. Coon, C. L.; Guimont, J. M. Stanford Res. Inst., Menlo Park, Calif., USA. Avail. NTIS. U. S. N. T. I. S., AD/A Rep. (1974), (No. 005654/9GA), 90 pp. From: Gov. Rep. Announce. Index (U. S.) 1975, 75(8), 71. CODEN: XTSRDM Report written in English. CAN 83:118022 AN 1975:518022 CAPLUS (Copyright 2002 ACS)

Abstract

The objective of the research was to find potentially inexpensive synthetic routes to HMX [2691-41-0] and RDX [121-82-4] that offer advantages over current procedures. The research concerns addnl. work on the optimization of the amide-triazine process, new procedures for prepn. of HMX, and new nitrolysis procedures. The amidetriazine process was studied to det. the effect of pressure on other reaction parameters. The possible use of Me phosphonamide [56343-49-8], hydroxymethyloxamide [17643-47-9], and bis(chloromethyl)acetamide [56343-50-1] in the prepn. of HMX precursors was studied.

Bibliographic Information

Nitrosative cleavage of 1-(acetoxymethyl)-3,5-dinitroperhydro-1,3,5-triazine by dinitrogen tetraoxide. Bonner, Trevor G.; Hancock, Richard A.; Roberts, John C. Chem. Dep., R. Holloway Coll., Egham/Surrey, Engl. J. Chem. Soc., Perkin Trans. 2 (1974), (6), 653-8. CODEN: JCPKBH Journal written in English. CAN 81:104224 AN 1974:504224 CAPLUS (Copyright 2002 ACS)

Abstract

Treatment of the title triazine (I) with N2O4 at 0° in the absence of solvent gave 85% II, but in MeCN with excess N2O4, 90% 1,3,5-trinitroperhydro-1,3,5-triazine (III) was obtained. The N-nitrosation in CCl4, first-order in I and N2O4, proceeds by an ion pair attack mechanism. Treatment of II with 100% HNO3 at -10 to -20° gave III.

Bibliographic Information

Preparation and purification of cyclotrimethylenetrinitramine (RDX). Singh, Balwant; Kujur, C. M. P.; Bhatia, P. S.; Gadhikar, P. N. Terminal Ballistics Res. Lab., Chandigarh, India. Indian J. Technol. (1973), 11(6), 260-1. CODEN: IJOTA8 Journal written in English. CAN 80:82897 AN 1974:82897 CAPLUS (Copyright 2002 ACS)

Abstract

A three-feed four-stage method was developed for the prepn. of cyclotrimethylene trinitramine (I) at 46 ± 3° hexamine is nitrated in the presence of HOAc-Ac2O using 1:1 NH4NO3-HNO3 at 46 ± 3° with 15% BF3 catalyst.

Bibliographic Information

N-(Nitroxymethyl) derivatives of 1,3-dinitroperhydro-1,3,5-triazine, piperidine, and succinimide. Bonner, T. G.; Hancock, R. A.; Roberts, J. C. R. Holloway Coll., Englefield Green/Surrey, Engl. J. Chem. Soc., Perkin Trans. 1 (1972), (15), 1902-7. CODEN: JCPRB4 Journal written in English. CAN 77:75101 AN 1972:475101 CAPLUS (Copyright 2002 ACS)

Abstract

Reaction of N-(iodomethyl)-piperidine and N-(bromomethyl)succinimide with AgNO3 gave N-(nitroxymethyl)piperidine (I) and N-(nitroxymethyl)succinimide (II), resp. I is unstable, is easily hydrolyzed, and undergoes nucleophilic displacement (e.g. with NaOEt) readily, whereas II is stable and unreactive towards water; this difference in reactivities was explained by the degree of carbonium ionic character of the methylenic C atom attached to the nitroxy group. 1,3-Dinitro-5-(nitroxymethyl)perhydro-1,3,5-triazine eluded prepn. from either the N-(acetoxymethyl) analog with HNO3-MeCN or the N-(chloromethyl) analog with AgNO3MeCN; in the former case an interaction with the solvent was explained while in the second case the formation of 1,5-bis(3,5-dinitroperhydro-1,3,5-triazin-1-yl)-2,4-dinitro-2,4-diazapentane was proved.

Bibliographic Information

Octogen manufacture. Cartalas, Rene; Konrat, Jean P.; Molard, Louise. (Etat Francais). Fr. (1971), 8 pp. CODEN: FRXXAK FR 2053804 19710521 Patent written in French. Application: FR 19690718. CAN 76:85850 AN 1972:85850 CAPLUS (Copyright 2002 ACS)

Patent Family Information

Patent No. Kind Date Application No. Date
FR 2053804 19710521 FR 19690718

Abstract

In the nitration of hexamethylenetetramine (I) in Ac2O or AcOH by HNO3 and NH4NO3, the octogen (II) is sepd. by filtration without diln. and the soln. heated to 80°, with conversion of Ac2O to AcOH and decompn. of secondary unstable nitration products, and refluxed. Concd. AcOH (e.g., 97%) is recovered by distn. (optionally with AcONa for HNO3 neutralization) at 120-30° in vacuo. Thus, at 44° II contg. hexogen (III) was obtained in about 72% yield (based on I), the recovered AcOH could be reused, and the final residue heated to boiling with water contg. 2% HNO3 yielded 10-15% of a 3:1 mixt. of III and II useful in place of III.

Bibliographic Information

Shock-sensitive cyclotrimethylenetrinitramine (RDX). Batten, J. J. Dep. Supply, Aust. Def. Sci. Serv., Ascot Vale, Aust. J. Appl. Chem. Biotechnol. (1971), 21(6), 163-7. CODEN: JACBBD Journal written in English. CAN 75:65762 AN 1971:465762 CAPLUS (Copyright 2002 ACS)

Abstract

A form of RDX with a shock sensitivity comparable with that of PETN was produced by sublimation. However, the material is as insensitive to heat, impact, friction and static discharge as are the normal forms of RDX, and it has a similar storage life. The shock sensitivity tests were performed with these explosives either cast in TNT or bonded in silicone rubber.

nbk2000
April 26th, 2002, 06:26 PM
Now see, this is the kind of information that people need to be posting here!

We're having too many cases of simplisitic info copied out of internet encyclopedias being posted here.

Explosives synthesis isn't a simple cake recipe that you can have some leeway in the amounts and such. It is EXACT.

Fortunately for us, some people like Mega have acess to the "good stuff". And, hopefully, more of us will be accessing such information in the future as you get into colleges and universities. It'd be nice if such information was on the net, but it's not...yet.

Keep up the good work. Now see, this is the kind of information that people need to be posting here!

Keep up the good work. :)

I found the article on RDX sublimination interesting. Wonder if the principle could be utilized with other energetics?

<small>[ April 27, 2002, 02:54 PM: Message edited by: nbk2000 ]</small>

mongo blongo
April 26th, 2002, 09:10 PM
Maybe he's stoned like me right now! :D
Mega- What can I say. That was a treat! Thanx a lot for all that hard work! :)

megalomania
April 27th, 2002, 12:57 PM
I should add that anybody can get the patents that are listed at espacenet.com. I will not be getting any of the Chinese literature, although I would love to get Huozhayao Xuebao (The Chinese Journal of Explosives and Propellants). As much as that journal may be nice to have, one, I can't read or translate Chinese, and two, nobody seems to have it in the USA. There may be a translation copy available (like how Zhur. Khim. now offers "The Journal of Russian Chemistry" in English, and how "Angewandte Chemie" has an International edition) but I have yet to find it. The Japanese Journal of Explosives is probably also out. Hmm, mayhaps I should get some refs for other major explosives like HMX, PETN, and CL-20.

Celtick
April 28th, 2002, 10:38 AM
Some patents with information about HMX compositions :D :

United States Patent 6,214,988
Lukasavage , et al. April 10, 2001
Process for making an HMX product
Abstract
A process for preparing an HMX product comprises the steps of: (a) providing a granule that comprises a plurality of alpha-HMX particles and which has internal void spaces; and (b) sorbing at least one second material into the void spaces in the granule. The second material can be sorbed into the granules by using a vacuum to draw a gas phase comprising the second material into the granule. Alternatively, the second material can be sorbed into the granules by dissolving or dispersing the second material in a liquid solvent, contacting the solvent with the granules, and evaporating the solvent, whereby the second material is sorbed into the granules. Various second materials can be used, such as energetic materials and fuels.

United States Patent 6,194,571
Lukasavage February 27, 2001
HMX compositions and processes for their preparation
Abstract
A process for making alpha-HMX comprises the steps of: (a) combining phosphorus pentoxide and nitric acid at a temperature of about 0-25.degree. C., forming a reaction mixture; and (b) adding a compound having the formula: ##STR1## wherein R is straight chain or branched alkyl having 1-5 carbon atoms, to the reaction mixture, whereby a product comprising alpha-HMX is produced.

United States Patent 5,268,469
Lukasavage , et al. December 7, 1993
Process of making impact insensitive Alpha-HMX
Abstract
An improved process of making a highly impact insensitive form of HMX cal Alpha HMX has been accomplished. Test results of insensitive impact from drop heights of 5 to 10 times greater than Beta HMX, the conventional explosive, has been successfully achieved. This accomplishment has been achieved without the addition of any additives, and is attributed to the attainment of small particle size, whole crystals, narrow size distribution, and sample purity.

United States Patent 5,250,687
Lukasavage , et al. October 5, 1993
Process for preparation of RDX
Abstract
1,3,5-TRINITROHEXAHYDRO-1,3,5-TRIAZINE (RDX) is prepared in a new simplif and efficient manner which provides near quantitative yield. Our process is based upon the nitration of 3,7-DIACETYL 1,3,5,7 TETRAAZA[3.3.1.]BICYCLONONANE (DAPT).

United States Patent 5,124,493
Lukasavage , et al. June 23, 1992
Process of producing XMX in 100% yield and purity
Abstract
An improvement when 1,3,5,7-tetranitro-1,3,5,7-tetraazacyclooctane is preed by nitrolysis of 1,3,5,7-tetraacyl-1,3,5,7-tetraazaceyloctane with a solution of nitric acid and nitrogen pentoxide or phosphorous pentoxide. This improved process herein before set forth produces 99% yield and purity of product.

United States Patent 5,120,887
Lukasavage , et al. June 9, 1992
Process of making pure SOLEX
Abstract
1-(n)-acetyl-3,5,7-trinitrocyclotetramethylenetetramine is prepared by nilysis of 1,3,5,7-tetracyl-1,3,5,7-tetraazacyclooctane with a solution of nitric acid and nitrogen pentoxide or phosphorous pentoxide.

United States Patent 4,794,180
Heinemeyer , et al. December 27, 1988
Process for producing fine-grained .beta.-HMX
Abstract
A process for producing fine-grained .beta.-HMX wherein a solution of .beta.-HMX is treated in a .gamma.-lactone in a temperature range of between 5.degree. and 15.degree. C. with toluene, and the desired fine and very pure .beta.-HMX crystals are precipitated. The resultant crystals have grain sizes of down to 5 .mu.m and exhibit an extremely small proportion of other modifications or forms of HMX. An additional aspect of the process resides in providing the very fine .beta.-HMX with a coating of a thermoplastic polymer. In this procedure, the .beta.-HMX particles, after having been separated from toluene, are made into a slurry in water and combined under agitation at temperatures of between 25.degree. and 60.degree. C. with a solution or suspension or emulsion of the thermoplastic polymer. During this step, granules are formed which can be separated after distillation of the solvent.

United States Patent 4,785,094
Levinthal November 15, 1988
Crystallization of beta HMX
Abstract
Method of directly precipitating substantially pure beta HMX from a substantially anhydrous nitric acid solution without forming and recrystallizing polymorphic HMX. HMX dissolved in a solvent consisting essentially of anhydrous nitric acid is added to water which is seeded with crystals of beta HMX to substantially completely precipitate all the HMX from solution as beta HMX without forming crystals of the other polymorphic forms of HMX. A preferred reaction and apparatus for preparing HMX in anhydrous nitric acid is also disclosed.

United States Patent 4,638,065
Svensson , et al. January 20, 1987
Crystallization method for HMX and RDX
Abstract
The present invention relates to a method for the recrystallization of the high explosives HMX and RDX. According to the invention, the explosive is dissolved in a low molecular weight, liquid (at room temperature) lactone, after which the degree of saturation of the solution obtained, is changed by either lowering the temperature or by diluting with water. This method produces, depending on the crystallization method chosen, .beta.-HMX crystals or RDX crystals of either 50-1500 .mu.m or 5-50 .mu.m median particle diameter respectively.

United States Patent 4,481,371
Benziger November 6, 1984
Method of making fine-grained triaminotrinitrobenzene
Abstract
A method of forming a fine-grained species of the insensitive high explosive sym-triaminotrinitrobenzene (TATB) without grinding. In accordance with the method, 1,3,5-trichloro-2,4,6-trinitrobenzene (TCTNB) is aminated by reaction with gaseous ammonia in an emulsion of toluene in water. The ratio of water to toluene in the emulsion is selected so that toluene is the dispersed phase in the emulsion. The size of the dispersed TCTNB-containing toluene droplets determines the particle size of the resulting TATB. The emulsion is preferably formed with an emulsifier such as ammonium oleate, which may be generated in situ from oleic acid, and stabilized with a protective colloid such as polyvinyl alcohol.

United States Patent 4,168,191
Benziger September 18, 1979
Thermally stable, plastic-bonded explosives
Abstract
By use of an appropriate thermoplastic rubber as the binder, the thermal stability and thermal stress characteristics of plastic-bonded explosives may be greatly improved. In particular, an HMX-based explosive composition using an oil-extended styrene-ethylenebutylene-styrene block copolymer as the binder exhibits high explosive energy and thermal stability and good handling safety and physical properties.

United States Patent 4,091,729
Bell , et al. May 30, 1978
Low vulnerability booster charge caseless ammunition
Abstract
A low vulnerability booster charge comprising single, fairly large crystals f 1,3,5,7-tetramethylenetetranitramine (HMX) or 1,3,5,-trimethylenetrinitramine (RDX) about 160 microns diameter coated with a polyurethane cement which comprises about 15 weight percent of the entire booster charge.

United States Patent 4,032,377
Benziger June 28, 1977
Method for the production of high-purity triaminotrinitrobenzene
Abstract
Triaminotrinitrobenzene is readily formed by the nitration of 1,3,5-trichlorobenzene to 1,3,5-trichloro-2,4,6-trinitrobenzene followed by amination to triaminotrinitrobenzene. The purity of the triaminotrinitrobenzene is significantly improved if, during the amination step, sufficient water is present that the byproduct ammonium chloride formed during the amination is rendered at least semideliquescent

United States Patent 3,985,595
Benziger October 12, 1976
Insensitive explosive composition of halogenated copolymer and triaminotrinitrobenzene
Abstract
A highly insensitive and heat resistant plastic-bonded explosive containing 90 wt % triaminotrinitrobenzene and 10 wt % of a fully saturated copolymer of chlorotrifluoroethylene and vinylidene fluoride is readily manufactured by the slurry process.

United States Patent 2,656,355
Bachmann October 20, 1953
Purification of Cyclonite

United States Patent 3,304,300
Watters February 14, 1967
Method for Isolation and Purification Of HMX

Microtek
April 29th, 2002, 05:02 AM
Dhzugasvili said that he had made 50 g of HMX using Mega's method which, if I recall, requires acetic anhydride but no BF3. So if what Dhzugasvili said was true, and he followed the recipe exactly then there would be a use for the AcO afterall.

Edit: I posted this in the wrong thread; it should have been in the one on acetic anhydride. My apologies.

<small>[ April 29, 2002, 10:20 AM: Message edited by: Microtek ]</small>

cutefix
May 9th, 2002, 01:34 AM
I doubt if Dhugas really succeeded in his experiments….
I was wondering whether he did really made HMX. I noticed in that post some inconsistencies in making RDX.
In my past experience with direct nitration it will need at least 7parts 99%Nitric acid per 1 part hexamine in order to obtain RDX.Were you guys able to make it using his ratio?
Meanwhile The Mega procedure for RDX,by direct nitration,it uses one part methenamine to more than 4 part nitric acid.In some procedures it will even react more than 10 part nitric acid per part of hexamine in order to raise the yield.Dhugas claims he can make RDX by using 1 part hexamine and 2 part nitric acid.Even if he claims he use 100% nitric acid and purified by removal of nitrogen oxides.
Did anybody was able to do this such low ratio between acid and the methenamine?
For details :
Check his post which says,
__________________________________________________ _____________________
The best procedure i have found for RDX with the best yields involves n-nitration, the most basic, taking 120ml of anhydrous nitric acid (purged of dissolved NOx with urea) to 75g dry methenamine, and then after addition is complete heating the mix to 55 deg Celcius for ten minutes and then cooling and precipitating
__________________________________________________ ______________________
HMX is more difficult to make than RDX,and I doubt if he really was able to make it.
Unless he can post some evidence of his recent work….

Microtek
May 10th, 2002, 07:34 AM
I usually use 2 parts nitric acid to 1 part hexamine dinitrate, but when looking at the amount of hexamine used, it comes to around 1:4 to the nitric.
Is this what he means, I wonder ?

cutefix
May 12th, 2002, 10:06 PM
May I ask how much RDX did you get based on hexamine with this system?

Microtek
May 13th, 2002, 02:42 AM
Quite good yields actually; around 2 grams from 2.5 grams of HDN. The scale I used when I did this was limited to about 0.25 gram accuracy, so...

mongo blongo
May 13th, 2002, 10:40 AM
What temp did you heat it to? Do you use the normal nitration process with it? It could be used like the K-process since the ammonium nitrate is used to create HDN as an intermediate. In other words you could use HDN like the hex in the normal nitration method but heat it to 70-80 degrees C instead of 55 degrees C. Would this work better?

Microtek
May 13th, 2002, 11:39 AM
I used the proceedure for nitrating hexamine directly, adjusted the ratios to take the two moles of HNO3 into account. In other words: I heated it to 55 C for 5 minutes.