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Alexires
June 16th, 2008, 09:46 PM
And this is exactly WHY all relevant information should be included in the original post. Rbick gave advice based upon what he uses and only because he didn't know that you used Sulphuric Acid he gave you wrong advice (through no fault of his own, I might clarify).

To all, if you want advice or help with something, please make sure that you include all information that you think may be relevant, no matter how slightly.

Better to have the right answer than to throw away your product, or worse, explosively remove parts of yourself.

Rbick - It might be that the turbidity is formed by air bubbles that are attached to small goblets of (in your case) Water, Hydrogen Peroxide and HCl. In my opinion, these air bubbles are more likely due to the catalytic decomposition of Hydrogen Peroxide by Sulphuric Acid than any thing introduced mechanically (such as a syringe). Or, if you are shaking it around, it sometimes takes a fair while for layers to separate out.

Hightimes
June 17th, 2008, 02:53 AM
I plan to make a few ml soon just to test out, how much more stable/unstable is this to TATP?.
Also would 50% h202 be alright ? or would I need to dilute it ?
( sorry for my noob questions lol )

Ethyl
June 17th, 2008, 05:08 AM
I had a problem with MEKP. I made it with 19% HCl, MEK p.a. and 30% H2O2 p.a. I mixed 20 ml of peroxide with around 20 ml of MEK and around 10 ml of HCl. The majority of MEKP formed in one minute. I let it stand for around 30 min. Then I extracted some MEKP (top layer) and soaked a piece of toilet paper with it. Strangely it only slowly burned. Them I tried to ignite a few drops of MEKP with a match. I couldn't light it. Then I mixed it with sodium nitrate in a ratio around 50:50, put it in a small plastic bottle with a hole in the cap for the sparkler and tried to ignite it with a sparkler. It only ignited and burned slowly until it extinguished itself. Strangely after 4 days of standing it started to behave normally. Does anyone know why did the MEKP behave like that?
That is very strange as I have made MEKP/AP and it behaves like it should, but pure MEKP doesn't (well it does but only after 4 days).


And as far as I know MEKP and MEKP/AP are storage stable. Are MEKP/AP/AN and MEKP/AN also storage stable?

Oh, there is one thing I would like to say about MEKP/AN. It is extremely important how the AN was prepared for it. If AN is made by recrystallization from a fertilizer, dried and then ground it wont work very well because when the AN is drying in the oven it melts in the water it contains. So when in solidifies it becomes compact and nonporous and even when ground up fine it doesn't absorb MEKP good. On the other hand if the AN is dried, ground up partially and then heated again (but not hot enough to melt), ground up a little more while hot and then finally ground when it cools it becomes much more porous and absorbs MEKP much better. You can also notice the difference between AN made with only one heating (much harder to ground, and the resulting powder looks like compact particles) and AN made with two "heatings" (much easier to ground and particles look fluffy).

Rbick
June 17th, 2008, 08:23 AM
Then I tried to ignite a few drops of MEKP with a match. I couldn't light it.

MEKP, although a liquid, is just like any other explosive. There will still be water in between the MEKP molecules, so you need to give it time to dry. Letting the air bubbles that we talked about earlier settle out could also be important, since air bubbles leave the chance for hot spots, therefore increasing sensitivity. Although it would increase sensitivity, I think it would lower power, making air bubbles something you don't want.

And as far as I know MEKP and MEKP/AP are storage stable. Are MEKP/AP/AN and MEKP/AN also storage stable?

I recall seeing a post where a guy stored MEKP in a jar for years under water and it worked fine. I personally wouldn't recommend it, as storing sensitive explosives is never a good idea. Try not to store it more than a couple weeks. Plus everyone knows how hygroscopic AN is, so unless it is sealed, that isn't a good idea either.

Thats a good idea for the AN. Remember that with a rise in temperature, solubility also increases. There isn't a point in heating the AN to near its melting temp of 169* C. You can dry it just fine at 100* C. Leave AN in the oven at 100* for 4 hours and you'll have the driest AN ever, ever... :D

Bert
June 17th, 2008, 09:51 AM
on the other hand if the AN is dried, ground up partially and then heated again (but not hot enough to melt), ground up a little more while hot and then finally ground when it cools it becomes much more porous and absorbs MEKP much better. You can also notice the difference between AN made with only one heating (much harder to ground, and the resulting powder looks like compact particles) and AN made with two "heatings" (much easier to ground and particles look fluffy).

AN undergoes a change in crystal structure at high temperatures- See Tenney Davis' Chemistry of Powders and Explosives on why AN based "black powder" didn't catch on as artillery propellants despite their good performance and cheapness. Essentially, cycling the AN back and forth past the transition temperature a few times causes the crystals to break up, increasing the surface area. A bad thing if you're trying to make a consistently deflagrating propellant, a good thing if you're trying to get larger amounts of liquids absorbed into the fine cracks in the crystals for HE uses.

Alexires
June 18th, 2008, 02:32 AM
To add on to Bert's comment - There is a document on the FTP that deals with the different densities of AN after certain crystallisation processes (different temperatures).

Perhaps I am missing something, but in Rbick's earlier post
Its been a while since I've made MEKP, but if I remember correctly, the MEKP forms as the bottom layer of the liquids as it is more dense than the remaining unreacted peroxide, water, and MEK. In that picture, the bottom layer looks more like the MEKP. What quality are your reactants?
he stated that the MEKP forms on the bottom, with the left over MEK/H2O2/HCl floating on the surface. If this is indeed the case, then you are actually NOT extracting MEKP, and the solution you have is still reacting (hence you leaving it for a while and it working).

Ethyl, have you ever tried burning the other layer?

Rbick
June 18th, 2008, 08:06 AM
Alexires; Thanks, I missed the part where he said he extracted the top layer and that he used HCl. I keep getting Infinie's and ethyl's posts mixed up.

To clear things up:

If you are using undiluted SULFURIC ACID in your MEKP synthesis, the MEKP will form on top, since SA is very dense.

If you are using HYDROCHLORIC ACID, the MEKP will form on the bottom, as it is more dense than the unreacted MEK, water, and HCl.

Ethyl; The reason it was only burning slowly was because you were trying to detonate unreacted MEK, H2O2, and HCl (make sure to read Alexire's response above). Try extracting the bottom, more dense layer and see what happens. It should detonate with an impact test even just minutes after extraction. Do an impact test first, try just a single drop and that should do the trick. Wear a gas mask, it smells like SHIT ;)

Ethyl
June 18th, 2008, 10:56 AM
I forgot to say one thing in the previous post, sorry. At first I could see the MEKP forming on top of the reaction mixture. Then I tried to burn it and it didn't burn as fast as it should. After 4 days the MEKP sank to the bottom (only a very small amount was left on the surface). Then it worked very good.

cpropellant
June 18th, 2008, 03:07 PM
Good day to all formites.
I am still learning,so please excuse any stupidity,mistakes made on my behalf.

I'd like to add a comment about observed sensitivity of MEKP and MEKP/AP-50%/50%.

The sensitivity of these two compounds differ a lot between shock initiation and
heat/flame initiation.

MEKP,when mixed with oak barrel wood shavings (used for smoking/flavouring meat), didn't detonate completely from flame,but it is still very shock sensitive.((as just pure MEKP tested *by throwing quite hard against wall (inside silicone tubing sealed with hot glue-gun at the ends.Crappy detcord)).

MEKP/AP on the other hand is easily initiated both way's.I always get full
detonation from whichever medium I mixed it with.It makes for useable detonator caps
in drinking straws sealed with hot glue.Just coat electric ignitor with NC.

Also,some 200 milliliter of both MEKP and MEKP/AP were put in sun for 3 day's to dry completely and then sealed in 500 milliliter normal plastic drinking bottle.
These were left in a hot summer sun for 3 months without any ill effects and still useable afterwards.
There was a partial pressure build-up in the bottle and I noticed liquid condensate
on the inside.
I don't see how this could be water vapour,maybe decomposition products?

Peroxide's were prepared by using 50%H2O2;30%HCL and lab-grade butan-1.
Temperature wasn't kept low and reaction vessel became very warm during addition of HCL.
Peroxide formed instantly and vessel was cooled to delay further evaporation of reactants.
After 24 hours product was washed using only H2O and neutralized with bicarbonate between many washings and decantations.

When left to stand the now clear peroxide sank to the bottom of vessel and was extracted.

I didn't cool the initial reaction as I wanted to observe the impact on the sensitivity and stability of formed peroxide's.
A pdf. file in this thread (link by The Duke) states that the trimeric form of MEKP decomposes to the dimeric form anyways,with up to six or seven other peroxide's forming as well.
So I didn't put much emphasis on the tetrameric form by cooling.


*Bad idea,but it was long ago and lesson learned.

Ethyl
June 20th, 2008, 03:28 PM
I also never cool the reaction mixture when making MEKP/AP.

Also I don't neutralize it. Apparently it is not required for MEKP/AP.

fluoroantimonic
June 28th, 2008, 08:32 PM
Yesterday (in a dream of course) I mixed roughly equal volumes of Hodgdon Longshot shotgun powder with MEKP/AP. Absolutely nothing happened. I then added about 4 times the mixture's volume of acetone. It formed a very pretty pearlescent black and silver mixture. After lengthy stirring it became mostly homogeneous and sticky. I then poured it in a thin layer onto aluminum foil. It is now drying.

I'm hoping it will evaporate the acetone quickly, but I'm afraid it will just form a dry skin on top and remain full of acetone. I'm not sure how that could be solved. A little acetone shouldn't hurt things much, just reduce sensitivity.

I think it would be easier just to absorb the MEKP/AP into powdered gunpowder. I don't know how to grind it safely though. Maybe slurried with water in a blender? And a long extension cord on it...

Also the way I synthesize my MEKP/AP is by putting a 1:1 Acetone:MEK mix and a 1:1.5 battery acid:50% H2O2 in the freezer. Once they're cold I add a little of the ketone mix to the beaker of peroxide/acid until the the temperature rises up to 5*C or so. Then I leave it in the freezer for a few more hours and repeat the process until all the ketones have been added. Then I suck it out and wash it with water and its ready to go. It gets good yields (maybe 60-70% based on ketones IIRC). I just did a batch that that has a theoretical yield of 480 grams. Have yet to measure yield. It will hopefully go into sensitizing a big load of AN and sensitizing DBSP for a booster.

EDIT: I just measure the yield of the MEKP/AP synth, 221 grams of nice clean clear MEKP/AP after washing with water twice. 46% yield, not too good, but I was in a bit of a hurry. I'm happy with it anyhow.

I also checked on my DBSP based plastic. It seems to have lost its acetone quicker than I expected. It now has a stiff rubbery consistency to it, maybe stiff enough to crack if pulled quickly. I don't know how much acetone is left because I never weighed it, but it doesn't look like much at all. If one wanted something easier to mold, a higher ratio of MEKP/AP would help. Also using straight MEKP would improve its elasticity. It seems promising for a cast primary or sensitive secondary depending on the ratio. It does present a challenge because it shrinks a lot when it loses the acetone. Not sure how to deal with that.

Alexires
June 28th, 2008, 11:52 PM
Right. Where to start?


I am still learning,so please excuse any stupidity,mistakes made on my behalf.


If you had read the rules, you would know that we do not excuse stupidity. We don't care if you don't speak English as a native language, if you are still learning, or if you profess to be some kind of genius. Proof is in the pudding. (Also the space bar is there for a reason, it goes AFTER the comma... any punctuation for that matter).

If we can't understand what you are talking about, you will be banned. If you say something stupid repeatedly, you will be banned. This is as much for your safety as ours. Stupidity is not something you can grow/learn out of, it is a trait that you will have for life, if you have it.

In the future, leave these asinine "disclaimers" out of your posts.


It makes for useable detonator caps in drinking straws sealed with hot glue. Just coat electric ignitor with NC.

I hope the hot glue was applied well before your mixture was put in the tube. Hot glue + sensitive explosive = lack of fingers.


These were left in a hot summer sun for 3 months without any ill effects and still useable afterwards.
There was a partial pressure build-up in the bottle and I noticed liquid condensate
on the inside.
I don't see how this could be water vapour,maybe decomposition products?

It could be water that was in the atmosphere when you closed the bottle, it could be unreacted reactants (the reactant was in excess originally) or it could be decomposition products. My guess is it is just water that was left over from when you sealed it (and reaction by-product), but you could always remove a sample and test it to find out.


Peroxide's were prepared by using 50%H2O2;30%HCL and lab-grade butan-1.


Butan-1 what? Butan-1-ol? Butan-1-amine? Butan-1-ene?

It is important to use correct laboratory names so we know what you are talking about instead of having to guess. In this case, I'm assuming you were talking about Butan-2-one? I'm guessing this because, after all, this IS a thread about MEKP and MEK is Butan-2-one (Butanone).

This is your first (and last) warning. Improve your post quality in the future.

I probably hate you
June 30th, 2008, 04:30 AM
I just wanted to add some of my knowledge of mekp with everyone I have been making this before I was a member here because it is easy and cheap. You need to keep the temp down when you are mixing it or it will vent acid like fumes (I assume by the burning and taste) horribly I learned the hard way from mixing too fast. Mixing some acetone (substituting approx 30% of the mek) IMO increases vod and density. In my syn. it usually would settle to the bottom with minimal layers elsewhere and after settling for several days would all join together in one layer (any random floating layers at different densities) Dampening not saturating wood or charcoal then allowing it to dry at least overnight seems to give the best results, I have tried to mix it with dbsp, perlite, aluminum, well you name it I was bored and tried it I think charcoal worked the best. I by no means know everything there is to know about mekp but I do have several years exp. with it. You will make your life more pleasant if you make/use it in a very well ventilated area I usually have a small fan blowing across my eyes to help with the fumes. This stuff while liquid can be stored for a long time my last batch, I just finished it, sat in its jar for over a year. I have some small explosives mixed up now if anyone would like a video I can make one and post it, they are just small crackling balls (emptied fireworks plastic containers) filled with a saw dust mekp mixture.

totenkov
June 30th, 2008, 11:32 AM
How long do you allow the reaction to sit? With a higher concentration of HP (in the mid 30% range) It goes in the fridge for one night only, I have found this is more than enough time for the MEKP to form and float to the top.

It should be obvious that any synthesis of a primary high explosive should be carried out in proper ventilation.

fluoroantimonic
June 30th, 2008, 05:04 PM
I have never noticed any fumes when making MEKP or MEKP/AP. If you are using HCl and allowing the reaction to warm up, that might do it, especially if HCl's solubility is reduced by the ketones. I have never needed special ventilation, and never smelled anything but the smell of MEK and MEKP later on. I never let it rise much above 5*C.

And why would MEKP+Charcoal be effective? MEKP is already very OB negative. Maybe the fine charcoal produces a secondary explosion when mixed with the surrounding air?

I usually let it sit in the freezer for a day or two after all the reactants have been mixed.

I probably hate you
July 1st, 2008, 02:01 PM
I usually allow my reaction to sit in the fridge until I use it all up but initially it is done reacting overnight but often, I dont know why, there are several different layers of mekp I can only imaginge it is different desities from adding the AP and after it sits longer they all seem to unite sometimes it takes a week or so. I know about proper ventilation maybe I am doing something wrong but the fumes from my mekp kill my eyes or maybe it is just me. Yes I do use HCI and it does warm up a little I try to keep it as cool as possible but due to my own impatience it doesnt keep cold so that probably explains that. As for charcoal I dont know wouldnt the OB balcane be way wrong with sawdust as well , if anyone knows why it works with different substates better would they please post it. I do not know the chemistry behind why it works and would like to know. Oh year something else that is fun is to apply about 5 drops to a piece of cardboard about 1.5" dia. (like from a box of a 12 pack of pop) allow that to dry for several hours then light that from a safe distance it will crack loud enough to make your ears ring, so you might want hearing protection if you value your hearing, it turns the cardboard to a fine floating cloud of dust. One last thing about the OB balance I just though of I tried to set one of my green cased balls in an enclosed box (late night mischieft) and it did not detonate a second one with the door to the box open only a small crack partially detonated and with the door fully open I finally got a full det blowing the back of the box out, so maybe an oxidizer could be mixed in with the mixture to help the OB.
I do appologize if my posts are jumpy and poorly writen I am just not that great with communication.

I probably hate you
July 2nd, 2008, 03:32 AM
I took some photos of a detonation but I don't know exactly how to link them or set them up I apologize but I have never done this before if anyone would like to see them please explain it to me if not don't worry about it.

FUTI
July 2nd, 2008, 09:13 AM
to I probably hate you: Maybe charcoal corrects negative OB of MEKP a little since it can adsorb good amount of oxygen (air) on its surface? MEKP is something I have no experience of and if I said something stupid MODS please delete post. What quantity of charcoal is mixed to a mass unit of MEKP?

fluoroantimonic
July 2nd, 2008, 08:13 PM
My MEKP/DBSP plastic has now hardened even more, I suppose the last of the acetone is gone. It is now the consistency of a hard plastic like HDPE but not as strong. I can't tell how much MEKP/AP is still in it, there must be quite a bit, it evaporates so slowly.

I tore off a thin piece and lit it with a match, it burned quickly leaving no residue. Not as fast as MEKP soaked paper though.

Now I need to figure out what to do with it...

Devourer
July 21st, 2008, 07:45 AM
Something just popped into my mind:

As MEKP is fuse sensitive when "soaking into things", could you make a fuse sensitive plastic explosive?

Maybe by mixing it with ETN, which is among the most sensitive secondary explosives, you could make a fuse sensitive mix..? ETN has much oxygen, so maybe we could get it OB! Or at least not far from.

When properly neutralized, both ETN and MEKP are storagable. ETN needs to be recrystallized, of course.

Maybe some chlorates, perchlorates, or Mg could be added to the mix to make it DDT, if it doesn't work with just ETN/MEKP.

I have no have no intentions to test this, but I think it was an interesting thought. So I just mentioned it to either be slaughtered, or brought to life.