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Author: Subject: Organic peroxides
KABOOOM(pyrojustforfun)
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[*] posted on 17-12-2003 at 18:59


it formes as an "intermediate" in AP synth. I doubt there's any way to prevent it from further reactions (which form AP) then isolating it



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smile.gif posted on 19-10-2004 at 08:13


I wonder, is acetone peroxide soluble in anything? :)



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[*] posted on 19-10-2004 at 09:17


Conveniently, its fairly soluble in Acetone (I think more-so in DCM), why you ask?
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[*] posted on 19-10-2004 at 10:59


AP is fairly soluble in anhydrous isopropanol .

But a more interesting AP solution is coprecipitated AP / MEKP ~ 50/50 , which
separates directly from synthesis as a reasonably pure anhydrous liquid ,
making it easier to isolate than either
AP or MEKP made separately .
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[*] posted on 20-10-2004 at 00:08


Just asking, might be useful for storage/separation from the reaction mixture.

[Edited on 20-10-2004 by Theoretic]




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Chris The Great
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[*] posted on 31-7-2005 at 02:39


Quote:
Originally posted by sylla
BTW, I've heard that dihydroperoxypropane could be formed using the common acetone/H2O2. I haven't done any search on it (I apologize if it is the first link on google :p). Have someone tried it ?

It's oxygen balance (-70%) is far better from other peroxides such as the acetone one (di/tri or tetra meric) and DPPP and a bit betterthan HMTD and TMDD. It's density is around 1.3 (following ACD/ChemSketch software).

But I'm sure with all these properties someone here had already tried it ! :)


I recently became interested in this peroxide and other non-tradition peroxides. Alot of organic peroxides have not been experimented much with, mainly HMTD, AP, etc. It forms, as already stated, as an intermediate in AP synthesis. Another peroxide also forms, basically two of these joined together by a peroxide bond:
HOOC(CH3)2OOC(CH3)2OOH
Both of these are soluble in water, but I think they could easily be extracted using something like methylene chloride or other non-polar non-water-miscible solvent. I would use methylene chloride because of it's low boiling point.

According to a journal on AP I read, it mentions that the peroxide you mentioned, HOOC(CH3)2OOH was isolated in 12% yield when 50% H2O2 and acetone where reacted in a 1:1 molar ration in the absence of the hydrogen ion (no acid). Hence, when you mix H2O2 and acetone you get a bunch of non-cyclic peroxides, the H+ caused them to form cyclic derivatives- the well known acetone peroxide.

When I attempt this procedure, I will mix H2O2 and acetone in a 2:1 molar ratio, with no acid. After several days I will extract with methylene chloride, and then gently boil if off along with the remaining acetone (the remaining acetone will also be picked up by the methylene chloride) to get the non-cyclic peroxides.

The Encyclopedia of Explosives gives some information on organic peroxide properties, which is based on structure. It appears that these peroxides should be quite stable (relative to other organic peroxides that is). For the C(OOH)2 type peroxide, explosive properties are listed as:
Polymeric peroxides formed as a decomposition product are extremely explosive

For HOOCOOCOOH type peroxides, it lists:
Very slight explosive properties

These could obviously be detonated but as organic peroxides go they seem to be quite stable. It will be interesting to attempt to isolate them.

Another interesting thing I noticed in that AP journal was that it mentioned "in the presence of the hydrogen ion, all three abducts have been isolated with the cyclic trimer being the predominant product in concentrated solutions."
Hence, it would appear that in lower concentrations of H2O2 and acetone, such as with 3% H2O2, the equilibrium shifts over to the non-cyclic peroxides, and hence a much larger amount of acid is required to push it back towards the cyclic trimer.

I recently picked up a liking for such 'non-traditional' peroxides and hope to prepare a couple of them in the near future. Some other ones I am interested in are the alkyl hydroperoxides, for example methyl hydroperoxide, CH3OOH. It's a liquid, seems to be sensitive from what I've read but info is very limited. The Encyclopedia says that it explodes violently (I would think so!) upon jarring or heating.
The explosion should follow:
CH3OOH --> CO + H2O + H2
It is prepared like this:
(CH3)2SO4 + 2H2O2 + 2KOH --> 2CH3OOH + K2SO4 + 2H2O
For the ethyl and isopropyl derivatives it says it is seperated by vacuum distillation but I'm not in a hurry to do that! Doesn't say anything about isolating the methyl hydroperoxide :(
I'm hoping it can be seperated by using methylene chloride as well, as thats simple. Unfortunately, "sensitive to jarring especially at warm temps" makes me wonder about the wisdom of boiling of a solvent. I think I'll let it sit in a cool dark location to evaporate.
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[*] posted on 31-7-2005 at 05:05


View: http://pulse.webtop100.net/images/methylhydroperoxide.zip 17pg 3.something MB

In German though. I had chemoleo translate some of it quite a while back, guess he wont mind me posting it. This regards the calcium/barium salts of methylhydroperoxide.

Quote:
Anyway, it says, 'crystalline barium hydroxide (presumably referring to Ba(OH)2*8H2O), or even calcium hydroxide, is easily dissolved in a concentrated aqueous solution of methylhydroperoxide.
Salts are formed, which are very soluble in H2O, and which can be isolated by evaporation at as low a temperature as possible (great care to be taken!)'.


But in the end, its quite hard to get any decent yield of the alkylhydroperoxides. I think there was a patent related to mixing methanol/H2O2 and salting out the hydroperoxide followed by distillation, give the patent office a search for methylhydroperoxide etc. but I think it was still <10% concentration.

Might be worth trying to extract dimethylolperoxide (formaldehyde/H2O2) with a more volatile solvent, as it wants to detonate if evaporated from water .. know that first hand. I think theres a Pb salt of this in PATR2700. Theres a soluble hydroperoxide of hexamine as well, also an insoluble one by using HNO3 check vol.8, H82.
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[*] posted on 31-7-2005 at 09:49


Quote:
But in the end, its quite hard to get any decent yield of the alkylhydroperoxides. I think there was a patent related to mixing methanol/H2O2 and salting out the hydroperoxide followed by distillation, give the patent office a search for methylhydroperoxide etc. but I think it was still <10% concentration.

I can't read German but at least that gave me a good idea of the synthesis as well as the yields. I guess 100g dimethylsulfate --> 7g methyl hydroperoxide is pretty poor. Couldn't find the patent but I would prefer to prepare it in the pure form, to make other interesting compounds and also for a small explosion test. I certainly don't want to make these to make big booms, I just wanna make them because they are interesting and unusual.

Thanks for the info! Can someone kindly translate the synthesis, which starts on page 12? It's fairly short. I can get the general idea but it would be nice to know exactly what they did, and not just generally what they did. Doesn't look that hard but it would be problematic if a sentence that I thought meant stir vigoursly actually means stirring causes detonation, etc.
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[*] posted on 16-8-2005 at 09:05
organic peroxides


Chris, sounds like you have some great ideas. Have you tried producing Methyl Ethyl Ketone Peroxide yet? I think you'll find that the VoD of this stuff is pretty good...and when mixed with Ammonium Nitrate can be quite powerful. Never mind TCAP...



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[*] posted on 16-8-2005 at 20:09


No, unfortunately I have not....

I haven't found MEK here (at least not in a product that it could be easily extracted from), but I haven't actually looked that hard.

If I see some I will definately pick some up though.
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[*] posted on 16-8-2005 at 22:07


Quote:
Originally posted by Chris The Great
No, unfortunately I have not....

I haven't found MEK here (at least not in a product that it could be easily extracted from), but I haven't actually looked that hard.

If I see some I will definately pick some up though.


It is avaliable, but getting scarcer due to its effects on health. Try Industrial Plastics and Paint, Cloverdale Paints, ICI paints, General Paints** I know they have a tonne of the stuff at dirt cheap prices. MEKP with an addition of a NITRATE is very fun to detonate. Its quite powerful :) oh, mixed with finely powdered Ammonium Nitrate 9:1 ratio proves to be awesome. No idea on the VoD...can't help you on that one. I bet it is more powerful than commercial PowerGel for rippin' a part rocks.

[Edited on 17-8-2005 by ((Blasta))]




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[*] posted on 22-6-2019 at 14:03
acetone peroxide/AP/triacetone triperoxide/TATP/TCAP/peroxyacetone from 3% H2O2!


So, the day before yesterday, I tried to make AP with 3% hydrogen peroxide disinfectant. I've heard of other people doing it before, they never gave their specific reaction conditions, and others saying it failed, and I wanted to know if it was possible. My first attempt failed, but the second I put about 70ml of disinfectant in a bottle, and left it in the freezer an hour until a bit of ice formed. Then I took it out, put 4ml acetone, and 7ml 10% hydrochloric acid and put it back in the freezer. My hope was that the low temperature (~-20C) would freeze some of the water out of solution, and make concentrated H2O2 in situ.

After 20Hrs, the mixture looked like a solid block of ice with a couple drops of free liquid. In reality, the block of ice was likely porous, with concentrated AP reaction mixture between the crystals. taking the bottle out of the freezer for an hour caused some of the ice to melt, although there was still frost forming on the outside of the bottle. The remaining ice rose to the top, while white particles settled to the bottom of the container. Then, before all the ice had melted, I added sodium bicarbonate until it stopped fizzing. Today, I filtered part of the mixture, and flame-tested the white sediment. Even when damp, it burned in a series of "puffs" of flame. After drying a piece slightly smaller than a rice grain, I put it on a piece of newspaper and touched it with a hot steel wire. It decomposed in a fraction of a second without burning the paper.

The yield from this procedure wasn't great, a gram or two I think compared to the theoretical 5+, but the material is definitely energetic. Just thought I'd share this method of using low concentration Hydrogen Peroxide.




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[*] posted on 22-6-2019 at 20:30


Interesting!
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[*] posted on 22-6-2019 at 21:57


In our shops "hydroperite" is sold. It is the complex of hydrogen peroxide and urea. Add some acetone and a few drops of HCl. wait, wash and dry.



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[*] posted on 24-6-2019 at 06:27


Interesting. More details like ratio, yield and procedure would be welcome.

TATP can be formed via air/light oxidation of diisopropyl ether, too.
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[*] posted on 24-6-2019 at 11:34


Quote: Originally posted by Rocinante  
Interesting. More details like ratio, yield and procedure would be welcome.

TATP can be formed via air/light oxidation of diisopropyl ether, too.


I used 30% H2O2. I'm talking about the experience of my friend. But the procedure is very simple. I think you should have an excess of H2O2. Make simple calculations. The aforementioned compound is sold as a big round tablet. You even do not need to smash it to pieces- only make it wet with acetone and drop HCl. Wait for one day, wash and dry.




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