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Author: Subject: Diphoronepentaperoxide (DPPP)
Dodoman
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[*] posted on 15-2-2005 at 15:09


I asked a Phd at my university the other day to help point me in the right direction. He told me that the information in most chemical patents are not written in details (may even contain missleading information) so that noone would replicate it without direct contact with the inventor.

He also told me that phorone is most unliky to form due to the reaction of acetone with HCl but would rather produce mesytyl oxide. I looked this info in Vogel and it sais that the oppesit is correct. Any way the Phd told me that phorone is most likly to be produced from a hydroxide with acetone rather than HCl with acetone.

So I got this strange idea. Why not make phorone by the reaction of NaOH with acetone then neutralize the solution with HCl and add the equvelent amount to form the phorone chloride stated by the patent and then peroxidise that.

I'd very much like to know your thoughts on that Rosco. Personelly I like that idea and would probably try the synthesis by this week end.
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[*] posted on 15-2-2005 at 15:12


They both lead to the same product. I had a batch of NaOH/acetone and they both formed the red liquid, with same properties, and same smell. It got me pissed off so I dumped it. DPPP is not possible via the current method.
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[*] posted on 15-2-2005 at 15:22


Quote:
Originally posted by PainKilla
They both lead to the same product. I had a batch of NaOH/acetone and they both formed the red liquid, with same properties, and same smell. It got me pissed off so I dumped it. DPPP is not possible via the current method.


Thats very strange :o I thought you would end up with a ppt.

This means that the red liquid (I thought was phorone chloride) is not phorone chloride since no chlorine is involved in the reaction.

Thats disappointing :(
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[*] posted on 15-2-2005 at 15:33


..... Are people missing posts or moreover pages? It was obvious that no Ph-Cl was made when I made "DPPP" using H2SO4....



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[*] posted on 15-2-2005 at 20:10


Quote:
Originally posted by Dodoman
I asked a Phd at my university the other day to help point me in the right direction. He told me that the information in most chemical patents are not written in details (may even contain missleading information) so that noone would replicate it without direct contact with the inventor.
Quote:
That is total bullshit . If anything , patents for compositions of matter and chemical processes are about the most detailed disclosures you will find in the patent literature . They have to be detailed and full disclosures in order to have any legal claim to the things being covered by the patent . So like other legal documents the patents tend to be filled with fine print that covers every conceivable variation so the patent can hold up to legal scrutiny or challenges from copycats who would try to steal the technology and claim it is their own invention .
Quote:

He also told me that phorone is most unliky to form due to the reaction of acetone with HCl but would rather produce mesytyl oxide. I looked this info in Vogel and it sais that the oppesit is correct. Any way the Phd told me that phorone is most likly to be produced from a hydroxide with acetone rather than HCl with acetone.
Phorone is not the object of the synthesis , neither is mesitylene . I would be more interested
in the triacetone dialcohol as a precursor .
Quote:

So I got this strange idea. Why not make phorone by the reaction of NaOH with acetone then neutralize the solution with HCl and add the equvelent amount to form the phorone chloride stated by the patent and then peroxidise that.
Phorone is not what you want to produce . What you want to make is triacetone dialcohol , and then phorone dihydrochloride from reaction of the triacetone dialcohol with HCl . All of this presuming of course that you still believe that somehow the patent describes reactions which take place but under more complex conditions than are disclosed by the patent . You are presuming that maybe a trade secret process is involved , and the patents description is an oversimplification .
Quote:

I'd very much like to know your thoughts on that Rosco. Personelly I like that idea and would probably try the synthesis by this week end.
Okay try this theory . Acetone is converted in the cold and in the presence of NaOH to triacetone dialcohol in 10% yield according to a patent process , and isolated by distillation , the unreacted acetone recycled . The triacetone dialcohol is then converted to phorone dihydrochloride by reaction with HCl gas , or by reaction with aqueous HCl , whichever method works . The phorone dihydrochloride is then chlorinated with gaseous chlorine , and then peroxidized .
When you have gone through all of this elaborate work you probably will not have the desired compound , and will be saying to yourself that the trouble and expense would have been effort more rewarded in synthesis of something more straightforward . You see the appeal of the alleged " DPPP " was ease of synthesis . When you remove that appeal by having to resort to extraordinary methods to accomplish the synthesis , well how much appeal actually remains for the
" DPPP " in comparison with more well known and absolutely proven materials which are made straightforwardly by simpler methods ?
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[*] posted on 16-2-2005 at 18:02


What intrigues me about this proposal is that it looks so unlikely. Normally when crackpots come up with something, it at least has some intuitive appeal. What in God's name caused M. to ever even think that something like this could happen? Wouldn't he have at least considered the possiblity that the chlorines might not have, you know, read the instructions he gave them? He does have some chemical knowledge after all.

Also, if you're looking for phorone (and I think that's what you want if anything like the descibed process is to happen) you want acid conditions. These are well known to do it. (Many books mention this, none bother to give real references, so it must be common knowledge, right?)
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[*] posted on 16-2-2005 at 19:27


Quote:
Originally posted by GeomancerWhat in God's name caused M. to ever even think that something like this could happen? Wouldn't he have at least considered the possiblity that the chlorines might not have, you know, read the instructions he gave them? He does have some chemical knowledge after all.
Some , yeah , but not enough .
In chemistry , stoichiometry is where either the rubber meets the road ,
or the flight of fancy crashes and burns .
Somebody should toss Wolfgang a fire extinguisher so he can put himself out :D
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[*] posted on 18-2-2005 at 21:58
Ok then...now what


I've been pretty silent of late, mostly because of my work schedule. However I just wanted to say...that even though this supposed DPPP is not going to result in a high VoD explosive...nor anything super fantastic perhaps, we still have a synth for making a AP similar primary, with very high yeilds....fairly simply, this is worth something is it not? Also if simple recrystalization to rid it out water and make smaller crystal size is simple as well...I'd almost replace making AP by this instead. What say you all?

[Edited on 19-2-2005 by Mickhael]




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[*] posted on 18-2-2005 at 22:15


Crystals are anhydrous if rinsed with isopropyl and put in a really cheap and easy dessicator as well. So there is no need to recrystalize from toluene.

I dissolved some of my "DPPP" in toluene and no water precipitated out. I will leave some sitting in the open for a few days and see if it soaks up any water.

Keep in mind despite the water it still explodes with a fair amount of power anyway.


But yes, this method does produce a cheap, powerful HE primary explosive in large yields.

Out of curiosty has anybody tried to determine the molecular wieght? If you have a super accurate thermometer you dissolve a small amount in a solvent and measure the freezing point change, from which the mw can be calculated. This only works with very small amounts (<1g per 100g of solvent). I would do it but I lack the very accurate thermometer (within 0.01*C is used for this). The accuracy should be within a few percent.
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[*] posted on 18-2-2005 at 23:30


GB620498 is a more straightforward method for TCAP
and the product is more pure and obtained more quickly with less time and trouble .

Recrystallizing from toluene does more than just providing the anhydrous product ,
it also improves the density and the purity .

ETN 1 part and TCAP 2 parts makes a nice melt cast , but I have no information yet on the stability or explosive properties of the composite . I have an idea that there is perhaps an ETN / MHN binary eutectic that would be better as a binder for melt
casting TCAP , hopefully to form a fuse sensitive melt cast which would be similar to
" AP putty " , but have higher energy and not involve the shrinkage problems of putty . It is probably possible to get such a melt composition to work like putty , if the correct proportions and combination of materials is discovered .
Such a melt cast might make a decent detonator filler composition .
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[*] posted on 19-2-2005 at 18:48


Quote:
Originally posted by PainKilla
They both lead to the same product. I had a batch of NaOH/acetone and they both formed the red liquid, with same properties, and same smell. It got me pissed off so I dumped it. DPPP is not possible via the current method.


I tested it for myself and got a very diffrent result.

After refluxing NaOH with acetone for two hours the solution turned slightly yellow and I got an orange ppt that I'm assuming is phorone.

The yeild was very poor (it seemed to increase by cooling) and smelled like new air mattresses the kind they have in swimming pools.

The yeild was so dissapointing that I threw it away but I'll be trying it again latter this week.
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[*] posted on 20-2-2005 at 17:38


I just left mine at room temp for a few days. The precipate is NaOH (I used solid NaOH not in solutiion)

[Edited on 21-2-2005 by PainKilla]




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[*] posted on 20-2-2005 at 19:04


I also used solid NaOH but that didn't preciptate, it formed a lower oily (white) layer that solidified on cooling.

The preciptate was suspended above it and was (orange) in color.
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[*] posted on 20-2-2005 at 19:06


I didnt heat and the NaOH was "dyed" an orangish color. I dont think it actually went through a reaction.



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mad.gif posted on 7-3-2005 at 12:27
hello there


I am currently doing research for university concerning these organic peroxides. They are quite interesting group of materials. Anyway I have to inform you guys that DPPP is difficult to understand at best. I have tried serveral ways of making it but all have seemed to obtain a derivative of DPPP but not pure DPPP itself. It looks as thought this reaction must take place in a vacuum chamber with no air present as high amounts of mesityl oxide co-form with what what seems to be a ~pentameric form of acetone peroxide with only trace amounts of the target phorone peroxide. Hence the punjent odor that is left behind when this substance deflagrates. That is phorone you smell. :)
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biggrin.gif posted on 7-3-2005 at 12:48


I was wondering when Hideki would show back up. Maybe I’m just overly paranoid but you remind me of a certain “brain damaged” individual.:P

What is being formed is not a "derivative" of DPPP and as far as I know there is no such thing as an acetoneperoxide isomer containing five peroxide bonds, where is the proof to back up these claims? You haven’t even drawn a plausible reaction scheme to show how you think this reaction is carried out. Let’s see some proof, or at least a theory we can shoot down or something.

Your claims mean shit without evidence to back them.
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[*] posted on 7-3-2005 at 23:02


Someone's pushing the DPPP scam over at the Amateur Pyrotechnics & Chemistry Forum too. I wonder if it's our 'friend' here...



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biggrin.gif posted on 17-3-2005 at 12:34
HDK isn't Hideki rather H&raquo;D&raquo;K from RedOrchestra online


Ya well I am not "hideki" sorry. I am just a passer by.
NONE of you have actually proven anything either on this little DPPP thread either so..... whats your point?
All people on this thread believe the Bullshit patent that was rigged on purpose to keep people away from it. This precusor material needed to be formed under tightly controlled conditions, unlike most people on this thread who beleived otherwise. It seems air cannot be present when Acetone is digested by HCl, but both materials must be in a gasious state in order to react properly!!! 2:1 HCl vapour to Acetone vapour. This condensed material is a ***dark green material** rather than dark red-yellow you were all getting. This is the material you peroxidize. The other was a highly explosive mesitylene-phorone derivative. as well as a whole host of acetone-peroxides. The ending DPPP is chalk white and acts very simularly to AP but is much more dense. I sure hope you skeptics are brave enough to try this, or you could hide behind all the BS theory floating around the web or textbooks... .
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[*] posted on 17-3-2005 at 12:41


Before you go critizaing all the hard wrok everyone ahs done, where are YOUR results. I want to see a rxn mechanism not some "o yea i seen it happen!!111." NOONE wants you here so leave.... espeically with dumb accusation that have no validity.

On top of that, who really wants to bother with this if :
Needs to be done with no air, strict conditons, pure chems etc....

Does that not defy the entire point of a powerful and SIMPLE primary. Id rather make an existant explosive that is proven and true.

If this is such a great esplosive why dont you go patent it and stop bitching to us because noone cares.

O yea, and I just looked on red orchestra online and um... your not a member... hideki!

[Edited on 17-3-2005 by PainKilla]




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Chris The Great
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[*] posted on 17-3-2005 at 18:28


Um, go easy on this guy! 99% of the info is this thread is stated by those who did the experiment, no other info provided. And with that info we've made a new primary explosive, even if it isn't DPPP or is just some larger AP molecule, it's still different. And no one has provided a reaction mechanism, it's all been just speculation so far. You don't need to have a reaction mechanism to prove that a reaction works, you only need it to understand why the reaction works.

I think that this is highly interesting, if I can I will cobble together something to attempt this gas-phase reaction.

What are the conditions and set up for your experiment? It has been stated before in the thread many times to provide a large amount of detail on exactly what you did to get your results. Can someone use an inert atmosphere (ie propane) instead of having a vacuum, which I assume is what you used. Even better can you provide a sketch of the reactor vessel and setup you used, this would be a great help for anyone attempting to reproduce your experiments.

Many people care about explosives that need strict conditions, etc to be made. I certainly do, making a new, very powerful HE is definatly an interest to me, and if it is challenging to do even better. Just throwing something out the window because it's 'hard to do' is not science, it's almost forced ignorance. There is no reason to assume that because the reaction is hard to do it is completely useless and no one should even think about it.
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[*] posted on 18-3-2005 at 09:29


Quote:

Just throwing something out the window because it's 'hard to do' is not science, it's almost forced ignorance.


???

Read the whole thread and the conclusions of so many different contributors.
This dream is over. - Try to accept it.

[Edited on 18-3-2005 by BASF]
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[*] posted on 19-3-2005 at 14:40


I have read the whole thread. He has offered a new route which has not been explored, tossing it out the window is not the way to go about it. Whether it produces DPPP is unkown, however, just going "Oh, he must be Hideki, ignore him, after all he's offering some new route but it's hard so lets just pretend everything he says means nothing."
Nothing has been tried that is even similar to performing a gas phase reaction in vacuum/inert atmosphere, and perhaps the method may work. There is only one way to find out. So, it looks like I'm going to be making HCl(g) and acetone vapour generator and inert atmosphere reaction vessel over the next for days.

I am thinking of a stainless steel pipe, heating up using a heating element or something, filled with a butane atmosphere. HCl will be generated by dehydrating HCl, acetone by heating. The pipe will lead into a gas trap (water). I am thinking of a pipe length of maybe 4 feet, and a 1/2 inch diameter. I have some old stove heating elements I can use to ensure the reaction proceeds rapidly enough so that it can take place in such a short pipe. If I end up with something different, I won't be able to peroxidize it as I have no H2O2, but it will at least determine if this approach may work. If not I get experience in building a reaction vessel for gas phase reactions under inert atmosphere.

EDIT:
Hmm, PVC pipe would probably work better. It should be fine up to about 160*C according to the limited information I could find, though it's ability to resist impact drops off sharply above 40*C. If I keep the internal temperature at about 100*C I should have no problem. This is mainly because I have 5 feet of PVC pipe and no stainless steel. The acetone will not attack the PVC as it is reacting with the HCl and will not be able to enter the liquid phase and start dissolving....I hope.

[Edited on 20-3-2005 by Chris The Great]
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[*] posted on 20-3-2005 at 01:56


The thing is he didnt give any results. Theorizing about what COULD happen vs what WILL happen is two totally different things. Sort of like C + H2 --> Benzene. Its not happening.

The same results can be achieved if one leaves there H+/acetone mixture for a while, it turns green. Does anyone care, no. Because it doesn't do anything new. This isnt one product being formed, its a slew. Obviously in presence of H2O2 most react to form this peroxide. It also doesnt seem to matter how complex or simple it is (acetone vs phorone) as they all seem to make the same thing or near same thing.

And I never said anything about it being too hard. I basically said that there is a point unto which something is not worth pursuing. I understand maybe for the adventure of it... but seriously think about what you are talking about, you are going to react Acid vapors with a flammable solvent in an enclosed space.... thats really smart. Of course, assuming we are still alive, we can then try to add H2O2 and make the EXACT SAME THING as before. Oh damn, I forget this was to be done in a oxygen-free enviroment (assumption from the vague post) OK well, you try it and tell us how it goes.

If you really want to get some REAL results stop playing around with acetone condensation products order some damn phorone and see for yourself that it doesnt peroxidise. If it does, kudos to you, but Im almost postive that it doesnt.

On another note, what is the point of making compounds which you do not the properties or anything of anyway. I would like to know the structure mechanism of reaction etc... There is like 15+ different condensation products from acetone, I want to see which react. I bet you its just diacetone alcohol forming a peroxide, via AP mechanism, except with less water and more direct reaction. Regardless, I am disregarding anything past Rosco's results because THAT was *DPPP.* It was proven to be false as per the patent. If you want to experiment with some random new things, I would start a new thread because its not DPPP.

O yea, Nitrous kicks ass :). Any incoherency is blamed on it ;). Errr.... I mean not nitrous.... :D



BTW: I hve came up with resalts! THis was form a LAB!!! Heating acetone with Chlorine at 500C in a inret atmo$phere (NITROGEN) makes phorone, I KNOW because its GREEN and it has no phase, its just material!!!!!! *sarcasm*

[Edited on 20-3-2005 by PainKilla]
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[*] posted on 20-3-2005 at 15:14


Quote:
Originally posted by PainKilla
If you really want to get some REAL results stop playing around with acetone condensation products order some damn phorone and see for yourself that it doesnt peroxidise. If it does, kudos to you, but Im almost postive that it doesnt.


That fact was already well established in the beginning of the thread, and it was determined that any route that lead to DPPP would have nothing to do with phorone at all, but would be through derivatives of phorone, which would not be formed from phorone itself.

Quote:
On another note, what is the point of making compounds which you do not the properties or anything of anyway. I would like to know the structure mechanism of reaction etc...


Once we find a successful route to something that seems to be it, we can then look back and try to figure out what is going on. We can do that by determining the molecular weight of this new product, it's atomic structure, our observations of the reactions which led to it, and then figure out what the reaction is from that information. We obviously can do none of that until we have actually made the product.

Quote:
I bet you its just diacetone alcohol forming a peroxide, via AP mechanism, except with less water and more direct reaction.


You are betting, and I am going to keep experimenting and see if I get any closer to the truth. I don't really care if I don't ever end up with something useful, I will then know that by doing such and such, you will not end up with something useful. *Insert overused quote of Edison and lightbulbs here*
As of right now, nothing about the reaction is known for sure. None of it, other than that the acid and acetone react, and when it is peroxidized, we get an explosive. We don;t know for sure what the reaction is. We don't know for sure what the end product is. Sure, we've made some good educated guesses, but none of them have been confirmed for sure by good hard evidence such as molecular structure and weight, etc.

Quote:
Regardless, I am disregarding anything past Rosco's results because THAT was *DPPP.*


No, we are not completely sure exactly what it is, although it appears to be a derivative of acetone peroxide, or something else. This has not been established in fact.

Quote:
It was proven to be false as per the patent.


I believe this was established perhaps around page 10 of the thread, but we all kept going, to see if we could perhaps figure out what we where doing. I don't see how it's any different right now.

Quote:
If you want to experiment with some random new things, I would start a new thread because its not DPPP.


The general concensus (which you are a part of) is that NOTHING in this thread ever was DPPP anyway.


But I don't see what this argueing has to do at all with science. You have stopped and figure you know all the answers, I have decided to keep experimenting because we DON'T have all the answers. I don't care if all I end up doing is showing for sure that we only have pentameric acetone peroxide, or a slew of different chemicals, or true DPPP or something completely different, the point is we don't know for sure, and I want to discover answers to these questions. Now, if someone has found the answers with great, undisputable evidence, I'd love to see it and be proved wrong, but I'm sure that no one has those answers.
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chemoleo
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[*] posted on 20-3-2005 at 15:36


Quote:
By the way, in Gattermann I read today that acetone reacts in the presence of HCl-gas to mesityl oxide and phoron.
This may be another thing to try, to bubble HCl gas into acetone!
According to Beyer&Walters Book on Organic chemistry, mesityl oxide is a clear liquid that smells slightly of peppermint (!!).
Phorone is, on the other hand, a yellow substance that has a melting point of 28 deg C !!! In this book it also says that it is obtained by reacitng HCl gas with acetone, while mesityl oxide is a side product.


May I just remind you of that. Two independent sources describe this route to phorone. Not wanting to hype anything, but maybe that's something that shouldnt be forgotten, to try this under anhydrous conditions.




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