Diphoronepentaperoxide (DPPP)

I suppose the loose definition of a shaped charge is those charges which
are not shapeless charges , but exist
in some form

Better for a charge to have some shape
and not just be a globlike amoeba

[Edited on 2-1-2005 by Rosco Bodine]

Please look at defintion of shaped charge

Bullshit! Vouching WTF?

Nope, you saw correctly.. sorry.

flaming.. I am pissed off!

second test plate

--- I have a word document (2.4 mB) which explains the process that used and aftermath of each test. This my clear up a few questions. I can email this to anyone who wants to view it.


[Edited on 3-1-2005 by Pyroz]

My file as a compressed PDF

DPPP detcord?

It's a thought but....

Ok, heres where i am in the synth...

I mixed:
100ml Acetone
105ml HCl Aprox. 31.5 conc

Heated at 75c for 2, 1/2 hours, liquid turned from clear to deep red, lost about 125ml of liquid volume.

Now my questions are:

Q: #1
I can put the solution in ice water at -10c outside, now how much HCl should I add just before the H2O2 to the solution?

Q: #2
Do I add double the first liquid volume (= 410ml of h2o2) or just double the current volume (= 190ml h2o2) ?

Q: #3
I've read that adding to much bi-carb or not enough will both destroy the batch, one by overheating, the other by to extreme a PH, so how much and how fast should I add the bi-carb, and can I just add the powder, or should it be in a water solution?

Thankyou for any help...I'm hoping to have some good results with the fresh Phorone

Edit: Light does pass through, but the red liquid is cloudy. I have the container sitting open on a shelf in a warm lit place. And so 5% HCl just before h2o2? ok.

[Edited on 3-1-2005 by Mickhael]

You lost that much of the original solution????
You should cover you’re reaction vessel or use a closed or sealed vessel of some form. Anyway add two parts 30% H2O2 to what you currently have.

You’re other questions have already been answered in this thread and the other related threads plus you don’t even mention the specifics like acid concentration, (not that it will affect much).

As for adding the sodium bi-carb, well I think it’s pretty much a given that it should be added in the form of a bi-carb/water solution.

Mickhael, I sent you a U2U message.

Ok, that makes sense...

I don't think you have read the recent posts

The current method of DPPP production is dropping the temperature down as cold as possible (-25c to -30c) in a freezer then slowly adding the H2O2 over the course of several hrs. This method yeilds the most amount of DPPP per ml. Heating is a nonissue with this current method.

too cold--- no good

Ok, I did miss some posts...sorry, I must have been trying to speed-read and skipped them Anywho's I'm going to try re-heating and bringing my remaining liquid (and covering the flask) down to the dark, thick quaility needed. I have noticed the sheeting of the liquid on the glass as I swirl it as well rosco, I can't see any seperation as of yet however...more results when I've completed them.

I might not be doing anything today, as its my 21st birthday wohoo!

Quote:

Originally posted by Mickhael Ok, I did miss some posts...sorry, I must have been trying to speed-read and skipped them Anywho's I'm going to try re-heating and bringing my remaining liquid (and covering the flask) down to the dark, thick quaility needed....

freezing phorone in ice brick works the best!

Drying?

IMO, I don't think temperature will affect the amount of formation of AP but it will affect the type of AP formed. The patent says 90% yield so we figure the other 10% has some amount of AP forming and the rest is waste, but since we and I don't think even the inventor even knows the exact reaction which is happening or how to separate and purify all the active chemicals from the waste, I don’t really have a solid basis for my conclusions or anything else to really back this up, as I see it there are two possibilities which I have derived from my experiments and observations.

One;
We cannot achieve anything greater than a 90%DPPP yield, no matter what, so we can either control the temperature to control the amount of trimer vs. dimer AP forming with our DPPP. And again, just because the temperature might not affect the amount of AP formed it obviously does affect the amount of DPPP formed and the time it takes to form it.

Or option two, we more than likely have to continue to conduct the necessary tests to understand the reaction fully and the exact chemicals involved and can find a way to purify and separate the active and waste chemicals. Then try to achieve a better than 90% total DPPP yield. Tracking down and making contact with Wolfgang Mackowiak still sounds like something that has to be done.


Rosco, the gas evolution is a problem with most reactions but it is only minimal, the only really visible gas evolution I notice during the procedure is during the initial mixing of HCl and Acetone and the peroxidation step, and the only gas I can really smell is chlorine, but that is what one would expect when attempting this reaction. The only other gases produced IMO is H, O, Cl, and these occurred only as a result of being lighter than the solution there in. therefore during the reaction the molecules split and the oxygen and hydrogen starts into accent and some of these gas molecules escape the solution taking some additional chlorine and *possibly* something else with them too.


Hideki, I now believe you when you say you and pyroz are two different people, it is quite obvious when reading you’re posts. You might want to try making a putty or paste by adding and kneading together 1 part NC (smokeless powder) with 1 part acetone and 2 parts DPPP. You can use a slight excess of acetone, as it will evaporate. And you might want to watch freezing you’re reaction vessel in ice, have you no idea how much pressure that puts on you’re beaker?

And pyroz, please note that Hydrochloric acid is spelled HCl, notice the lower case l.

Hey joey...

Well I know it took long enough for people to start to understand that 2 people can infact share the same IP address via the "magic router" ...... Vulture is a prime example of this.

Yes it is possible to get a 90% yeild, I have got this on several occasions only when I concentrated the solution at 30c for 1 week. patent says nothing about a yeild greater than 90% being possible.

Anyway, I agree that high temperatures affect the kind of AP if at all that co-form with the DPPP. So far I can tell you that concentrating your Phorone HCl at 30c or better for 1 week results in no AP being co-formed when using the cold formation method. All that forms as a result of this is pure brilliant sulphur yellow crystalline DPPP.
I think for safety's sake cold formed DPPP method is best since it decreases the risk of a caustic boil over or steam explosion, i think this is due inpart by too much Cl2 being given off at one time in the reaction.. I have seen a couple nasty ones
, I will tell you!

[Edited on 4-1-2005 by Matsumoto_Hideki]

Finally a mole weight.

breaking the law of mass action gets everybody busted every time

That sounds a bit better,,

Can anyone try the following test?

Try heating some crude DPPP with 1% CuCl in 5% HCl for 2 hours at 80 °C. After cooling extract any remaining DPPP with ether (or something else that doesn't mix with H2O) and crystallize. If the product is still explosive, you can be sure it's not AP!

This should decompose any RCOH(OOH)R type compound, like AP and AP-isomers. ROOR type compounds like DPPP should not be affected.

thank you rosco

There is no green during the Phorone production

Green! well that's great!

Hideki

Hold on there, pure phorone can be any color between yellow and dark green, so surly its precursors can be green?
How can you be so sure he's doing it wrong? I am actually interested to hear his findings and results. What did you do different then the rest of us Mickhael? Just because you're reaction seems different from ours DOES NOT mean you have done it wrong, it may just actually provide us with important information crucial to this thread, please share you're experiment results and conclusions in details

Ok, well heres what I did...

Sorry for deleting the previous post, it wouldn't let me add the file I wanted so just decided to repost rather then double post

Maybe I wrecked the batch...but here's what happened:


I started out with aprox. 100ml 31.45% HCl and 100ml of acetone. The liquids were at room temp. and I put them in a 500ml flask, and heated that in 1/2" of water in a metal pot, to a temp. of about 70C, and held it there for 2 1/2 hours...without a cover on. In about 1 1/2 hours, there was a loss of 100ml of liquid, and a transition from clear - yellow - orange - red, at which point it stopped changing over the course of the next hour. I removed it from the heat and sat it on a shelf over-night, no change was observed except that I was down to about 75ml liquid by then. Upon hearing that more heating was likely needed I proceeded to heat some more, at this point I put it back in the same pot, covered in saran wrap at the same 70c and left it there for about 5 hours, it then changed to the dark green...which is semi-transparent, that happened in about 2 hours, and after that no more changes could be observed, however when swirled it does exibit oily quailties (light oil) and light does pass through...but only as a lighter haze...not like like through water clearness at all. I hope thats all the details...

I might try cooling the liquid and then adding the h2o2 tonight...what say?

Ps: Just as one of my first test videos, here is 3 drops of MEKP in a tiny christmas light bulb, ignited by a 12v battery.

[Edited on 5-1-2005 by Mickhael]

Attachment: !3 Drops of MEKP.wmv (612kB)
This file has been downloaded 1418 times

Confusion Mickheal?

Alright, just to clear things up we are NOT making phorone here rather Phorone HCl which is DARK RED, Black oily liquid with a very punjent metallic smell ... yes the initial stages of the reaction are yellowish idicating the acetone is changing to Phorone but the phorone produced becomes phorone HCl in a matter of seconds while steeping the reaction at or near boiling point. (60-90c)

Mr. Pyroz I am glad you have discovered the high yeild DPPP synth produces. I have got up 75-80% without trying too hard and a couple times 90% when the solution is completely concentrated.
By the way you should get at least 760g - 900g from a 1L jug of Phorone HCL.
Are you cold forming your DPPP in an Iceblock ?

test the green stuff

Mickhael,
Yes please try to "peroxidize" the green solution, it could produce some very interesting results, or none.

Try cooling a few ml in a test tube and add H2O2 drop by drop until the reaction seems to stop, then right down everything you observe and report you’re findings. You say you’re left with less than half of the original volume of the starting reactant chemicals, so I am wondering what exactly you are left with???

Hideki, since you are reporting such LARGE yields, why not do some major blasting and testing to prove the VoD is 9000m/sec?

Very nice

Rosco, that’s exactly what we have all been waiting to hear, so it would appear that the top layer is waste material or worse our precious phorone dihydrochloride that has decomposed from the extended heating period. But you mention the color change of the top layer as well, which indicates a chemical change or reaction takes place somehow involving the top layer during the reaction.Hmmm, very peculiar.

Many more tests are needed to actually figure out what the top layer is and if it is important to the reaction. Another test where the top layer and bottom layer are separated, then individually added to the H2O2 should produce some more tantalizing info and results.

interesting indeed...I wonder of pure DPPP is really yellow or that is some contamination of sorts. It would interesting to know.

[Edited on 5-1-2005 by Pyroz]

It is uncertain at this point that my hypothesis is correct . It could be that
as the lower layer is peroxidized that
the upper layer will begin to disperse
into the reaction zone , *if* the separated upper layer is the same material as the lower layer and was just driven out and
separated from oversaturation during formation . That would be okay too
because it would also reveal that you
can know when the precursor formation is finished when the upper layer stops growing . So the results will be useful information either way it goes . But I have a feeling , just a guess really that
it is likely the decomposition product from
taking the digestion too far . There is a method to my madness the purpose of which should be revealing itself . The emulsion which I am churning for this reaction makes the entire mixture look like milk chocolate during peroxidation .
It is so well mixed it takes ten minutes to
stop swirling like smoke and even begin to stratify again , so the upper phase is getting every chance to redissolve and react further if it is going to do that .
Presently I have 100 ml (~ 1/4 of the total ) peroxide
introduced , stopping and examining the
results after each 25 ml . It takes a couple of hours to get a read on what happened and resume . Mainly I am not trying to get a good yield of DPPP , but to
see what the story is on the upper layer ,
whether or not it will enter the reaction .
Then obviously will be revealed a crucial piece of information which will define the
reaction endpoint determination for the precursor , so any subsequent synthesis aimed at producing the DPPP in a "clean" synthesis can be studied for learning the other factors that likely also apply to increasing the yields , temperature and addition rates are two things likely to affect the yields as well .

You want simple ? Okay here's simple .

Actually , the most likely reaction scenario to me seems that first three acetones conjugate , stick together , polymerize to form * triacetone dialcohol * ( a real compound that is something like a trimer of acetone ) It is similar to what happens with formaldehyde solutions when they are acidified , the formaldehyde polymerizes to paraformaldehyde , an indefinite number polymer , or three formaldehydes can combine into a trimer? (who knows!) called trioxane . The reactions of aldehydes and ketones are similar , so that fact lends support to my belief that the acetone polymerizes to a trimer , triacetone dialcohol . Then it further enters a * condensation reaction * with 2 HCl's , with the elimination of 2 H2O's , to form * phorone dihydrochloride * , which may be considered to be a
* derivative * of phorone because of structural similarity to phorone , while never requiring the formation of any phorone itself . Now that's what I believe happens , and yeah it is different from what the patent says in words about "acetone polymerizing to phorone" but hey here's the deal , phorone is not a polymer of acetone in anybody's book , if that book was written by anybody who knows the difference between polymerization and condensation reactions . Sometimes one can follow the other like here . Condensation reactions are water producers . And there is no way to get phorone from acetone without producing water . Anybody check me out on this please . So Mackowiak either goofed or the word translation is inaccurate , however the symbolic diagram showing the reactions is aligned with what I am saying likely happens . The 2 H2O's are sort of circled in bean shaped boxes on the * triacetone dialcohol *which is an acetone trimer . Even if phorone formed as an intermediate , before then combining further with 2 HCl's , phorone would still be an acetone * condensation product * and * NOT *any sort of " acetone polymer " BECAUSE acetone does not polymerize to phorone , but to diacetone alcohol ( the dimer ) , triacetone dialcohol ( the trimer ) , and even to higher polymers from what I understand may be possible , even to a solid plastic acetone polymer .....none of which are ever phorone So the best phorone could ever be is a
* polymerization condensate * , a "dehydrated polymer" of acetone is another way of stating this .
I have gotten sick of the focus and emphasis on "phorone" like it is the precursor for its own derivative , when plainly if the reactions are drawn correctly it is the dihydrochloride derivative of phorone which is the actual precursor .

Forget phorone ! Erase from your mind that DPPP comes from phorone !

DPPP no more comes from phorone than trinitrobenzoic acid comes from benzoic acid .

The structural similarity and similar names is where the similarity ends .

Cast out the phorone demon right now ! Save yourself from this "phorone illusion" ,
or I shall be forced to perform an exorcism to rid us of this pretender ,
this pseudoprecursor who deceives with subtlety and causes confusion
to the washer of test tubes and master of the molecular

This rant was brought you by reading and rereading the first stumbling half of this mammoth gargantuan thread one too many times

Alright, out with that word...

Results...if you can call them that :P

Jome...as far as I'm concerned the whole synth smells bad from start to finish...except perhaps the final product.

Now about my attempt to peroxidize my "green stuff" That was a complete flop...I cooled everything, and slowly 10ml at a time, added twice the h2o2...and absolutly nothing happened...so just in case I added 5ml of the same HCl as before...nothing. The only change of any kind was when I decided to add the bi-carb to be safe and the damn thing fuzzed and bubbled over the top. So whatever it was i made, it isn't the right thing for DPPP! I must have allowed to much to evaporate, and the reactions never finished properly to allow the correct precurser.

Of somewhat enteresting note however, I have started heating another batch of Acetone and HCl in the same flask as before, and there was a small bit of black residue left inside it, which I left because I figured I was working with the same ingredients so why not?
Anyway, I began the heating again, except this time slightly higher...at 75c...and in a larger batch of 400ml total (covered of course) Now withen just 20 minutes and no noticeable bubbling as with the last time...the whole container has changed from clear to dark red! The change was so fast in fact that it was almost straight to red before I walked back in the kitchen and noticed. So maybe its possible to seed the reaction, and get it started faster by having a little of previous batches in the new one?? Hmm.

1 Hour after applying the heat...(now staying around 80c) and the mixture is completely black! With no trace of red even when held up to a bright light. I think this 'seeding' idea might have some merit...anyone else have experience with this?

2 hours, 10 minutes - removed from heat and sat on a shelf uncovered, at 21c for the night, liquid is now thick, oily and very black! Woo, I think I've got it this time

[Edited on 5-1-2005 by Mickhael]

My solution has turned clearer after I evaporated acetone (and some water), that "upper layer" (same sticky substance that is on the jar walls) is hardly visible.

EDIT: Of course thats gotta mean that the tarry shit is no longer soluble when the acetone is evaporated, thats why it seperated out and formed an upper layer.

If I get what you are saying, rosco, then my solution has hardly even begun to decompose? Sounds great

[Edited on 5-1-2005 by Jome]

detvol .. how to prove? ideas?

The colour of the crystals

Testing the VoD

Ah i see what you are talking about..

Quote:

Forget phorone ! Erase from your mind that DPPP comes from phorone ! DPPP no more comes from phorone than trinitrobenzoic acid comes from benzoic acid . The structural similarity and similar names is where the similarity ends . Cast out the phorone demon right now ! Save yourself from this "phorone illusion" , or I shall be forced to perform an exorcism to rid us of this pretender , this pseudoprecursor who deceives with subtlety and causes confusion to the washer of test tubes and master of the molecular This rant was brought you by reading and rereading the first stumbling half of this mammoth gargantuan thread one too many times

In fact I also don't think you're correct about your phorone dihydrogen chloride theory. I don't have much time now to come up with a better explanation myself.

You could prove me wrong though if you were able to prepare the same black liquid from commercial phorone and HCl.

What???

Dodoman, what are you thinking teasing us like that "I think you're wrong, but I got to go" WTF? Please share you're thoughts about this?

Hideki, boomer's timer machine is a bit more complicated than that and takes some calculating and a hell of a lot of ingenuity to build. But it is possible.

phorone will not form Phorone HCl by itself.

I don't mean to tease anyone but the thing is that I'm having my term exams right now and don't have the time to do any testing.

Doodman WTF?

Hey why don't you try the synthesis before you attack all of our hard work, THANX

Quote:

Originally posted by Dodoman I don't mean to tease anyone but the thing is that I'm having my term exams right now and don't have the time to do any testing.

Yeah right , likely story . Probably wasting your time with failed attempts to make phorone and HCl react to form phorone dihydrochloride in an aqueous system which parallels the reaction conditions

Under these aqueous reaction conditions I don't think it will form via phorone either because it appears to be an unstable species which
wants to hydrolyze back to being just phorone or possibly something else . So trying to get phorone to form phorone dihydrochloride in this reaction system is
like sending it backwards through its reaction equilibrium to convince it to return to a more unstable form . It's like trying to make it defy gravity and float back down to the bottom layer in the beaker , and be a good little unstable emulsion of the hydrochloride , from which
unhappy home and marriage it demands to be free I think the only way we are getting the phorone dihydrochloride to form
in a dispersed "solution" or reactive quasistable microemulsion is that is where it is formed in a nascent state where it exists only according to a certain
half-life , a window in time and concentration where it is phorone dihydrochloride only for awhile and to a limited concentration , in an irreversable condition where it begins hydrolysis soon after formation . Can I prove that this is true ? No , but my own experiment suggests that it is true under the conditions for this particular reaction .
Under different reaction conditions you might be able to happily make phorone react with HCl to form phorone dihydrochloride any time you wish , if you have already formed the phorone by a different path . But the reaction conditions which we see in effect here place constraints upon what is logical to be occurring and what is not . If you have an explanation which seems more plausible , then hey I'm all ears , tell me about it

[Edited on 6-1-2005 by Rosco Bodine]

agreed rosco.

Going to make some detchord with DPPP.
hehe. Movie coming this saturday of homemade detcord sheering a tree or thick material in half. hopefully I will get some time to do this....
BTW this is 650g in the bag

DPPP Oxygen Balance?

Quote:

Originally posted by Matsumoto_Hideki Hey why don't you try the synthesis before you attack all of our hard work, THANX

OB

OB? just look at the chemical formula, if you can't get a good idea from that, then there is no hope for you

As Rosco has mentioned, a mix of DPPP and MEKP is deffinatly a must try.

Ok, I admit I was being lazy and was hoping someone would just give me a number ...I've got the chemical structure from the first page of the thread...so I'll jsut have to work it out from there, I never took any chemistry in school...so I'm just one step above clueless when it comes to most chemical theory...but I'm learning...slowly...lol

Sounds good Rosco.

That sounds like phorone!

Well I think so..