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Rosco Bodine
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In a test of my "scorched" precursor , I added 30 ml acetone and swirled the mixture . Within 5 minutes the color has deepened to a purer
tint and the mixture is forming the bright yellow film similarly as was observed in the first experiment .
The indication is that the ratio of acetone to HCl is important . Very unusal to "thin" a mixture with acetone and observe a viscosity
*increase* but that is exactly what it appears to do . Anyway , I am wondering whether to ditch this batch and adjust quantities , or try to
peroxidize it . I am trying to get a repeatable process worked out with no snags like this to complicate matters .
Aside from the unknown effect of the bit of peroxide I added , the HCl amount seems to contradict j-scan's 2 to 3 volume amounts for acetone to
HCl . What adjustments or refinements if any have you found useful during the batches you have completed ?
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Mickhael
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Ok, hope my math is right, OB =
Early on in this threat it was suggested that its hexa, not penta, and I haven't heard that disproved...so:
Diphoronhexaperoxide's OB = -255% O2. As far as I can tell from counting the mol's of the C, H and O2.
What do you all think? Pretty deficient for its power...how does that work?
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chemoleo
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I think not too many pages back, someone tried to make the peroxide with Sigma phorone , and this didn't seemingly work.
Thus it seems possible, if not likely, that pure phorone on its own is not a suitable substrate for peroxidation.
Also, I'd assume that the chloro derivative of phorone is more reactive than phorone on its own.
Never Stop to Begin, and Never Begin to Stop...
Tolerance is good. But not with the intolerant! (Wilhelm Busch)
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Dodoman
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| Quote: | Originally posted by chemoleo
I think not too many pages back, someone tried to make the peroxide with Sigma phorone , and this didn't seemingly work.
Thus it seems possible, if not likely, that pure phorone on its own is not a suitable substrate for peroxidation.
Also, I'd assume that the chloro derivative of phorone is more reactive than phorone on its own. |
Which I think is in favor of my reactions  . I don't think that these
reactions are correct anyway but they seem as a possiblity never the less.
I think the key to understanding the reaction is analysis of that black oil. And I shall do that when I have the time. I think spectral analysis using
NMR, UV and IR should do the trick .
I'll try to make friends with professors at my universty which could probably help me with this. BUT NOT BEFORE I FINISH MY EXAMS. Which is in 10
days .
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Rosco Bodine
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The "black oil" which accumulates as an upper layer during a long heating of the acetone and HCl mixture actually only looks black against
the dark red lower layer . When separated , it is a brownish yellow resinous material which leaves a light tan colored stain on white paper towel .
It is extremely adhesive in nature and has an odor and other properties something like a vegetable oil which has been partially polymerized from
overheating and then gells upon cooling .
It is insoluble in alcohol , but dissolves readily in acetone . I believe the composition is predominately phorone with some impurity of triacetone
dialcohol and higher acetone polymers . The material would seem to make an excellent component for paints and glues . It sticks to glass tenaciously
like urethane or epoxy resin , really gummy stuff , and in thin layers exposed to air it gradually hardens much the same way as does linseed oil .
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Chris The Great
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I remember getting in the -155% range for it's O/B, I think. I remember that it was within a few % of APs O/B.
I is more powerful because it releases it's energy much faster than AP.
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Matsumoto_Hideki
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great now we can try and undo all our work. BUT!!
Hey guys have you checked on the Organic sytheses site for phorone production?
look at this http://www.orgsyn.org/orgsyn/chemname.asp?nameID=33576
quote:
There are two general methods for the preparation of mesityl oxide: the action of condensing agents (hydrochloric acid, etc.) on acetone, 1 and the
dehydration of diacetone alcohol. 2 The action of acid condensing agents is very unsatisfactory; the yields are poor and considerable quantities of
**phorone and similar substances** are invariably produced.
this other substance this person was reffering to is Phorone HCl?
[Edited on 7-1-2005 by Matsumoto_Hideki]
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Rosco Bodine
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Organic Syntheses has a primitive idea about hydrazine sulfate synthesis too .
They should really update some of their labs
But yeah if you keep cooking the stew . so to speak , the stew being the acetone and HCl mixture , that upper layer that separates is likely chock
full of phorone , if phorone is what you want . Of course that needs to be confirmed for certainty .
Anyway I have a clean batch of acetone and HCl reacting , in which I made a far less excess acidity than the earlier batch that I think I scorched
with too much acid .
I remembered when I was observing the first sealed bottle experiment that I had the idea that this reaction is pH sensitive , so I tried to measure
very carefully the acetone and HCl to achieve
just a 3% excess of theory of HCl to acetone . The results are distinctly superior in terms of color development and the purity of the color is
striking at
3 1/2 hours . The color is that of "ruby glass" pure red , brilliant red , not any "tea color" to this batch . I have a good
feeling about this ratio just based on
the clarity and depth of color . If nothing else it is pretty . What I used was exactly
112 ml acetone and exactly 105 ml HCl 31.45% , mixed and allowed to stand in a sealed bottle for 1 1/2 hours without supplemental heating , and then
heated for 2 hours still in the sealed bottle , in a 75 C water bath . I have removed it from the bath , and am allowing it to cool and stand
overnight .
I must say that quite different reaction rates and color developments are being observed with small changes in the acetone to HCl proportions , so
obviously
some exactness is needed about these
measurements and reaction times and temperatures . And then when to proceed with the peroxidation and at what rate and temperature and other
conditions are important also . This synthesis is not one which is likely to work across a wide range of conditions ,
as is the synthesis of regular AP . So please , those of you who are having success make careful and detailed notes of what you are doing and what
you are getting out the other end as yields .
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Mickhael
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Ok, my first official DPPP (or is it DPHP?)
Alright well I to do not believe that the top filmy layer has anything to do with forming the peroxide, here are my results and why I think that:
To 100ml of chilled to -15 "black stuff" I slowly added 200ml almost exactly of h2o2, by the time I had added a third of my h2o2, the
tempature had risen from -15 to +5! So I stopped adding, and left the mixture in the freezer for about a half hour, when i came back, the
"liquid" had turned into a solid mass of yellow crystals, however there was chunks of black film, which seems to slowly harden, still in the
mix, and no matter how much I mixed it (hand stirred) the film never seemed to break up and just stayed in little dark flakes/chunks, I then slowly
added the rest of the h2o2, I don't know how many more crystals formed, but when I was done, I left it for another half hour to make sure things
were done percipatating, the container was still pretty much stuffed with crystals, I'd say at least a 90% batch, I then dumped the whole thing
slowly into another larger glass container filled with bi-carb, I think I lost some product here, it became all foamy and filled with air bubbles, I
then strained and washed several times with fresh water (through a coffee filter) and now i've spread it out on newspaper to dry, I'd say I
have about a half cup of solid crystals if they were packed tight, I haven't weighed yet, since obviously they are not dry  ...So, all in all a pretty good turnout!
Quick question however, since this is my first high explosive...and only second batch of crystal peroxide: I have it drying on newspaper, how safe
will it be to collect after its dry? and how can I get it into another container without scraping it at all? I want to mix it instantly with
MEKP...but I also want to be able to move it around safely, any suggestions so i don't kill myself with this stuff. For its power, I probly have
enough sitting beside me to destroy the room I'm sitting in....Eeep!
[Edited on 7-1-2005 by Mickhael]
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Pyroz
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There are many variables that we cannot be sure about until we do further testing.
My questions that I'd like answered: i keep harping on:
•is real DPPP yellow or is that unreacted material mixed in with DPPP.
•while the power of this substance is substantly more powerful than AP or MEKP/AN what is the yellow materials true VoD?
•how much more powerful would DPHP (hexaperoxide) than DPPP(pentaperoxide)?
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Dodoman
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| Quote: | Originally posted by Pyroz
•is real DPPP yellow or is that unreacted material mixed in with DPPP.
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I think that's its color because when you wash it with water its color doesn't change. This means that if there are any imuprities at least
they are not water soluble.
You can try recrystalizing it from acetone. I don't think that's a good idea though Because if its similar to AP (forming diffrent isomers
at diffrent tempretures) then that would be a problem regarding both the physical properties of the product (color and stuff) and also senstivity.
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Rosco Bodine
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The color of the still wet DPPP which I am getting is a light yellowish tan . The shade is about the same color as the default color scheme for every
other message posted here on this page , the background color .
Many more experiments will be required before these ideas can be regarded
as conclusive findings about the synthesis of DPPP , however I am willing to
share some early observations so that others may do their own tests
to see if these ideas square with their own results .
First of all the molar ratio of HCl to acetone is important , as is the time and
temperature they are reacted before the peroxidation . It is the soluble or
finely dispersed portion of that digested acetone HCl mixture which will be
reactive with the peroxide . The resins or oils which may precipitate represent
a loss of precursor and should be filtered before peroxidation using a double
thicknes of coffee filter wetted with water before filtration . There isn't much
of anything to be gained by excessive temperatures or extended hours of heating
the acetone and HCl to the point it becomes so dark as to contain suspended
or separated resinous precipitate . Such "black oily" material will not be converted
to DPPP , but will only precipitate as clumps of sticky insoluble goo contaminating
the more and more aqueous peroxidation mixture . This is why filtering before
peroxidation is a good strategy for removing the bulk of such suspended material.
Molar ratio of HCl to acetone should be 2 to 3 , with only very slight excess of theory
for the HCl on the order of 3 % seems in the ballpark . Using more HCl or heating
the mix too high or too long causes resinous insoluble products to precipitate and this
should be avoided to the extent possible . Exact optimums for ratio and times have not been yet determined so this can be an area for close
measurement and comparison of
results .
The greatest exotherm during the peroxidation occurs during the addition of the first
10 to 15% of the total peroxide to be added . This initial peroxidation should be done
with efficient stirring and slow , even dropwise addition of the peroxide . I have used no
cooling during this initial addition , or only a shallow plain water bath , and allow the
stirred mixture to heat up from the exotherm to about 65 C . The addition of peroxide
is stopped and then ice is added to the bath to cool down the mixture to 10 C , the stirring
being continued the entire time , and then addition of the peroxide resumed more rapidly
at such a rate as to maintain about 15 C to the end of the addition . The stirring is continued for thirty minutes after the end of the addition and
stopped . The crystals
will form a floating raft , from adherent bubbles of oxygen which make them buoyant and
may be skimmed from the surface using a plastic spoon and transferred to the filter .
The crystals should be rinsed on the filter , and neutralized with only dilute alkali . Strong
ammonia will decompose the DPPP . The material is very aromatic and the vapor is irritating
and perhaps intoxicating , and should not be considered harmless until more is known .
[Edited on 7-1-2005 by Rosco Bodine]
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Pyroz
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Rosco that jives with what i have experienced
[Edited on 7-1-2005 by Pyroz]
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Rosco Bodine
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Great to have confirmation on those things . The major points of the synthesis
are now known , and all that remains really are the tweaks and refinements
that are likely to be discovered from many
experiments . This whole thread will probably be reduced to a few paragraphs
on one page when the optimized synthesis tried and true is set down in
its finished details . I was looking back
at this thread and it is like a 200 plus page transcript if printed . This has been one
BIG ASS SCIENCE EXPERIMENT Somebody ought to drop an e-mail to BASF , aka
Hoffman LaRoche who started the thread and see if he has
been aware of the recent developments since the mid December post by Dr. Boom
which breathed new interest into these DPPP experiments .
Where is Dr. Boom exactly anyway ?
I sort of have this mental picture of
Dr. Boom having catnapped Mackowiak's
kitty , and then a call is made to Wolfgang
saying
" Okay listen up professor , we have your cat and it is okay for now anyway . So give up all the lab notebooks and the patent dossier ,
or else the cat gets it " 
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Matsumoto_Hideki
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Dr.Boom returns as a re-incarnate
Well I will tell you Pyroz is Dr.Boom
Pyroz has many cats and trhey are all fucked up from DPPP vapours some are even some bristle with their own electric current. unfortnate no German
wolfgang cats though. ie) none that could lend a paw to your experiments anyway.
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Mickhael
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?
Just wondering, how long does it usually take to dry peroxide crystals? I've had the DPPP sat out in a 70f room for 24 hours now, and it seems
quite dry, however a test proved it to not make a very loud bang, so obviously its not dry, whats the usual number of days before dryness reaches its
max?
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Pyroz
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| Quote: | Originally posted by Mickhael
Just wondering, how long does it usually take to dry peroxide crystals? I've had the DPPP sat out in a 70f room for 24 hours now, and it seems
quite dry, however a test proved it to not make a very loud bang, so obviously its not dry, whats the usual number of days before dryness reaches its
max? |
Even slightly damp DPPP will explode with considerable energy. What did you pack the material into? Was it compressed tightly or was it in loose form?
You my wish to try the rifle shell casing test and make a blasting cap from it!
[Edited on 8-1-2005 by Pyroz]
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Mickhael
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| Quote: | Even slightly damp DPPP will explode with considerable energy. What did you pack the material into? Was it compressed tightly or was it in loose form?
You my wish to try the rifle shell casing test and make a blasting cap from it!
[Edited on 8-1-2005 by Pyroz] |
All I did was put about a 1/2g into a film container (yes it was loose) and stick a fuse into it, with a little papertowel to hold it in the bottom,
it made a sharp crack, but nowhere near the noise the same amount of MEKP makes...which led me to believe it needs quite a bit of drying still.
I take it from your compression question, that compressing it helps alot? I'm hoping to mix it 50/50 with MEKP and test that shortly.
I unfortunatly do not have access to any rifle casings, strange as that may sound, rifles are pretty uncommon around me, so unless I could get to a
range...or find someone who has them, I'm out of luck.
Do you have any idea what would happen if I put some slightly damp DPPP into MEKP? would it desolve the crystals and seperate the water out?
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The_Davster
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Rosco, I tried a slight variation on your method of reacting the HCl and acetone. 26mL of HCl and 28mL of acetone were mixed at room temp (18C) in a
250mL flask. The flask was outfitted with a 2 hole stopper with a thermomehter in one hole and in the other hole was a 3' lenght of glass
tubing. Upon mixing the HCl and acetone in the flask the temperature shot up to 36C. THis was allowed to sit at room temperature for 1.5h, at the
end of which the solution was only very slightly yellow. Still mostly clear. What color was your solution after sitting at room temp for 1.5h,
Rosco? This flask was transfered to a hot water bath. Since I was doing this outside and had set up the bath earlier when the flask was put in the
bath the temp of the flask dropped to 15C. over a period of 20min the temp of the hotplate was adjusted to end up with a fairly constant temperature
of 60-63C. Acetone condensing was noticed at around 60C in the piece of glass tubing. The acetone stopped condensing after around 20 min. Total
heating time was just under 2.5h( 30 min @ 55-65C +2h@60-63C). After this time The solution was an incredible deep red, like you Rosco, no tea like
color. If one swirls the flask the residue on the flask walls appear deep yellow. There was a very slight slick of oily substance on the surface.
When peroxidizing this what is a good temp to keep it at maximum? I think I will try 0C or 10C. Any ideas?
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Mickhael
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| Quote: | | When peroxidizing this what is a good temp to keep it at maximum? I think I will try 0C or 10C. Any ideas? |
Just for the record, I peroxidized mine at -15c, and it seemed to have a perfectly good yeild *shrugs* maybe it could be better, but the container
seemed packed with crystals.
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Pyroz
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thats how you do it! Low temperature synth seems to do fine.
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Matsumoto_Hideki
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Hum hhuuum, excuse me but !
Pyroz, I have to admit damp DPPP will explode but not anything like when it is dry. When I compress it I always moisten it with pure distilled water
but that water (slight moisture) is expelled when I compress my caps or explosive devices... I would recccomend anyone useing large amounts of DPPP
in metal containers to give a good solid coat of urathane to the inside of your device to prevent any sensitization by any AP impurties. I would hate
to see what a 150g - 250g shaped charge could do to a person if it prematurely detonated while you were holding it!
A FUCKING MESS! 
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froot
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After browsing this wickedly immense thread I cannot seem to find any confirmed info on the sensitivity and storage stability of the products being
made here. It has been mentioned that it gives off an odour which indicates that it probably decomposes during storage like most other org. peroxides.
Good storage stability was mentioned in the original patent,-hmmmm.
Shouldn't you folks be making this 'relatively untested and therefore mysterious' explosive substance in much smaller sample
quantities????????
Im sure nobody here wants to have to type their posts using a pen in his mouth.
Otherwise good work so far.
We salute the improvement of the human genome by honoring those who remove themselves from it.
Of necessity, this honor is generally bestowed posthumously. - www.darwinawards.com |
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Matsumoto_Hideki
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Well to answer your question
Actually it does store well over long periods of time and is stable at room temperature. I have even taken this material to 70c without it subliming
or decomposing. By the way the smell does fade after a while.
If you take DPPP up to 170-200c you risk detonation and or if you were to hit it hard with a hammer on concrete about 30-40lbs of force. I am still
investigating DPPP's sensitivity to metals ie) copper.. and alloys like brass. So far brass will not sensitize DPPP as I have discovered in
making many blasting caps with it. Still I am careful while loading..
So far nothing much to report... still determining this thought.
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Joeychemist
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Smarten up man!
It does react with brass, and copper and every other metal I have tested it on. Don’t you think you should actually do both short and long term
tests in order to see if it reacts with metals before you go telling people it is ok, Christ man! What if it’s going to ignite after a moth or two
of being “seemingly dormant” and kill a kid that read you’re post saying that it’s perfectly fine to store DPPP in brass for a month or two?
Hideki you really need to stop making all these assumptions before someone (YOU) gets hurt. I mean fuck man. It’s bad enough that you’re making
hundreds of grams of a *PRIMARY* explosive. But to do so with out the proper knowledge is *STUPID, NEGLEGENT, and IMMATURE*
You ask anyone here if they have ever made that much of a primary explosive of which they know *NOTHING* about and see what they’re answer is.
Before you hurt yourself or even worse someone else, slow the fuck down and smarten up PLEASE.
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