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chemoleo
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Hmmm - it seems you are posting exactly the same thing at the E&W forum. I don't quite understand what the significance of this is.
It doesn't prove or disprove anything.
Chloroacetone - maybe this is a later product that makes you all cry literally, but certainly NOT during the reaction between HCl and acetone (having
done it myself - it's harmless).
Btw, I found that leaving the mixture of 37% HCl and acetone for one week at room temperature would still produce this dark red oil, visibly no
different to the mix that was heated at 65 deg C for 90 min.
I am tempted to believe that the production of the 'DPPP precursor' is a temperature-dependent process, I.e. if heated, it will go faster,
if not heated, it will just take its time (a week). But the reaction is the same nonetheless, no? I will test for the appearance of water-insoluble
oils that somone described above, using this particular mixture.
Nice and proper science 
Btw, if someone is interested as to what conditions are NOT to be employed to get 'DPPP', here is an attachment on the formation of acetone
peroxides in the presence/absence of acid. THanks for forwarding this Bromic
It gives a full mechanism for which conditions are required for producing AP, and, more interstingly, the conditions required to form acetone
peroxides which are NOT cyclic. Check it out.
If someone pursues this. please create a separate thread, as this thread is big enough as it is!
Attachment: acetoneperoxides.pdf (582kB)
This file has been downloaded 1424 times
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Rosco Bodine
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| Quote: | Originally posted by chemoleo
I don't quite understand what the significance of this is. It doesn't prove or disprove anything. |
The significance is that with elevation of temperature of a mixture of H2O2 and HCl that chlorination activity increases , and
chlorination is what is being done to the precursor to form the next intermediate for the DPPP . | Quote: |
Chloroacetone - maybe this is a later product that makes you all cry literally, but certainly NOT during the reaction between HCl and acetone (having
done it myself - it's harmless). |
Right , it isn't the reaction of the acetone and HCl , but the
reaction of the H2O2 and HCl which is producing chlorine that then reacts with the acetone to produce chloroacetone . This production of
chloroacetone is analogous to the production of pentachlorophorone , only the precursors are different . The chlorination mechanism is the same
. | Quote: |
Btw, I found that leaving the mixture of 37% HCl and acetone for one week at room temperature would still produce this dark red oil, visibly no
different to the mix that was heated at 65 deg C for 90 min.
I am tempted to believe that the production of the 'DPPP precursor' is a temperature-dependent process, I.e. if heated, it will go faster,
if not heated, it will just take its time (a week). But the reaction is the same nonetheless, no? I will test for the appearance of water-insoluble
oils that somone described above, using this particular mixture.
Nice and proper science |
That squares
with what I am seeing too . Only with the ratio of 95 ml HCl 31.45% to 100 ml acetone , my sealed bottle is reaching the "cloud point" at 3
1/2 days , 84 hours , and then the surface accumulation of insoluble oily byproduct begins . I know the reaction rate is sensitive to the molar ratio
of HCl to acetone , and of course to time and temperature . Freezing the mixture tends to virtually stop the reaction , but not totally .
This discussion of DPPP which began here at this forum has followed a parallel at times over at E&W with similar thoughts and experiements , and
many of the same people having membership at both boards . So I ask your understanding to simply paste any pertinent posts here and there when it
fits into the point of discussion , avoiding having to retype and reword saying the exact same thing in lengthy posts at the separate forums .
The information as follows fits this parallel discussion and elaborates on the chloroacetone / pentachlorophorone "connection" .
Nobody that I know of is talking about the formation of chloroacetone from
reaction between acetone and HCl . What is being described by the GB620498 patent is that in a reaction system containing acetone along with
hydrogen peroxide and HCl , that increased concentrations of HCl combined with increased temperatures favors increased chlorination of the acetone to
form chloroacetone as an undesired byproduct ,
instead of the intended trimeric acetone peroxide . This is good information about the reaction condition where hydrogen peroxide reacts with HCl to
produce chlorine , which is different from the condition where peroxidation would be the desired purpose for the hydrogen peroxide . The intended
reaction for the phorone dihydrochloride is to be a chlorination reaction resulting in conversion of the phorone dihydrochloride to pentachlorophorone
. The chlorine is being supplied by a side reaction from H2O2 and HCl , the HCl being present in some excess in the red phorone dihydrochloride
solution , because more HCl than required by theory was used to form the precursor
originally , and/or some extra HCl was added to the red precursor solution just before the addition to it of the H2O2 is begun . The production of
chlorine is favored by warm temperatures and excess HCl , according to the GB620498 patent . And from what I have read elsewhere about the reaction
of H2O2 with HCl , the reaction takes place slowly ,
therefore it is reasonable that a very slow addition rate of the H2O2 to the warm and HCl rich reaction mixture would favor the chlorination reaction
preferentially to a
peroxidation reaction which would be favored by opposite conditions , such as cold temperatures and lower concentration of HCl .
Early in the discussion of the chemistry of the reactions stated by Mackowiak for the
formation of DPPP , I stated that I had reason to wonder if perhaps the formation of the pentachlorophorone would be favored by warm temperatures ,
followed by cooling of the pentachlorophorone solution for completing its conversion to DPPP . That was a "guess" about the reaction which
is supported by the additional information which is provided by GB620498 . So it would seem likely that since 6 of 11 of the moles of H2O2 to be
added to the phorone dihydrochloride are consumed in the chlorination reaction producing pentachlorophorone , that 6/11 of the portion of total
peroxide should
be added to the reaction under conditions which favor that intended chlorination reaction . To reiterate , the conditions favoring chlorination are
excess HCl , warm temperatures , and slow addition of the H2O2 . Of course it may not be possible to exploit such a strategy for the chlorination
unless the pentachlorophorone is a stable intermediate
which may form in increasing concentration without peroxidative decomposition in advance of the point where the mixture will be cooled for conditions
favoring peroxidation of the pentachlorophorone to DPPP . Ideally , if the pentachlorophorone is a stable intermediate which cooperates in
accumulating to a high concentration without any further tendency towards decomposition , then the formation of the pentachlorophorone intermediate
could be accomplished by performing the reaction *warm*
during the time of addition of the first 6/11 of the peroxide required for the eventual formation of all the DPPP . When all of the
pentachlorophorone intermediate has formed , the mixture would be chilled very cold before the remaining 5/11 of the peroxide is added . So the
addition of the peroxide would be done in two stages , with the first portion being added to a warm reaction mixture favoring chlorination , and then
the second portion of peroxide added to a cooled reaction mixture favoring peroxidation of the chlorinated intermediate having accumulated during the
warm first reaction stage .
The volume of H2O2 stated by Mackowiak at 2 volumes of 30% H2O2 for each 1 volume of acetone is deficient the amount of theoretical requirement for
the reactions as Mackowiak has the reactions written . A minimum of 2.55 volumes of 30% H2O2 for each 1 volume of acetone would be required for the
stoichiometry to be satisfied where 6 moles of acetone are eventually converted to 1 mole of DPPP .
Closer to 3 volumes of 27% H2O2 for each 1 volume of acetone would be required by theory . Anyway , I find such an error in stoichiometry found in a
patent
to not be reassuring since the technical disclosure of chemical reactions is a highly proper place for exactness about such quantities .
[Edited on 23-1-2005 by Rosco Bodine]
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Pyroz
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RANGE TEST COMPLETE w/ video
Here is the range test for an 80 gram shaped DPPP charge. The test target was 4mm thick stainless steel pot...enjoy.
update for anyone who wants to recreate this experiment...here is how to do it.
1)get a small metal butane refill cylinder. The bottom of the cylinder is shaped for a perfect punching charge as it is concave
2) fill the cylinder with 80grams of highly compressed "DPPP" material and insert a detonating cap 1/4 of the way into the
filler---I used a 1.6gram cap which was a crimped .223 remingtion shell casing with a 1 meter long cXa thermalite fuse attached to it. I had 30seconds
to retire behind a steel reenforced backstop---
[Edited on 24-1-2005 by Pyroz]
Attachment: 80gramDPPP.mov (938kB)
This file has been downloaded 2483 times
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Joeychemist
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See hideki, you have told too many lies to even remember what you posted a few days ago.
I was referring to one of the videos you posted at RS, (The 20mg spoon video, not the new 80g video, the one before) the same spoon video that pyroz
posted page 26 of this thread, but he clearly said it was 30mg. the title of the attachment you posted at RS clearly reads 20mg DPPP but is the same
video. I find it very suspicious that pyroz would post the same video saying it was 30mg and you say its 20mg.So again I ask you again, what was it?
20 or 30mg? It is obvious that “one” of you or “both” are exaggerating.
Edit by Chemoleo:
Good idea, let's not waste more bandwidth on pointless arguments, which includes yourself too. I deleted the relevant posts above. Harsh measure,
yes, but this is where the buck stops
Guess we have to live with some exaggerations/errors, as the constant criticising does produce nothing but more bickering. Blatantly false posts will
be just corrected.
And, 20 vs 30 mg is already an improvement to 1-3 mg vs 100 mg.
Apart from that, you are always welcome to correct the errors/exaggerations with hard data, that is, your own experiments
[Edited on 24-1-2005 by chemoleo]
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Matsumoto_Hideki
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Lets get down to the recent video and thoughts?
Thank you chemelo..
I appreciate your kindness very much. I really wanted someone to analyize the video that Pyroz posted. I see something major here as it seems that
there was a signifigant enought energy to atomize the aluminum can and ignite it hence the white flash before the pot starts to get airborn. This is
what it looks like to me?
 ?? any thoughts
Oh and bTW just on that "remembering and supposed lying thing" thing chemeleo, I have short term memeory loss due to a car accient I was
in while I was finish school at Tohoku Daigaku near Sendai. So I can't help much.
Understand plz. My memory short term is bad = Brain damaged. yes it may be funny to you guys, brain damaged Japanese person.
[Edited on 24-1-2005 by Matsumoto_Hideki]
[Edited on 24-1-2005 by Matsumoto_Hideki]
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chemoleo
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Sigh. Matsumo you aren't off the hook.
I don't think you can conclude much from the video, except that it is an explosive with a reasonable VoD.
Atomised Al ... you meant stainless steel I thought.
Regardless- this video is interesting, but not really of great significance as it doesn't show the comparative power to
another HE, or even that of AP.
And this is what we should be after. So please let's focus on that.
[Edited on 24-1-2005 by chemoleo]
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Matsumoto_Hideki
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Butane cylinder is Aluminum not steel
Chemeleo I think pretty sure pyroz did say the can was Al not steel.
The pot was 4mm steel that I do Know.
Any comment on the shockwave and other things in the video. VOD I cannot measure nor can pyroz.
[Edited on 24-1-2005 by Matsumoto_Hideki]
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Rosco Bodine
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A more revealing test would be what a film canister size charge does to 1/2" thick plate . No shaped charge is needed .
Something comparable to PETN will hole the plate with no problem .
See page 2 of US5140908 for some plate test data for 35 ml volume charges fired against 12 mm thicknes steel plate . Sensitized nitromethane which is
only something like 10% stronger than ordinary TNT blows a hole more than six inches across through 12 mm plate .
[Edited on 24-1-2005 by Rosco Bodine]
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Pyroz
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I am planning on doing a film canister filled with some compressed "DPPP" sometime next week when i get around to it. It is very difficult
for me to say that this material is in fact as powerful as the patent claims to be...but hey, who knows ?
I saw a pretty decent sized explosion yesterday but that doesn't mean much...and this video was more for general info and such. One thing i left
out was the dime sized indentation left behind on the 3cm thick steel rebar which was also bent from the force of the blast..which looked like a
oxyacetlyene torch was been used to slice into it ---if i'm not mistaken this is a product of high velocity jetting? I think one of the reasons
why the shape charge didn't do more damage to the plate below was the fact that most of the gasses had time to escape out the sides thus lowering
the downward velocity of the jet. As well the steel pot (top to bottom was 15cm) --- so that may be another reason.
a note to everyone:
The previous video on pg 26 was 30mg of "DPPP" powder melting and detonating...not 20mg as hideki keeps posting.
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Rosco Bodine
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There have been a few experiments done by me over the years with different organic peroxides , and while some of the compositons are "in the
neighborhood" of TNT , *none* of the compositions are anywhere near the nitrated polyols in power . The strange thing is that the peroxides make
a helluva bang like they are really high output just going by the noise , but when you look at the actual work done on the target you just don't
find
the sort of damage that the noise would have you expect to find . It is sort of the same story for lead styphnate and lead azide if you detonate say
50 mg of the loose crystals of each on a thin sheet of aluminum . The lead styphnate will make a helluva loud noise and barely scratch the metal .
The lead azide will make more of a short quick snap like the sound a plastic ruler makes if bowed up slightly and allowed to fly downward against the
surface of a desk , a sharp snap more than a loud echoing bang , and yet the difference in the work done to the target is astonishing because a clean
edged hole is found to be cut right through , complete with the "missing metal" effect and not a lot of banana peeling on the underside
either , the metal which was in the opening is just gone , atomized . So never be deceived by the noise signature of a particular composition as it
has nothing to do with the power or brisance of what made the noise .
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Pyroz
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| Quote: | Originally posted by Rosco Bodine
...yet the difference in the work done to the target is astonishing because a clean edged hole is found to be cut right through , complete with the
"missing metal" effect and not a lot of banana peeling on the underside either , the metal which was in the opening is just gone , atomized
. |
Well, that makes perfect sense. The charge itself was shaped --the bottom of the cylinder was concave so wouldn't that cause a "punch"
and "peel" type of blast regardless of VoD? i don't know because I've never tested PETN or RDX before..my loss, oh well. I've
included a close up image of the top and the bottom of the pot itself...the video quality stills aren't great but the picture quality from my
digital camera is much better... so have a look
update:
I think I will try making a conventional shaped charge with a standoff w/ copper insert. This should blow a hole in 1" thick plate steel --- and
make a clean hole if the velocity is anywhere near 9000m/sec.
[Edited on 25-1-2005 by Pyroz]
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WaveFront
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Want data? Repeat the same experiment with AP
Want fun? Mix with KClO3. In small amounts it is close to HMTD.
EDIT: and I am not talking about noise, but shattering power
[Edited on 25-1-2005 by WaveFront]
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Matsumoto_Hideki
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.. I don't understand
| Quote: | Originally posted by WaveFront
Want data? Repeat the same experiment with AP
Want fun? Mix with KClO3. In small amounts it is close to HMTD.
EDIT: and I am not talking about noise, but shattering power
[Edited on 25-1-2005 by WaveFront] |
Sorry mix what with what to get shattering power?
AP with KClO3?
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WaveFront
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My "DPPP" was pretty bad making holes in thin metal plates; in a similar way to AP, it tends more to bow the plate. (I use only small
amounts).
On the other hand, HMTD is very good in this task. (As seen in my video posted before)
When I mixed my "DPPP" (or whatever the impure thing that in fact it is) with finely powdered KClO3, there was little if any increment of
BOOM, but the plates are perforated. It is not a clean cut, but you will appreciate clearly the difference.
I use the product by heating it in aluminum foil. The Aluminum metallisations are better too.
AP and Chlorate? May be I do tests with both mixes to compare
The HMTD also makes good mixes with chlorate, but what I remember is an increase of the power (bigger hole and more noise)
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Rosco Bodine
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DPPP chemistry related , 90+% yield conditions
After doing several experiments under varying conditions , I have found a set of conditions which has produced very good yields which are in close
agreement with the DPPP patent . The conditions for achieving the highest yields so far obtained are as follows .
100 ml acetone was placed into a bottle and then 95 ml of HCl 31.45% was added and the bottle sealed . After standing for 30 minutes the bottle was
warmed in a water bath at 65 C until the solution had an orange color . The bottle was removed from the heating , and allowed to stand at room
temperature for 72 hours and then placed into a freezer to cool overnight at -10 C . 280 ml of 27% H2O2 in a plastic bottle was placed in the freezer
also overnight . A 1000 ml tall form beaker was placed in a 3000 ml plastic bowl and set upon a stirplate . Into the beaker was placed a 40 mm
diameter cross form stirbar and a thermometer leaned diagonally with the tip against the bottom wall of the beaker .
An addition funnel was set in a support above the beaker . 1500 ml of ice cubes was distributed around the outside of the beaker and about 75 grams
of sidewalk deicing salt ( calcium chloride / sodium chloride ) was sprinkled over the ice cubes . The cold precursor was poured into the beaker ,
and the addition funnel was filled with the cold H2O2 . The stirrer was started slowly and the temperature reading was -10 C . 40 ml of HCl 31.45%
was poured into the stirred precursor and the temperature rose to -2 C . The addition of peroxide was begun immediately at about a drop per second
and then gradually increased allowing a fairly rapid rise of temperature to 15 C , and regulating the rate of addition to maintain 15 C , which
appeared to be a very smooth reaction temperature allowing a fairly rapid run in of the H2O2 , in a small stream as the addition proceeded .
Temperature actually began falling on its own towards the end of the addition even with the valve nearly full open . The mixture had the appearance
of eggnog , a smooth emulsion like appearance with no crystals visible , and the mixture gradually thickened , requiring higher and higher stirring
rates to maintain the mixture in circulation . There was only a trace of any insoluble byproduct globules , a very tiny droplet maybe a tenth gram in
mass . The mixture gradually cooled down to about 0 C after an hour past the end of addition . Stirring was stopped for intervals of 1 hour and then
the mixture stirred up again . This was repeated twice and then the mixture allowed to stand overnight in the salted ice . The next morning the
mixture was at - 4 C and had set up into a semisolid floating mass of nearly white crystals occupying three fourths of the volume of the mixture with
clear liquid underneath .
200 ml of distilled H2O was added and the mixture stirred up to a pouring consistency so it could be filtered . The
mixture was poured into a filter and the residue rinsed from the beaker into the filter . The filter was removed and set onto a blotter to remove
residual liquid ,
and then the filtered mass was rinsed from the filter into a clean beaker with 300 ml distilled H2O . A stirbar was added and the mixture stirred up
with the distilled H2O . 10 ml strong ammonia water was diluted to 200 ml with distilled H2O and poured into the stirred mixture for neutralization
of residual acidity . After 10 minutes stirring the mixture is filtered and dried . The material dried to a free flowing powder weighs 98 grams . A
few percent of residual moisture remains but not much . 88.6 grams would be 90% of theory and 98.5 grams would be 100% of theory . So this yield
which I have gotten is nicely in agreement with the patents reported 90% yield .
This result also presents an opportunity for testing the residual reaction liquid for unreacted H2O2 . If the substance produced has a structure
agreeing with the patents designation as DPPP , then there should not be much H2O2 left unreacted in the mixture . What I propose to do is to repeat
the synthesis under the same conditions as what are supposed to be producing a nearly quantitative yield of "DPPP" , and when the reaction
is complete , to then add an equal amount of acetone as was used to form the precursor to the "spent" reaction mixture and allow it to react
further in the cold and produce any more precipitate that it would produce from any residual H2O2 ( which shouldn't be present ) if the reaction
mixture *did* form DPPP originally . After adding more acetone , if there is a substantial precipitate of AP produced , increasing the weight of
product substantially beyond what is the 98.5 gram theoretical yield for DPPP which had been "supposed" to be what was the first product ,
then it will be a certainty that the first product was actually not DPPP , but likely some AP isomer or variant instead . This will have been
established by the "proof by synthesis" method which will have stoichiometry revealed not consistent with the first product having been DPPP
. This weekend
I hope to get around to doing this experiment for "chemical sleuthing" the nature of the spent reaction mixture , to see if it is or is not
what it is "supposed" to be , making the case for or against DPPP ........ quietly , by one entirely shockwave free method All this is in keeping with the axiom there is more than one way to skin a cat .
[Edited on 25-1-2005 by Rosco Bodine]
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fatkangaroo
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I just attempted the DPPP.
150ml of 30% hydrochloric acid was added to 140ml 100% acetone. I put a lid on the jar and put the jar in a hot water bath in a electric frypan on 80
.C for 3 hours. I saw the same colour changes that have been reported in the thread from clear to light yellow to dark yellow to brown to amber. I
stoped heating and put into frezzer overnight. By morning there was a couple of drops of black oil floating on the top and and gram of green- yellow
crystals on the jar lid. Added the 50% peroxide in a ice bath. The second the peroxide hit the solution crystals formed straight away and there was a
temperature rise. 5 minutes later the jar was just about full so I filtered and washed the crystals. They came out white and looked and smelled just
like AP. I have put the filtered solution back into freezer in the hope maybe now the DPPP might form.
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Pyroz
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| Quote: | Originally posted by fatkangaroo
By morning there was a couple of drops of black oil floating on the top and and gram of green- yellow crystals on the jar lid. Added the 50% peroxide
in a ice bath. The second the peroxide hit the solution crystals formed straight away and there was a temperature rise. 5 minutes later the jar was
just about full so I filtered and washed the crystals. They came out white and looked and smelled just like AP. I have put the filtered solution back
into freezer in the hope maybe now the DPPP might form. |
Well, the indication of yellow green crystals means that phorone-isomer has formed... so at least his part of the reaction sounds correct. The
addition of HCl after the phorone solution has been chilled to -5C or less as a catalyist must be done before the slow (drop by drop) addition of
conc. hydrogen peroxide. I have found that when the temperature gets above 10 degrees C for the peroxidation process of phorone isomer seems to
produce a very similar material to AP, but further investigation reveals that the crystal structure is vastly different. The best explosive properties
are obtained when the material stays in a temperature below 0 degrees C throughout the reaction process. You should be left with a very pale sulphur
yellow/green crystalline material that should smell slightly camphorus after purification in pure water/carbonate and isoproply alcohol.
[Edited on 26-1-2005 by Pyroz]
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Rosco Bodine
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The reaction temperature has a definite optimum range where good yields are produced , and excursions even briefly outside the range , particularly in
the upward direction will cause the yield to be reduced substantially . The 15 C which I have found is limiting is in contrast with the limiting
temperature of 30 C described by a patent GB620498
for trimeric acetone peroxide . I find this difference in limiting temperature to be interesting .
The temperature for the DPPP reaction does give best results in the cool to cold range . But the greatest yield which I have gotten with very good
cooling and careful control of the rate of addition is with the temperature not above 15 C . Also for the temperatures in the cool to cold range
there is not produced the irritant byproduct , and the odor is very mild and the color very nearly white especially after the mixture stands in an ice
bath for six hours or more after all the peroxide is added . The high yield batch which I described a couple of posts above actually had a pleasant
odor and no irritant properties . The smell reminded me very much of the smell of ripe bananas on the wet material and faded as the material dried .
The smell of the dry material is very faint and to me smells almost exactly like pyrethrin based aerosol mosquito spray . The true color of the
material is colorless , as proven by sublimation , where all colored samples leave a tiny amount of yellowish residue after the sample is sublimed
away , and all the crystals which condense from the vapors are colorless .
P.S. The limiting temperature is possibly related to the amount of excess of HCl which is present . It is my guess that the more the excess of HCl ,
the colder will be the limiting temperature .
[Edited on 26-1-2005 by Rosco Bodine]
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Pyroz
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I am curious if just about any acid could be used to create Phorone -isomer. How about replacing Hydrochloric Acid with concentrated Nitric Acid w/
concentrated Sulphuric Acid? I wonder if it might help create a more energetic substance?
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Rosco Bodine
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If the chlorine containing intermediates are essential , and it looks as if they would be for the DPPP , then other acids would not work , except for
other halogen acids like perhaps HBr or others .
This would actually be a good experiment to see if using sulfuric made no difference and you still got what seems to be DPPP ,
which would pretty well prove that what you suppose is DPPP is actually something else , maybe not AP , but for sure not DPPP either .
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PainKilla
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The purpose of this experiment is to possibly eliminate the phorone part (i dont beleive its possible this way) from "Dppp" ( non existant).
If any acid can be used then it is completely relevent towards H+ instead of Cl-. If this is the case, then most likely phorone is not part of the
process since h2so4 with acetone makes*mostly* mesitylene. However, if I get small yields of DPPP, then it is probably a phorone derative. We will
see....
O yea, it is quite possible that this is merely tetrameric AP. I mean, there is no other way to form it except via CHLORIDE salts. Therefore, if my
experiment doesn't bear fruit to a product, then this is either a phorone derative OR tetrameric AP, which has only been SOMEWHAT succefully
formed using chloride salt catylsyts (sncl2, sncl4 etc). Even using these methods, note that yields are 40% so therefore it is part tri/dimers
too.....
In other words, theres an excellent chance this is not DPPP bit simply TeAP. I think this is much more plausible. It's obviosuly stable enough to
exist, which is more than we can say for DPPP.
[Edited on 26-1-2005 by PainKilla]
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Rosco Bodine
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One thing I can say pretty conclusively is that our suspected DPPP is *not* tetrameric AP as I have on hand thirty grams or so of tetrameric AP and it
is a quite different material in volatility , density , minimum quantity for DDT , ect .
And the synthesis of tetrameric AP is very straightforward . It is a room temperature synthesis too , no cold temperatures required .
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PainKilla
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The only REAL TeAP i have seen is with the use of SnCl4 for even decent yeilds. I ahev not seen any other ways. I almost positive that what you have
is not TeAP. TeAp is supposed to subliminate almost not at all.
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Rosco Bodine
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What I have is definitely tetrameric AP and this was confirmed several ways ,
volatility way lower than AP , different explosive properties , and different crystal density and appearance . The yield was 44% using 75 ml of
acetone with 125 ml of 27% H2O2 which was mixed at room temperature , and while rapidly stirred
was treated very slowly by an injection below the surface of 6 ml of H2O solution containing 2.5 grams of SnCl2 , which made a "frying
sound" upon contact with the mixture from the vigorous reaction . The yield was 42 grams of sparkling crystals . In a loosely covered container
the weight loss after one year was 25% ,
which is less than half the loss for a like control sample of AP stored beside it in an identical container .
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PainKilla
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Ah I see you used the SnCl2 way, but you msut take into account that not only TeAP was formed. I think its like a 35% yield using SnCl2. We will see
soon though :p.
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