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Author: Subject: Diphoronepentaperoxide (DPPP)
Matsumoto_Hideki
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[*] posted on 8-1-2005 at 18:45
Ammonium Hydroxide decomposes DPPP?


Rosco and others can you explain why Ammonia decomposes DPPP? I did for all my other sucessful batches use NaOH to nutralize the DPPP. It worked very well. I have noticed that Ammonia attacks DPPP, I just don't know why and what forms as a result of this. Does it start to form an amine of Phorone ?

BTW I am not going to be able to do a video of my detcord and BIG shaped charge since the weather in my parts is very DANGEROUS, too much ice and snow on the roads. I FUCKING HATE FUCKING SNOW! I AM PISSED OFF:mad:

maybe next week????
[Edited on 9-1-2005 by Matsumoto_Hideki]

[Edited on 9-1-2005 by Matsumoto_Hideki]
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Rosco Bodine
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[*] posted on 8-1-2005 at 19:16


It is the elevated pH caused by free ammonia which destroys the DPPP . And it is so easy to overshoot neutralization using any hydroxide , that it is best to calculate the neutralization equivalent and then add somewhat less of a very diluted hydroxide than needed and then complete the neutralization with a separate addition of much milder base like sodium bicarbonate in slightly greater amount than needed to effect the neutralization . Adding too concentrated of a hydroxide creates a local caustic concentration which destroys the organic peroxide it contacts . Good stirring and using a diluted hydroxide added quickly limits the decomposition . Most peroxides tend to be decomposed by alkali and stabilized by acid , except for HMTD which is an exception . Phosphoric acid is actually added to hydrogen peroxide solutions to stabilize the solutions against decomposition in storage , while any alkalinity accelerates the decomposition .
Organic peroxides behave the same way , generally speaking , being stabilized by slight acidity and destabilized by alkalinity . Evidently DPPP follows the general rule . But in a way this is good because in compositions containing Ammonium Nitrate for example the natural acidity will probably enhance the stability of the DPPP , MEKP , AP which may be part of such compositions , while the same acidity would be detrimental for the stability of HMTD .
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smile.gif posted on 8-1-2005 at 20:16
Breakthrough???


Rosco, you might want to try re-crystalizing this stuff. I just recystalized 1g by dissolving in acetone and was left with half the volume of crystals but they still weighed almost .9g still. Also the smell is not as bad as before, it's more sweet now and not as iritating, the crystals ar whiter but still with the slight yellow tan color. All I can say is you must try this for yourself.:D:o:D
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Rosco Bodine
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[*] posted on 8-1-2005 at 20:48


What method exactly did you use to
perform the recrystallization ? Did
you precipitate using water dropwise ,
or let the acetone evaporate , or saturate
hot acetone with DPPP and cool ? Please everybody , be precise .
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[*] posted on 8-1-2005 at 21:01


Sorry I was exited and kind of busy playing with the stuff.:D

I dissolved the DPPP crystals with a few ml of Acetone at room temp then allowed the acetone to evaporate until most was gone and I was left with a thick “slurry” I poured onto a paper towel, the remaining acetone very quickly evaporated as I gently “kneaded” and powdered the crystals to avoid large crystals from forming. The remaining crystals burned pretty nice with a Whoomp!
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Rosco Bodine
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[*] posted on 8-1-2005 at 21:10


Yeah letting the solvent evaporate or
slowly cooling hot solutions will both
grow the crystals bigger , so will watering out the crystals very slowly from acetone ,
or using alcohol if the substance is alcohol insoluble . Dittos for toluene or naphtha .
There are a half dozen ways this could be tried . Conversely , dumping a hot saturated acetone solution of DPPP into
cold water would give you a dust like product . The most dense granular composition may be an aggregate of the
the coarse and the fine , just enough to fill the spaces between the larger crystals .
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Matsumoto_Hideki
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[*] posted on 8-1-2005 at 22:48
Wow thanx rosco!


Ya, that is what I was thinking about free NH3 destroying the DPPP yet when I added my Ammonium nitrate nothing happend. hmm this is looking better and better. NExt question is what does DPPP decompose into when it has reacted with ammonia???
I am tring a crystal seeding method with cool forming Pentachlorophorone to see if there is any difference in quality of the crystals.. keep you posted..

[Edited on 9-1-2005 by Matsumoto_Hideki]
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Pyroz
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[*] posted on 8-1-2005 at 23:49


Quote:
Originally posted by Joeychemist
Sorry I was exited and kind of busy playing with the stuff.:D

I dissolved the DPPP crystals with a few ml of Acetone at room temp then allowed the acetone to evaporate until most was gone and I was left with a thick “slurry” I poured onto a paper towel, the remaining acetone very quickly evaporated as I gently “kneaded” and powdered the crystals to avoid large crystals from forming. The remaining crystals burned pretty nice with a Whoomp!

Thats excellent news...and may I add thats a smart idea. I used 100% pure Isoproplyene and found that it dissolves the DPPP rather easily as well but it does not vapour as quickly as Acetone. Good work Joey
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[*] posted on 9-1-2005 at 08:29


I came up with some strange results. I had to keep my acetone-HCl mix on hold for a few days, and now it has turned from red, almost black back to bright yellow.

I tried to peroxidise 2 ml of it, I performed the experiment in such a small scale because my freezer was filled with food (!) and the weather warm so I had to use a small ice-salt bath.

1ml H2O2 19,5% was added to 2ml of the mixture after cooling it down to -10 C. Temperature only rised to -5. After a few minutes temperature was down at -10 again, and the rest of the peroxide, 3ml, was added.

No crystalls formed whatsoever. No gasbubbles either.
I'm going to keep it in the icebath, so it will stay at a temperature of about 0 C for a time. Perhaps stupid HCl completely left the solution, but I find this unlikely. I will try again with some HCl added later.

The big question: What happened to my solution? Why is it bright yellow again? (Tarry shit is on the jar walls)

I used 20ml of pure acetone, and 26ml of 30% muriatic acid (aq HCl). It was heated in a closed container to 60-70 for an hour (It did not leak) and later heated to 35-35 C for two more hours. Then the jar lid was opened and the solution was heated to 35-45 C for another six hours.

By the end of that heating (to evaporate exc. acetone) the solution divided into brown-red tar goo on the walls and on top of the solution and the liquid itself, now bright yellow. What is this?

The lid was corroded, and it was made of plastic covered iron. Perhaps the solution was iron-contaminated but one would think that'd make H2O2 fizzle when added.




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Matsumoto_Hideki
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thumbdown.gif posted on 9-1-2005 at 09:51
I know what happend!


Jome, this yellow you speak of has occured in my peroxidations before and may related to a couple of things
I think you are looking at what happens when you over heat your Phorone HCl and or what happend when impurities react with leftover HCl and cause secondary reactions with metal ions Fe+causing your Phorone HCl to decompose?
More detail is needed. Never use ANY metal near H2O2 or HCl as you can really get some nasty reactions, especially when they are mixed.
My experience leads me to beleive that your iron lid caused your problem. USE nitrile or rubber to seal your reaction next time.
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[*] posted on 9-1-2005 at 10:24
Summary of Experimental Findings related to Chemistry of DPPP


Phorone Dihydrochloride Precursor :

The sealed bottle reaction has definite advantages . If a bottle or jar
has a metal lid it will not withstand the corrosive effects of direct contact
with vapors of acetone and HCl , and its gasket liner will likely detach
and contaminate the reaction . This can be overcome by laying flat across
the opening of the glass jar , one of the heavier thickness ziplock freezer bags
and then pressing the metal cap downward to engage the threads and tightening
securely . The polyethylene sheets of the bag will act as a gasket and prevent
the inner surface of the metal lid from being attacked by the vapors .
A completely polyethylene or polypropylene cap with compatable liner
or friction seal , or most desirable a teflon seal is actually the best option .
The precursor can be prepared in any shape of bottle , even a wine bottle
and transferred to another vessel of more convenient shape and volume
for performing the peroxidation .

From several slightly different experiments it has been found
the preparation of the acetone and HCl reaction mixture is the
secret for producing good yields of DPPP . The molar ratio of
HCl to acetone must be 2 to 3 , with the HCl limited to only a
very small excess of theory on the order of 2 to 3 % . The volumes
of acetone and HCl must be measured very precisely for the reaction
to produce the precursor in a concentrated and pure form . The
* exact volumes * for HCl 31.45% and acetone to accomplish a
correct mixture are 104 ml of HCl and 112 ml acetone . For convenience
in measuring using a 100 ml graduated cylinder , for exactly 100 ml acetone ,
use exactly 93 ml HCl 31.45% to achieve the correct ratio . Small
departures from these amounts will produce disproportionately
larger changes in the quality of the precursor produced by the reaction
which appears to be sensitive to pH . If you are using a different
concentration of HCl , then you need to calculate the amount of
your HCl to achieve the same molar ratio as above . The mixture
should be done in a glass jar or bottle and sealed immediately to
prevent the loss of acetone and thereby preserve the reaction mixture
proportions unchanged during the time of reaction , which involves
gentle heating of the mixture . The first heating which occurs is the
exotherm of the self-reaction , immediately upon mixing the acetone
and HCl . This self-reaction is allowed to continue for 1 and 1/2 hours
and then supplemental heating for 2 to 2 and 1/2 additional hours is
performed by placing the still sealed bottle into a 75 C water bath ,
to complete the reaction which forms an intensely red tinted but transparent
solution of phorone dihydrochloride . The beam of a flashlight shined
through the deep red solution gives the appearance of "ruby glass"
and if the solution is swirled so that a thin film of liquid sheets across
the inside walls of the bottle , the thin film appears bright yellow .
This color development is the marker for the endpoint of the reaction
producing the phorone dihydrochloride precursor . The supplemental
heating should be ended at this point and the sealed bottle removed
from the water bath and allowed to cool . A very slight oil slick may be
seen on the surface of the intensely red liquid if light is reflected from its
surface , and it will have the shimmering rainbow irridescent appearance
which is similar to the effect seen when a drop of oil strikes the surface
of still water in sunlight . The trace of oily material is insoluble higher
polymerization and precursor decomposition product which would increase
in amount with continued heating of the acetone HCl mixture , and the
oily surface precipitate therefore represents a loss of the desired precursor .

Higher acid to acetone ratios and higher reaction temperatures
and longer reaction times increase the amount of the oily precipitate ,
so these factors are to be avoided . The cooled reaction mixture
may be kept in good condition by refrigerating it until the peroxidation step
is performed later . The mixture in the sealed bottle does continue to react
after being removed from the heat , only at a much reduced rate , and the
further reaction nearly ceases under refrigeration . If the reaction has been
allowed to proceed beyond the desired point and becomes very dark from
precipitated material or has a distinct upper layer of oily material forming on
its surface , then it should be filtered through a double thickness of coffee filter
which has been pre-wetted with plain water before filtering . The filter will
trap most of any the oily precipitate and the solution can then be used for the
peroxidation without precipitation of the insoluble impurites which would
otherwise occur if they are not removed by filtration .

Peroxidation of Precursor to DPPP :

Generally this has been done by first adding 2 or 3 ml
of fresh HCl to the cold precursor solution before proceeding with the peroxidation .
The greatest exotherm during peroxidation will occur during the addition of
the first 10 to 15% of the total peroxide to be added . The initial exotherm is quite
energetic and must be done dropwise , very slowly with swirling or stirring ,
drop by drop additions are imperative here . This initial peroxidation converts
the phorone dihydrochloride to pentachlorophorone , and the reaction is ten times
as exothermic as is the remainder of the peroxidation . So it cannot be too
much emphasized to go * slowly * with the first additions of peroxide in order to
control the thermal spike which everyone observes to occur at this point in the
reaction . If peroxide is carelessly dumped into the mixture at this point , a
full blown steam explosion has been reported to eject the contents of the mixture
from the reaction vessel . A salted ice bath is a good idea here , and keeping the
reaction below 10 C thoughout the addition of peroxide is good practice . The reaction
mixture is allowed to stand in the cold for at least 30 minutes to complete the precipitation . One hour would perhaps be better .

I have tried an alternate method which has also worked , using a magnetic stirrer
but I have not compared the yields of the alternate method to the cold method
just described . The alternate method is to perform the initial peroxidation having
the reaction vessel in an unfilled cooling bath containing a shallow layer of plain water , and allowing the precursor mixture to warm at a fair rate during dropwise addition of the first 10 to 15 % of the peroxide , controlling the rate of addition so that the reaction mixture attains a peak temperature of 65 C at the end of the addition of the 10 to 15 % of the total peroxide . The addition is stopped and the bath is filled with ice so that the stirred mixture is cooled below 10 C before the addition of peroxide is resumed . The rate of peroxide adddition is increased cautiously so as to maintain the reaction temperature below 15 C to the end of the addition , and stirring continued for thirty minutes beyond the last addition . Stirring is then stopped and the mixture allowed to stand for a few minutes , and the mixture is dumped into the now melted cooling bath and neutralized . Slightly less than the calculated amount of ammonium hydroxide required for neutralizing is dumped into the well stirred mixture , since it has been observed that excess alkalinity of free ammonia decomposes the DPPP . Local caustic concentrations decompose the DPPP , so the neutralization mixtures should be dilute and mixed quickly , and perhaps it is best to then complete the neutralization using a small excess of theory of a milder alkali like sodium bicarbonate .

That pretty well summarizes where things are at this point in the experiments
so far regarding the synthesis of DPPP . The material evolves extremely irritating
vapors which should be avoided , as they are quite similar to the irritant effects
of "tear gas" . The effect is noticeable to put it mildly , even at low concentrations
where the smell is not noticeable . There has been consistent observation and agreement by everyone reporting that good ventilation and / or other protection
is a must . DPPP is one of those materials which will render an area vacant quicker than a fart filled elevator , you have to experience it to believe it :D

[Edited on 10-1-2005 by Rosco Bodine]
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[*] posted on 9-1-2005 at 11:27
THings still to be done?


Good work everyone!

Having been away for a few days, this thread has grown yet by another couple of pages !

Anyway, regarding odour, and the purity of the putative DPPP - am I correct in reading that noone actually tried to dissolve it in isopropanol or acetone (i.e. a saturated solution of DPPP) and then to precipitate it with an excess of water?
I strongly suspect that this may partially remove the bad smell, and as rosco said, produce a more powdery precipitate.

Also, has someone determined the solubilities at this point? I.e. in ethanol, ethylacetate, methanol, IP, acetone, and less polar ones such as toluene, trichloroethylene, chloroform etc??

Then, did anyone do some friction tests? I really would like to know how it behaves when it is scraped with a spoon against stone or something. That way I always managed to ignite small amounts of chlorate/sugar (had to press very hard), which is otherwise fairly friction insensitive.

Rosco, you give a very detailed summary of the procedure - but I wonder where you got your thoughts on the importance of stoichiometry from (i.e. to quote your 2-3% excess). Did you do detailed yield studies, i.e. measure the yield at various stoichiometries (acetone vs HCl), to find the optimum yield?

That brings this to another point: yield.
What is the yield, from the quantities you describe? How many grams from 112 ml acetone?

Then, you all seem to be making very large batches. Did anyone try making small amounts, producing only a couple of grams worth of DPPP? Did this work ok? Or was the yield considerably less?

Oh, and Axt, we need you for the old drop test! As far as I remember you have it nicely calibrated against PETN and various others :)

Stability: it might be wise to take, say, 5 grams, and leave it at RT in a safe place, for several weeks, to then weigh it again to determine whether and how much DPPP decomposes/sublimes.
This is of course a function of purity, so, the recrystallised stuff is desired.

[Edited on 9-1-2005 by chemoleo]




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[*] posted on 9-1-2005 at 11:48


I have been working with smaller batches. 26mL of HCl and 28 of acetone. It is still drying.

Rosco, you are quite excellent at those long writeups.:) However I have some conflicting evidence on the aroma of DPPP. I (kinda) LIKE IT, it does not bother me. The worst smells I noticed during this reaction is of the phorone dihydrochloride. Sure the DPPP has a smell, but it does not seem lachramatory as you have been making it out to be. I used bicarbonate for my neutralization which could be a factor in this. Perhaps ammonia somehow complexes with the DPPP? I used gloves and goggles during the peroxidation and filtering of the DPPP and the smell was noticeable but not terrible, and I was doing this in a closed basement room without the window open. The smell of DPPP is different from that of AP but they both have the same intensity( if that makes sense, neither was stronger than the other). Is there a danger of decomposition of DPPP when too much Na-bicarb is used to neutralize it?




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[*] posted on 9-1-2005 at 12:09


Regarding the smell I too noticed that irretating smell (that's why I got rid of the ppt). I too used ammonia to neutralize it. But my prepration faild as I ended up with AP.

So I think its correct to assume that ammonia doesen't react with the DPPP (my yeild didn't seem to contain any) but rather with the phorone dihydrogen chloride or other crap that may exist in the mixture.
Please someone correct me on this if I'm wrong.
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[*] posted on 9-1-2005 at 12:16


DPPP is soluable in acetone, Isoproplyene, methyl and ethyl alcohol. It is insoluable in water.

--becomes extremely dangerous around 150C when it begins to melt---it will explode without warning at 200C unconfined state
--is much less sensitive when fully dry in comparion to other organic peroxides and it take a significant amount of force from a 5lb sledge hammer to explode it. Unlike dry AP or HMTD which takes very little force.
--in explosion tests 2grams of compressed DPPP inside of a 2.5" X 1/2" copper tube blasting cap has more than double the explosive power than the same amount of AP.
--DPPP charge: Brass casing punctured the steel plate completely--sharpnel peirced the steel plate in several area, indication of extremely high velocity sharp fragments
--AP charge: Brass casing chunked and moderately indented the steel plate---no penitration. Slight scoring on the plate from sharpnel.

[Edited on 9-1-2005 by Pyroz]
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thumbup.gif posted on 9-1-2005 at 12:32
Na bi-carb seems the best


R chemist
I have not noticed any decomp while using sodium bi-card to bring the ph down and I am glad that you did wear goggles while filtering, the filtering does seem to be the worst part. I am shocked to find that you like this smell? I guess each to their own, I don’t like the smell.

Pyroz, what’s with the gigantic quote? The thread is large enough as is.
I have done some friction tests between two rocks and between a rock and a spoon and well, what can I say?, it’s a primary explosive, it is friction sensitive in the way that it seems to perform like the rest of the explosive peroxide family, similar to TCAP but a little more stable and requires a heavier blow to detonate compared to AP.

I think getting Axt to do a test is a simply marvelous idea
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[*] posted on 9-1-2005 at 13:00


Quote:
Originally posted by chemoleo
Rosco, you give a very detailed summary of the procedure - but I wonder where you got your thoughts on the importance of stoichiometry from (i.e. to quote your 2-3% excess). Did you do detailed yield studies, i.e. measure the yield at various stoichiometries (acetone vs HCl), to find the optimum yield?
Usually it doesn't take old Rosco long to get the lowdown on a reaction from empirical data , eyesight and intuition , and then apply the amount of theory that seems to fit the experimental observations . Yeah I know that's doing things the old fashioned way , but in the absence of pricey equipment to do the analytical work , I have to do what I can with the data I do have and then go out on a limb with a best guess interpretation . It's early I know to be making some bold conclusions about the chemistry , but it seemed that the priority at this point is really the physical chemistry of making the synthesis work and then the details and tweaks can be debated later .
Quote:

That brings this to another point: yield.
What is the yield, from the quantities you describe? How many grams from 112 ml acetone?
The yield is very good .
I haven't weighed my last batch because it isn't fully dried yet . It's been raining here and its taking its time drying . But this yield won't be definitive because some was lost during neutralization by
taking the pH too far past 7 , not knowing it would cause some loss of product . It will take some more work to get good numbers from a clean , error free procedure .
Quote:

Oh, and Axt, we need you for the old drop test! As far as I remember you have it nicely calibrated against PETN and various others :)
I second that . The professional services of one wacky Aussie are required at this point :D Also we need to get Philou Zrealone in here for another chemistry lesson ;)

rogue chemist :

Quote:
Originally posted by rogue chemist
I have some conflicting evidence on the aroma of DPPP. I (kinda) LIKE IT, it does not bother me. The worst smells I noticed during this reaction is of the phorone dihydrochloride. Sure the DPPP has a smell, but it does not seem lachramatory as you have been making it out to be. I used bicarbonate for my neutralization which could be a factor in this. Perhaps ammonia somehow complexes with the DPPP?
Actually my first idea was that
* Chloramine * is the likely culprit arising from a mixture of ammonium hydroxide , HCl , and unreacted H2O2 ......But Joeychemist reported that the irritant vapor was present even if no ammonia was used but only sodium bicarbonate ,
so that shot down my theory about chloramine . So now rogue chemist and Joeychemist are providing contradictory information . Guess that leaves the question unresolved , until somebody tries both ways . It would get sort of "foamy" using bicarb for the entire neutralization so I will likely go with NaOH for 97 % neutralization and finish the process with bicarb .


[Edited on 9-1-2005 by Rosco Bodine]
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[*] posted on 9-1-2005 at 13:51
damb!


Yes that does conflict!Arg!!!
I did do it both ways ammonia and sodium bi-carb, the smell remained in or on the crystals stronger and slightly different than the bi-carb even after washing with additional portions of water and the smell did remain. And as I did mention yesterday after I recrystalized the DPPP in acetone the smell was considerably less but still remained. But you know Rogue chemist also said that he’s doesn’t mind the smell.Hmm... maybe it just does not affect him like it does us. :o

Rosco,You reported the same as I have experienced when I comes to this odor, the eyes become agitated and the nose and mucus glands become slightly inflamed and agitated causing a runny nose.

Rogue, you experienced no effects like a runny nose or soar throat? You didn’t even shed one tear? I’m not sure what to say or what to do now? This thread is going to be 50 pages before we figure this one out.
:(:(:(:(:(

[Edited on 9-1-2005 by Joeychemist]
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Rosco Bodine
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[*] posted on 9-1-2005 at 14:04


Maybe rogue chemist has fondness for cajun food , three alarm chili , and slices onions with a smile :D You know the sort that eats hot peppers like they were celery sticks , peppers which would be lethal to the average person :D

[Edited on 9-1-2005 by Rosco Bodine]
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[*] posted on 9-1-2005 at 14:46


Joey, Nope, absolutely no effects.

And now for my most recent "holy shit" observation.:)
All of you may remember how I said that I kept my filtrate after filtering out the DPPP but before neutralizing. Well yesterday it was still yellow, with some DPPP crystalizing on the surface. Well, today I go back to it and the solution and the crystalls are completly white. :o I filtered it out and neutralized it. It was still completly white. So, I decide to take a whiff of the crystals after filtering and IT SMELLED NOTHING LIKE DPPP AT ALL IT SMELLED LIKE CHLOROBUTANOL. Of course I flame test the still wet crystals and I get the nice fwump(no diference from the usuall DPPP). I smelled my vial of chlorobutanol, then smelled my "DPPP" the DPPP was like a slightly milder version of the chlorobutanol.

My theory on this is that the colour and smell of the origional pale yellow DPPP is a result of phorone dihydrochloride/ pentachlorophorone entrapped within the crystall latice of DPPP. Allowing the crystalls to sit in the mother liquor at room temperature overnight frees the unreacted precursors through use of the solubility equilibrium, the precursors then react with the remaining H2O2. This process occurs untill all the precursors have been used up, indicated by a clear solution.


EDIT: Rosco, I cannot stand very spicy food, I have acid reflux:( I am fine with moderatly spicy though.


[Edited on 9-1-2005 by rogue chemist]




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Rosco Bodine
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[*] posted on 9-1-2005 at 15:17


The DPPP that I have is nearly dry and the odor / irritant property is at least 75% decreased for the relatively dry material , so it appears the offending substance is something else which has attached itself as an impurity or is a byproduct in the reaction mixture . Whatever it is appears to be more volatile than the DPPP since it slowly dissipates from a layer of the damp crystals exposed to air . It could well be occluded pentachlorophorone trapped in the crystal matrix of rapidly forming crystals , in which case slowing down the
precipitation , and I mean slowing it way down could result in much purer crystals not containing so much of the "tear gas"
component . This could also be related to the temperature at which the reaction is
performed and the level of agitation . The precipitation of DPPP crystals could be slowed by simply slowing down the rate of addition of the peroxide . The presence of some nonreactive solvent added to the reaction mixture could help also , possibly some methylene chloride or chloroform or methanol in small amount would be useful in precipitation of purer crystals .

It is possible that the 90% yield reported by the patent is because the other 10 % of reaction product is some undesired and
perhaps unavoidable byproduct , and that this byproduct is the irritant material . If we can determine what it is or how to eliminate it , by any sort of neutralization or crystallization strategy , even to substantially reduce its concentration would represent a great improvement .

Perhaps there is improvement from simply letting the reaction mixture stand , which could be complicated because of "rafting" of the crystals , after which they rise like bread dough and overflow the container , remedied by keeping the mixture stirring moderately for an extended time to keep any bubbles dispersed . Perhaps limiting
the excess of H2O2 used to only a minimum excess , or other strategies could clean up the product .
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The_Davster
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[*] posted on 9-1-2005 at 15:52


Quote:
Originally posted by Joeychemist

Rogue, you experienced no effects like a runny nose or soar throat? You didn’t even shed one tear? I’m not sure what to say or what to do now? This thread is going to be 50 pages before we figure this one out.
:(:(:(:(:(



I had a family member go into the lab and they did not experiance an overpowering smell either. Just to test that I am not somehow resistant to it.:P

Does anyone have any thoughts on what the white chlorobutanol smelling substance is? I heard mention of diphorone hexaperoxide on roguesci could this be it? Or is just a purer form of DPPP? DPPP could be cream colored as a result of incomplete peroxidation which allows a chlorine atom or two to stay on the carbon chain of the phorone part of the DPPP molecule. I have no idea what this is...

[Edited on 9-1-2005 by rogue chemist]




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[*] posted on 9-1-2005 at 16:13


The very surface edges of the crystals of DPPP which I have been air drying have
tinged with white or very nearly white ,
as if the color was faded and the edges
of the yellow crystals were bleached out nearly white . It looked sort of like a thin
layer of white frost on the surface of the crystals exposed to the air . But of course it isn't cold enough for it to be frost so it is evidently a loss of color on drying , and
all the crystals are somewhat lighter in color , even those not directly on the surface . I noticed this when stirring the
drying crystals to smooth out any clumps and speed the drying .
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[*] posted on 9-1-2005 at 16:37


I too noticed that loss of colour in my DPPP while it is drying, the assumption I made on the previous page of this thread may have been correct about unreacted precursor within the crystall. However I am still looking for an explanation for the smell of my new crystalls, it is nothing like DPPP. The smell of the pale yellow DPPP will have to be determined after a long period of time. It is possible that the smell of the more volatile component overpowers its actuall smell. Anyone who has experianced nearly lachramatory DPPP, when you made your phoronedihydrochloride, was there an oil slick on the surface? the milder odor of mine could be attributed to only a very small oil slick. Perhaps this oil acts as nucleation centres for the precititation of the DPPP, and then evaporates slowly later.

Most of this could be wrong...




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smile.gif posted on 9-1-2005 at 17:20


I just recrystallised my DPPP in 100% pure rubbing alcohol. The yellow tinge is completely gone and the smell has decreased quite a bit--- it looks slightly green and smells similar to AP. When detonated--- this material maintains its high power and no smell or smoke is produced.

this is one way of doing things :)
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