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Pyroz
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cool! Glad to hear that you've had a fairly successful go at making DPPP.
If you want a better yield you might want to try leaving the boiled Acetone+HCL mixture go black then.....
Leave the solution at room temperature for at least 24hours and the liquid volume will decrease quite a bit. Remember you are using 30% or so HCl
---70% water ---there will be considerable amount of acetone left over unreacted. Unreacted Acetone will create dreaded TCAP almost instantly in this
procedure when reactants are added. You are looking for a solution that has an oil like consistancy.
Your yield should be pretty decent---- german patent states 90% yield--- that seems a little high for me. I'd say 60% being more reallistic.
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PainKilla
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Just a note for everyoone, be careful when working with all this stuff because there is a very good chance it is cancerous, or toxic or mutagenic
w/e....
I will be trying this synth most likely thursday, using both Cl and non-cl methods, with luck, I'll be able to get some conclusive results, as
the Cl method cannot be used in formation of AP, at least as far as I know.
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mr.pyro
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Pyro z,
How many ml of reagent do you have there in that jar, it seems you have a fairly large yeild of DPPP in the previous pictures. When you heat your
Phorone DiHydrogen Chloride, do you do it covered, uncovered? How Long Approx? And you let it sit out, and it changes I presume from Dark Red to Black
and thickens up.
My Phorone DiHydrogen Chloride after boiling for an hour or so lost about half the volume and is dark about as dark as red wine, but not black at all.
I will leave it out tonight and see what happens.
I also will tommorow do some testing with making this stuff, I shall boil 2 large batches of HCL+Acetone One covered, One Uncovered for 2 hours each.
Then I will seperate each batch into 4 equal amounts each One covered into the freezer, one uncovered in the freezer, one covered laid at room temp,
and one uncovered at room temperature. I want to experiment to see which one(s) will make the thick black motor oily Phorone DiHydrogen Chloride.
[Edited on 28-12-2004 by mr.pyro]
[Edited on 28-12-2004 by mr.pyro]
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Pyroz
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I have about 1L of phorone dihydrogen chloride in a mason jar.
Phorone diHydrogen Chloride will darken if left at room temperature for several hours. After 24 hours the solution will stop reacting a should be
black oily and viscous.
Likely your acid/Acetone mix will continue to be warm well after you've taken the heat off of it--- the reaction is still continuing.
If you are saying that after heating the mixture you have a red-wine like solution it either means you've added too much acid which can be easily
corrected by adding in more acetone--then heating the mixture back up again to 80-100C for 30 minutes
---or the reaction needs a little more heat to get it polymerizing into a phorone-- this does happen some times due to acid concentrations. Keep a lid
on it while boiling--do allow gas to escape by making some air holes in the contianer lid! When the solution is cooling off leave the lid off of it...
it will become darker as the free acetone vapours off.
[Edited on 28-12-2004 by Pyroz]
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Rosco Bodine
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| Quote: | Originally posted by Joeychemist
It looks like Rosco is doing most of the work here. I think that you are correct with most of what you said and upon a second glancing of the patent
it is actually quite obvious now what reaction is happening. But why the hell don’t they specify and elaborate, I mean why the hell wouldn’t
patent specify such important details, I guess they felt it wasn’t necessary. I do however think that the procedure mentioned above is working but
it is rather vague and some mistakes need to be fixed but I think we have something to go by now, something to build on. This latest information you
have provided is the most crucial piece of the puzzle we needed. |
One thing I have considered is that the
inventor may not even be certain himself what exactly is the reaction mechanism for the compound he invented .
[snip]
| Quote: |
Rosco, since you do not wish to waste you’re reagents and you have obviously put fourth you’re time and effort into identifying the reaction which
occurs, I am willing to waste mine to further our knowledge and understanding of DPPP as well. Just let me know if there is something you would like
me to try or test. I have used the last of my acetone and must get more to further the testing. |
Something
which I have considered possible is that a phorone monohydrochloride may actually be the precursor desired , ( at least as a first polymerization
product ) and that if this is true then essentially twice as much HCl as needed initially may be what has been used in efforts so far . A hint at
exploring this possibility is demonstrated when adding some extra HCl to the "red oil" before the peroxidation step . The thing I have
wondered is if the initial formation of a monohydrochloride derivative of phorone is preferable for the first step where acetone is polymerized by HCl
, and then there is added an equal amount of HCl and perhaps a subsequent heating to complete the reaction in two stages , which forms the phorone
dihydrochloride . This strategy may possibly improve the yield by decreasing the formation of undesired higher polymers which could be produced by
the higher initial acidity of the present approach . I can't really provide any better justification for testing this theory than it is simply
a suspicion which may or may not have any bearing , but it is one variable that did occur to me as possibly worth testing . Another variable is the
amount of peroxide described by the inventor seems to be excessive , but the amounts you are using seem more in agreement with theory . My estimate is
that it would do no harm to reduce the amount of hydrogen peroxide specified by Mackowiak by about 15% , in its relative
amount in proportion to the acetone . And as I mentioned earlier , the HCl specified by Mackowiak seems excessive by a slight amount also . These
proportions and probably the method also could be refined by small adjustments . The details of how Mackowiak achieved a 90% yield may be proprietary
, and the result of his own fine tuning of a process whose details are the secret we learn little by little by experiments .
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mr.pyro
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Well good, I was heating that red wine batch at 60 C for about 1 hour, I think it needs more heat? As soon as I took it off the burner it went right
into the freezer. Is that stopping the reaction from polymerizing into Phorone Dihydrogen Chloride.
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Pyroz
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It will likely will slow down the reaction to a snails pace if you put it in the freezer--I'd warm it back up and leave it uncovered on a shelf
and allow for it to digest. It should be nearly black by the morning---
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Matsumoto_Hideki
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More pics coming of other syth with explosion footage!
Sorry for the long post
Edit] I just realized why the yield was so shity. J-scan is off on his measurements and I followed his instructions carefully so while scaling down
the procedure I didn’t even notice the error. That tard J-scan is using two parts 35% H2O2 when the patent calls for two parts 30% H2O2, so I wasted
precious H2O2 because this fool mis-calculated and I assumed he was right. But still that little miscalculation did not affect my total yield that
much. Like I said there are problems that need ironed out.
[Edited on 28-12-2004 by Joeychemist]
Are we trying to start another war here? Joey that is immature! We understand your pain. errors are what make science a challenge. live with it.
EXPERIMENT #15 Room temp Phorone HCL production.
I just did another batch of Phorone and I am letting that react at approx 20c. I would like to cold form it so that I can study the reaction even
further. I will keep you guys posted with pics.
--------------------------------------------------------------
1:1.1 1 part Acetone to 1.1 HCL 35% Muratic acid
flask is sealed shut.
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vulture
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Warning
You are again using different usernames to talk to yourself. Schizophrenia is treatable, go see a neurologist. Otherwise be banned and this time by
IP.
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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Matsumoto_Hideki
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Vulture WTF?Not this again, short memory?
Nope... Please pleaseeeeeeeeeeeee, understand the concept of the router.
The IP adress being the same is because I am on a LAN. You are a gatekeeper so I assume you know computers.. ie) Local area network. I am one of 3
compters. 
[Edited on 28-12-2004 by Matsumoto_Hideki]
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vulture
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You just don't get it, do you? Do you really think everybody on this board is stupid?
If you are on a LAN, you don't need to talk to and ask people that are on the same LAN, because you can speak to them IRL. I know sock puppets
when I see them.
[Edited on 28-12-2004 by vulture]
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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Pyroz
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Hey vulture--- you mind if we keep topic on track. Rather than lashing out at a particular user lets start cooperating and share some valuable
information here.
Thanks.
PS. for someone who is a gatekeeper you sure don't get the concept of sharing a network connection. I am the host for hideki and I've talk
to the admin of this site--- you may contact me if you have problems understanding this. Thank you for listening.
[Edited on 28-12-2004 by Pyroz]
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mr.pyro
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I tried today boiling 200mL Acetone + 300 mL HCl at 100 C. After about 15 min it was vaporing off alot of white vapor that smelled of chlorine.
Also, It boiled off about 100 mL of reagents in that time, I tried to keep a cover on it, but it would have burst the saran covering it. After about
20 min or so it was a little darker then piss yellow, but I couldnt stand the fumes so I dumped it down the drain. What is going wrong. PyroZ how
did you manage to make 1L of Phorone DiHydrogen Chloride? It seems like I was loosing way to many mL by vapor then I was supposed to.
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Pyroz
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| Quote: | Originally posted by mr.pyro
I tried today boiling 200mL Acetone + 300 mL HCl at 100 C. After about 15 min it was vaporing off alot of white vapor that smelled of chlorine.
Also, It boiled off about 100 mL of reagents in that time, I tried to keep a cover on it, but it would have burst the saran covering it. After about
20 min or so it was a little darker then piss yellow, but I couldnt stand the fumes so I dumped it down the drain. What is going wrong. PyroZ how
did you manage to make 1L of Phorone DiHydrogen Chloride? It seems like I was loosing way to many mL by vapor then I was supposed to.
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...you had the reaction going, and you should have continued to heat the material for at least another 20-25 minutes. You would have seen a major
colour change--- and it would have gone much, much darker.
Punch a few holes in the top of your saran covering to prevent the saran lid from bursting. As for loosing a large volume of liquid-- this is
unavoidable. I started off with 2L of acetone+HCL ----I have 1 L left and its really concentrated material. It is so dark light does not pass through
it. It also has a flowery smell to it unlike acetone.
hope this helps,
feel free to send me an email message and I'll see what I can do to help.
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Joeychemist
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| Quote: | Originally posted by Pyroz
Punch a few holes in the top of your saran covering to prevent the saran lid from bursting. As for loosing a large volume of liquid-- this is
unavoidable. |
It is avoidable with a slow hot water bath on a hotplate. As long as you are careful not to let the acetone/HCl/phorone solution boil
your loss will be minimal, this has already been said
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Matsumoto_Hideki
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just concentrated more Phorone HCL
I am starting a slightly different Phorone HCL
synth using 100ml Acetone to 110ml HCL 40-42% vol muratic acid.
We will see what comes from this.
QUESTION FOR ALL OF YOU WHO HAVE ATTEMPED TO MAKE DPPP... Has anyone been able to get the dark orange material that I have fetured on webshots? Has
anyone had that as a precipitate yet? What properties did you notice about it?
BTW... Agreed Joey in the last batch one container that pyro did actually polymerize, I guess this is due to him getting the solution too hot to
fast. ( a brown/yellow plastic formed on top of the Phorone HCL. A slow boil 60-90c on low is better idea. Good suggestion, as I had my best results
from this heating method.
---Pyroz, no the black liquid that you are reffering to has a hidious smell to it and reminds me of the worst tar smell you could imagine.. putrid.
Pyroz is away and won't be back until tommorrow early. I am using his computer right now.
[Edited on 29-12-2004 by Matsumoto_Hideki]
[Edited on 29-12-2004 by Matsumoto_Hideki]
[Edited on 29-12-2004 by Matsumoto_Hideki]
[Edited on 29-12-2004 by Matsumoto_Hideki]
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Rosco Bodine
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An experiment was begun today to perform the acetone polymerization to phorone dihydrochloride , using a closed
pressure vessel to prevent escape of vapors and maintain the proportions of reactants . A sparkling wine bottle 750 ml capacity , having a threaded
aluminum cap with a poly sealing gasket has safely contained the reaction mixture for eight hours so far . In the bottle is 225 ml acetone to which
was added 200 ml of HCl 31.45% , and the bottle sealed firmly but not overly tight using the threaded bottle cap . The mixture warmed spontaneously
to about 60 C and the gentle exotherm continued for 45 minutes
as condensation on the upper portion of the sealed bottle formed and trickled back down the inner surfaces returning to the reaction mixture . At 45
minutes the temperature began to fall and refluxing vapors ceased to condense on the inner walls of the bottle . The color of the mixture had changed
from being clear to a pale yellow . Supplemental heating was applied using a small electrically heated water bath of the sort used to steep spices
to produce fragrances , a potpourri "crock pot" into which the lower third of the bottle fits with a bit of clearance at the sides . A
coffee mug warmer would probably work as well for
gentle heating for hours unattended .
I estimate the temperature of the bath is about 80 C . On the upper portion of the neck of the bottle is wrapped a moist layer of paper towels
secured with a rubber band , to provide some evaporative cooling if needed . At 2 1/2 hours the color is deepened to a bright yellow and at 6 hours
the color is a red orange tea color . At 7 1/2 hours the color
has darkened further to a dark reddish brown and the mixture is becoming opaque , taking on a dark milky appearance as if there was suspended
colloidal material as contrasted with simply a dark tint . The scattering effect on a light beam can be observed by shining a flashlight beam through
the mixture . It is planned to let the mixture
continue reacting overnight . One observation I did make is that even with supplemental heating , there has been no condensate of vapors observed
since the
original spontaneous exotherm tapered off leaving a pale yellow mixture which evidently at that point experienced an elevation of boiling point due to
the reaction product . So I am inclined to believe there is already a reaction product of some sort present in significant amounts even as early as
the end of the first hour , before any supplemental heating is applied . If the mixture was still chock full of unreacted acetone at the end of the
first hour , then it would seem likely that the refluxing would continue to be observed , and because it isn't refluxing then the acetone must
already be substantially combined to form some higher boiling point material . It would be interesting to monitor the pressure drop using a gauge or
manometer which would detect the sudden elevation in boiling point for the mixture , and try to determine what exactly is the predominant product at
that point . Except for the slight vapor pressure of the acetone which decreases to nothing at the end of the intitial exotherm at about 45 minutes ,
the reaction produces no further vapor pressure of any significance thereafter . I loosened the cap on the bottle from time to time to check for and
release any pressure and there isn't any acetone pressure evident after the spontaneous exotherm ends . I suspect that this point marks the
conversion of the acetone to triacetone dialcohol , and the slight tinting is due to
the early presence of some phorone dihydrochloride which appears later in increasing quantity and gradually darkens the color of the mixture . A
yellow dyestuff will appear darker and darker red as its concentration increases and its state of subdivison is decreased . The same effect can be
observed for picric acid where a boiling hot concentrated solution is very dark red , but one drop added to a liter of cold water will color it bright
yellow . The same for sodium polysulfide , dark red in the beaker , but bright yellow in a thin layer on a white surface . I think this is possibly
the same story for the phorone dihydrochloride . It's yellow for sure , so yellow it looks red ,
and even darker depending on its concentration .
[Edited on 29-12-2004 by Rosco Bodine]
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Matsumoto_Hideki
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Right on
Yes, before coming back to this form I was discussing my "success" with others on Rogue science. All I did was heat the red Phorone HCL to
black and then left it to settle for a few days. The solution darkend even more until it became oily. You should be able to clearly see the formation
of Phorone/ Phorone HCL on the top of the black liquid as a slick of sorts. This was my signal that digestion was nearly complete.
What you are describing is exactly what I saw before my "success". I am eager to see what happens when to try and peroxidate your
pressureized PHCL
*****I would also do a pH test to be safe..
****
I was just checking on my two containers of PHCl and one of them was red at the bottom knowing that i added more acid to acetone.. I added 1ml more
acetone and the solution beagn to reheat... aha..
my other container was almost completely black..
[Edited on 29-12-2004 by Matsumoto_Hideki]
[Edited on 29-12-2004 by Matsumoto_Hideki]
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Rosco Bodine
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I did notice some small thin rafts of solids floating on the surface of the reaction last time I checked to see how it was proceeding . I suppose the
mixture is oversaturated with whatever it is producing and some of it is precipitating .
After evaporating some of the water by
use of a shallow heated glass tray , I may
end up having to add methanol to get a good clean solution for the peroxidation .
Update : After the mixture has continued heating overnight , at 17 hours from the start of the reaction there is clearly an oil separating and
floating upon the surface , a small amount perhaps 1 or 2 ml , too little to form a separate continuous layer , but enough to be certain it is an
oily precipitate . The mixture is extremely dark red en masse , but when swirled so that a thin film can be viewed as it sheets across the walls of
the bottle , the solution is very bright yellow in layers thin enough for light to pass through .
And about the pH , I was going to hold
a strip of pH paper in the vapor above the hot solution and see if it would indicate any residual HCl vapor coming off the surface . I used just a
tiny bit excess of theory of acetone hoping to tie up as much of the HCl as possible and not have excess HCl to cause problems later over-catalyzing
the reaction and causing too rapid precipitation for good crystals to form . I am trying to implement some of the ideas which have developed as I read
these other posts , and try to discover any potential refinements , since the reported yields aren't yet squaring with the 90% reported by the
patent . Sheesh , I havent even added up the mole weight of DPPP yet to know what
to expect and calculate yields . My H2O2 is so old that I will have to do a specific gravity test to determine its strength and I know it's down
below 25% so that won't help , but maybe by drying out the excess water good from the phorone dihydrochloride , I can help make up the difference
for the extra water in the slightly diluted peroxide .
[Edited on 29-12-2004 by Rosco Bodine]
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Matsumoto_Hideki
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Sounds good so far.
I think you are probably going to have a decent batch,
you are getting soild masses which sounds good to me. I think that evapouration method is one i should give a go with increased surface area.
Although I didn't do that last time and I managed to yeild a full 1.5g.. I guess I just got lucky? The liquid I removed was from the top of the
solution that seemed to yeiild the product. As I said again it looked like "wulfenite"
red-brown clumpy crystals but would dry to finer product, the colour though stayed and never changed. In a flame a small amount would deflagrate with
a big wooomp and a small puff of black smoke. IF the crystals were held above a propane flame they would melt and then detonate with a terrific force
and no soot would follow. There was absolutly no smell either after detonation.
BTW...I get my H2O2 at the local hydroponics store for $32-35 CDN per 4L . I get a student discount of 10% though. It ranges from 35-36%vol.
My HCL is dirt cheap.. 35% for $15 CDN /4L
Acetone is $13CDN/4L
By the way could one use calcium peroxide to make organic peroxides? My organic chemisty is weak I know..
Woops, I can't get better than 42%, ohk.. solves that problem/
[Edited on 29-12-2004 by Matsumoto_Hideki]
[Edited on 29-12-2004 by Matsumoto_Hideki]
[Edited on 29-12-2004 by Matsumoto_Hideki]
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Joeychemist
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IICR, there is no such thing as 70%HCl. You can use calcium-peroxide in most cases, but why? I don’t know if it’s cheaper of not. You would be
left with Ca and H2O as a by-product, this could complicate some procedures.
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Matsumoto_Hideki
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My orange red product deflagrating
Well here is some video of a microsized amount deflagrating in a candle flame.
this amount is maybe 1-2mg? about the size of drop of water
slow the video down and you may be able to seet the black soot.
[Edited on 29-12-2004 by Matsumoto_Hideki]
Attachment: 100_2533.MOV (239kB)
This file has been downloaded 1229 times
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Joeychemist
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Check this out.
http://members.fortunecity.de/potatoguns/DPPPSyn.html
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Pyroz
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It would be interesting to know what colour DPPP is in its true-pure form. This would cetainly help to quickly identify DPPP from other peroxides 
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Rosco Bodine
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There is for me some uncertainty that the compound DPPP and its precursors are even correctly designated in the patent . It seems entirely plausible
that there could be some variations upon the structures specified by Mackowiak , and I am curious as to what lengths the process of accurately
identifying the precursors and end product was taken ,
and how accurate is the reaction scheme stated by the patent .
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