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Joeychemist
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I wonder
Well that’s just it pyroz, pure phorone can be any color ranging from a light yellow to a dark green, so I would imagine that the derivative
compounds of phorone and similar or other related chemicals (phorone dihydrochloride, pentachlorophorone) could be any color as well, therefore there
might not even be a pure color of DPPP. But from what I have gathered it’s not white like AP.
Rosco, just a thought, but if you heated the Acetone/HCl until a very thick pure layer of phorone is left. You could used a separatory funnel to
separate the two layers, Then you would have the pure sample of phorone and the bottom solution of…phorone dihydrochloride and triacetone
dialcohol??-is this right?) left over, you can then experiment much more efficiently and be more conclusive in you’re testing and results.
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Rosco Bodine
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| Quote: | Originally posted by JoeychemistRosco, just a thought, but if you heated the Acetone/HCl until a very thick pure layer of phorone is left.
You could used a separatory funnel to separate the two layers, Then you would have the pure sample of phorone and the bottom solution of…phorone
dihydrochloride and triacetone dialcohol??-is this right?) left over, you can then experiment much more efficiently and be more conclusive in you’re
testing and results.
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In my estimation there is *never*
any phorone itself produced , but a phorone related derivative , phorone dihydrochloride , which forms from the further reaction of HCl with
triacetone dialcohol . In a basic system the triacetone dialcohol might yield phorone by dehydration , but in this acidic system the reaction blows
right past phorone to form the dihydrochloride of phorone . I believe the separated layer is not a different substance from what remains in solution .
When and if enough of it separates so that the color of the layer can be observed , this will be further information of possible value . Another
possibility is that the oily precipitate is a monohydrochloride derivative of phorone ,
or some "ether" of triacetone dialcohol ,
or possibly some other minor polymerization product . I may leave the reaction mixture for a week to digest at 70 C , simply to observe any changes
and so long as changes are occuring , let the reaction run its course until no further reaction is evident . This reaction mixture reminds me
greatly of the condensation reaction of benzaldehyde and nitroethane in the presence of a small amount of butylamine , to form phenylnitropropene ,
with the expulsion
of water which then floats on top of the
hot reaction mixture . That digestion is
steady for several days , even up to a week before it completes . And it is just my guess that this condensation may follow a similar course .
Driving these sorts of reactions with heat can make them finish more quickly , but reduce the yield and cause increased formation of undesired
byproducts of the "highly colored higher polymers" variety . Whether that applies in this case is unknown . But I am in no hurry so I will
probably just let the mixture "steep" ,
incubating it to see what will "hatch"
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vulture
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| Quote: |
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.
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Don't push your luck by getting cocky mister. I do understand the concept of LAN sharing as I am the network admin in two such cases, for a total
of seventy users, thank you.
I therefore also know, that those users usually are in the same building and happen to talk to eachother, certainly if they share interests. Funny you
don't address this point, which I mentioned earlier. Maybe you don't understand the concept of reading?
One shouldn't accept or resort to the mutilation of science to appease the mentally impaired.
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Rosco Bodine
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It can get confusing who is who on a LAN .
It is sort of like being at a convention for cross dressing multiple personality bisexual Wiccans , very difficult at any particular moment to know
for sure just which witch is which  
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Matsumoto_Hideki
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Vulture give it up! please/ new discovery?
enough with that same IP = same person crap.
Roomate is my main host though the LAN. He is away notice PYROZ is not logged on at the moment.
... I think I just made a new discovery about DPPP... I think there may be derivatives? After letting my Phorone HCL sit overnight I then took 30ml of
the dark red liquid out and added 0.8ml of HCL and let the entire solution settle. The solution layered and a thick black liquid shot to the surface
after about 2mins. I then proceded to peroxiate it, and this material smells a hell of a lot like woops not camphor but Acetone.. aha there are lumps
of AP in my DPPP that is why... , however the yellow crystalline material has exactly the same characteristics of the stuff featured on my webshots
account (dark orange). You can see there is a white material mixed in the form of lumps. These I think are not AP as they do not resemble anything
like it. I have yet to test these lumps to see if they will behave like AP in flame, yup they did. yellow stuff deflagrates with a sharper snap ...
weirdness
[Edited on 30-12-2004 by Matsumoto_Hideki]
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Rosco Bodine
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The oily material which is floating on top of my acetone / HCl after 24 hours @ 70 C is a water clear material , unlike the highly colored mixture
from which it is precipitating . Anybody care to venture any theories on what the clear oily precipitate may be ?
There is also a very strange looking sort of barely perceptible motion on the surface of the dark red liquid , almost as
if there were thousands of tiny bubbles
effervescing from the liquid , but the liquid is so darkly colored that the cause of the surface "animation" cannot be seen even in direct
sunlight , the surface of the liquid seems to be "vibrating" is the only way I can describe the effect , and I have never before seen
anything like it . There is no vapor pressure being produced , so I have no idea what to make of this "Brownian motion" on steroids !
[Edited on 29-12-2004 by Rosco Bodine]
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Matsumoto_Hideki
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Video and thoughts
Well I think you might have some H2O if your reaction totally finished???
Here is a video of that yellow material deflagrating. Notice it makes a real whoomp whereas AP deflagrates with little noise at this amount, at least
in all the batches I have made.
Attachment: 100_2557.MOV (553kB)
This file has been downloaded 1454 times
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Rosco Bodine
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| Quote: | Originally posted by Matsumoto_Hideki
Well I think you might have some H2O if your reaction totally finished??? |
There is already about 158 ml H20 present from the 200 ml of HCl 31.45% which were added at the beginning , plus 36 ml more of water formed from the
dehydration of triacetone dialcohol , and the clear preciptated oil is more viscous than water , more like "white mineral oil" in appearance
. I am thinking perhaps it is a bit of unreacted triacetone dialcohol or an ether thereof .
I have been thinking more about the strange vibrating effect I have been observing on the surface of the reaction mixture , and perhaps it is
something like what a "lava lamp" does with two immiscible liquids which are close in density but that changes as they heat and cool . What
I am thinking is there may be an emulsion that is being circulated by the heat , and I may get a phase separation if I let it cool , so I am going to
do that and see what happens .
[Edited on 30-12-2004 by Rosco Bodine]
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Matsumoto_Hideki
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Another DPPP breakthrough?
it looks as though major breakthough has occured on rogue science in the synth of DPPP.
I need more evidence that this is really DPPP and not phoronated Triacetone Peroxide. i do think this is the target chemical however...
Member by the name of The_Rsert has done it!!
http://members.fortunecity.de/potatoguns/DPPPSyn.html
He is cooling his material down, this is what happened to me when i did mine on top of a cool fridge in a wide container and this is probably why I
was unable to reproduce my success. If the temp goes above 5c the reaction overheats and TCAP %ile increases with a lower Diphorone Pentaperoxide
yeild. I think finally someone has a properly documented method of making DPPP. I would be very interested in knowing the detonation/deflagration and
other physical characteristics of this material R_Sert has produced.... It looks so simular to the material I obtained that I took a picture of on
(webshots)
I am sooo interested!!!!  Boy oh boy this is like Xmas all over again.
[Edited on 30-12-2004 by Matsumoto_Hideki]
[Edited on 30-12-2004 by Matsumoto_Hideki]
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Tweenk
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The rxn proceeds not quite as stated on this site... IMO this sholud happen only in alkaline conditions like all aldol condensation reactions :/ No
idea why this sholud work
And now we add powdered sugar to the previously liquefied chlorine dioxide...
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Matsumoto_Hideki
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?oh What do you mean.?
You don't think it worked? not sure what you said?
I am just making a batch at about -32c and it seems aOk so far.
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Tweenk
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Well I'm wondering why this procedure works (or seems to work) when the reaction conditions are totally different from those supposed. Everything
that should be happening is chlorination of acetone to monochloroacetone.
[Edited on 30-12-2004 by Tweenk]
And now we add powdered sugar to the previously liquefied chlorine dioxide...
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Pyroz
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You can't get chloroacetone from heating HCL with acetone. Chloroacetone is formed with raw Chlorine bubbled through acetone---its quite a
different process. HCL will digest the acetone into a Phorone. Once the Phorone appears it will go from a clear yellow liquid to a red, then it will
darken until the liquid no longer passes light. At this point, the liquid begins to thicken as unreacted acetone is vapoured off. Phorone diHydrogen
chloride is left behind.
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Matsumoto_Hideki
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Yes. Please go see R_Sert's page
R_Sert has proven the power difference as well although he was unable to measure due to the fact his scale has a minimum of 0.5g he provided some
AVI's showing the power difference between DPPP and AP. The results are quite what I had expected and should provide evidence to those who
doubted my orignal conclusion about DPPP "before I was banned from here."
Does anyone remember those videos of DPPP I posted several weeks ago? ie) like the one with the exploding foil?
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Tweenk
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Chloroacetone is made by bubbling Cl2 gas through a solution of acetone in HCl, the process is not similar to chlorination of alkanes (it involves
addition of Cl2 to a double bond of enolized acetone, and not the addition of atomized chlorine).
This must be one of those reactions which go completely other way than most people think.
And now we add powdered sugar to the previously liquefied chlorine dioxide...
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Matsumoto_Hideki
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agreed this is a strange reaction.
Well all i can tell you is if I had made Chloroacetone I would know about it as it is incredibly volitile and deadly. As I said it was used as a
blister agent in WWI and in WWII by the Japanese. "I have heard this"
Also i don't think chloroacetone is a liquid at room temp... Correct me if I am wrong.
Black liquid is phorone HCL without a doubt.
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Tweenk
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To make something clear: I do not doubt if it has formed, but how has it formed
It's very strange.
Is HCl driven off from the mixture during evaporation of unreacted acetone, or is it still there when you add hydrogen peroxide?
[Edited on 30-12-2004 by Tweenk]
[Edited on 30-12-2004 by Tweenk]
And now we add powdered sugar to the previously liquefied chlorine dioxide...
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Rosco Bodine
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The time is approaching 48 hours on my sealed bottle experiment . And a new development has appeared , a slight pressure was evident the last time I
loosened the cap , giving that pffft sound of escaping gas when the cap was loosened , and then I saw immediately a slight refluxing of vapor on the
inside walls of the neck of the flask . The temperature of the liquid measured 66 C ,
and no free boiling was noted when the pressure was released . This is the first appearance of any pressure or refluxing since the end of the first
hour when the
spontaneous exotherm had ended . I believe the extended heating for 47 hours at 66 C has possibly reached a point of diminishing return , and this
development of slight pressure is possibly
a marker , and indicator of some decomposition of the product of earlier reaction , or further conversion perhaps to some ether or halogen-ether
derivative . More simply , perhaps there
is a reversion to acetone or an alcohol of
some kind . I will end the supplemental heating now at 48 hours and allow the
mixture to stand for further observation .
The drop of material left as residue on the thermometer tip stained a white paper towel an orange brown color almost identical to the color of fresh
iron rust .
In thin layers which sheet across the glass when the bottle is swirled the liquid remains bright yellow , although en masse it looks ink black with a
dark red tinge , to the surface . The mixture seems to have a physical property and viscosity more like an emulsion than a solution , but it does not
separate into 2 phases except for a slight oily slick which has remained only a few ml , floating on the surface . It appears that it could possibly
be separated by centrifuging or chromatography . But that may worsen the ability to get it to react in the peroxidation reaction , if concentration
should result in a water imiscible product .
Update on sealed bottle experiment :
After cooling and standing for six hours an upper layer about 3 mm thick is visible , and its color appears darker and
more consistent than the majority of the
mixture below . The color difference is distinct , but barely perceptible because
both layers are so very dark colored . To see the interface between the layers requires bright sunlight . Swirling the bottle so that the mixture
flows upwards across the inner surface of the bottle and then flows in a thin sheet across the glass as it drains back down , it is evident that a
complex mixture which is an emulsion has formed , containing at least two and perhaps three liquid phases which are so very near to each other in
density that the mixture is mostly a dispersion of very small blobs . There is a distinct separation of colored and clear oily phases visible in the
thin sheet of liquids flowing across the glass after the mixture is swirled . But the separation is not clearly so visible in the dark liquids mixture
en masse . After observing that this upper layer of more consistent and dark color is growing in thickness , I have decided to return to heating the
mixture for a further time to see if the conversion of the lower layer continues . I am uncertain whether there is any difference between the upper
layer and the lower layer , except for the water content , or if the upper layer is a actually a different compound accumulating as an end product of
the reaction proceeding in the mixture below . This mixture is complex , and so very darkly colored as to test the observers skill at distinguishing
what are differing shades of "blackness" so small in contrast as to strain the eyes to see the difference , which is never the less ,
visible there . The progress of this reaction is
important to understand , in identifying which component of the complex mixture is indeed the actual precursor for the DPPP , and how to optimize its
yield in this step in order to get the highest yield of DPPP in the subsequent peroxidation .
And even if it is not necessary to isolate the active precursor , it would be good to determine the markers for the reaction which indicate completion
of the formation of that precursor and where is the point it has formed in highest yield , or at which point its form , whether emulsified or
separated will afford the highest yield of DPPP upon peroxidation . Understanding these variables will be necessary for optimizing the process for
synthesis of the DPPP .
Another curious observation regarding this very strange mixture concerns the rust colored stain which a drop of the mixture made upon a white paper
towel .
After sitting overnight , the dark red orange stain faded away leaving only a light tan colored spot on the white paper .
Go figure !
[Edited on 31-12-2004 by Rosco Bodine]
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Pyroz
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acetone peroxide vs DPPP
here is a movie I made to show the difference of the two materials... the sound is poor but notice the sharp cracking as the yellow power ignites.
---this is DPPP without a doubt.
Attachment: deflagration.mov (810kB)
This file has been downloaded 1529 times
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Matsumoto_Hideki
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Just finished a low temperature DPPP syth from totally digested Phorone HCl
The colour of DPPP is bright yellow almost green-yellow and not red-brown. Red brown colouration is unreacted Phorone HCl crystals tinting the DPPP.
This was giving me the black smoke last time I had a sucessful synth and tried some out. There was also an unusual odor of phosgene-like smell, sort
of like when methyl chloride burns. This bright yellow stuff has no odor after detonation or deflagration.
btw also I tried a test against AP and there is a much noticable difference in detonation characteristics.
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Pyroz
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Movie of detonation 0.1mg TCAP/ DPPP
Aliright first movie is of TCAP detonating via compression in Al foil on top of a copper strip 2mm thick. A flash is visible, notice that the strip
moves quite abit and no crater is created in the copper. The detonation temperature is higher than that of DPPP.
I wasn't about to mesure surface temp next to it.. As I would like to keep my fingers.
Video #2 DPPP. No flash! In fact there actually was one but it happens so incredibly fast the camera didn't pick it up. My camera is set at
15fps movie mode. Notice the crater on the metal surface.
both The TCAP and DPPP were mesured out very very carefully on an electronic scale.
[Edited on 31-12-2004 by Pyroz]
Attachment: detvideo.mov (662kB)
This file has been downloaded 1424 times
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PainKilla
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I am not sure...all those vidoes look pretty similair, we need a lead block test realyl to see what's better. There might have been no flash as
it might have just been in between frames... I will hopefully do some conclusive testing soon...as soon as I stop being lazy.
Of course, I am not sayign what you have is fake or anything, just not anywhere near the power of the patent. Unless this has a VoD of 6000 or is
consideribly less sensitive I will still be using AP as my primary, until I get a still anyway or some well, no just a still :p.
Can you perform some sensivity tests? Dropping a weight from varying hieghts? This would be much more conclusive. This could be some of AP possibly
too... here is another idea....what happens when you add perxoide to chloroacetone?
[Edited on 31-12-2004 by PainKilla]
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Rosco Bodine
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A fairly easy to do brisance test might be possible by making a putty of a weighed amount of AP and weighed amount of binder , compared with another
putty
with DPPP subsituted for AP . Each could be detonated on a witness plate and the damage compared . A soft aluminum sheet metal such as used for
roof flashing is ideal for small charges . A more brisant material will show a cutting effect upon the metal , while a lower brisant sample will do a
lot of tearing and banana peeling
of remaining attached shards on the underside of the material , if the witness plate is placed over the open end of a coffee can for example . The
fragments will leave their signature on the bottom and walls of the can also giving witness to
velocity of the fragments , which is related to the brisance of the sample charge . Whether or not DPPP would make a similar putty with
nitrocellulose made into a thick syrup with acetone , as does AP , and whether or not it would be reasonably stable like AP putty is unknown . Using
dextrin as a binder is another option for making such test pellets . These should detonate easily from a touch with a glowing splint or spark from a
fuse .
[Edited on 31-12-2004 by Rosco Bodine]
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Mickhael
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Testing DPPP
Although I am very enthused about trying DPPP out, I'm still relatively new to working with peroxides and I want to be very careful with them. So
suffice it to say, I'm waiting on a more solidly tested synth, before mixing it up myself. Also because I don't have much lab equipment
beyond a mixer, thermomiter, freezer, glassware and safety wear. If anyone thinks they have a fairly safe synth (not likely to form AP) I will happily
try it out, I have a digital camera and such that will make documenting easy.
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Rosco Bodine
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| Quote: | Originally posted by Mickhael
Although I am very enthused about trying DPPP out, I'm still relatively new to working with peroxides and I want to be very careful with them.
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Thoughtful regard and study of such reactions is the credential of those who are still living after much
time experimenting with energetic materials , and there are no "old" fools left to tell of their experiences speaking from their golden
years , since mistakes are inconsistent with longevity in this area of scientific interest | Quote: | | So suffice it to say, I'm waiting on a more solidly tested synth, before mixing it up myself. |
That work is yet in progress | Quote: | | Also because I don't have much lab equipment beyond a mixer, thermomiter, freezer, glassware and safety wear. If anyone thinks they have a fairly
safe synth (not likely to form AP) |
The presence of AP should not adversely affect the safety at moderate
temperatures , and there is likely no significant amount of AP going to be produced by the current method . | Quote: | | I will happily try it out, I have a digital camera and such that will make documenting easy. |
None of those
things being lacking is the impediment now , it is just a matter of time and charting experimental results to pin down the details of an optimized
synthesis . Have patience as it could take some time to analyze all the data from different experiments and arrive at the definitive conclusions for
what works best , even if it is never completely understood exactly why .
There have been some uncertainties I believe for some to believe that three acetones polymerize and then further react with two HCl . And yet the
same doubters surely know that in the case of AP , there are what else but three acetones condensed in the presence of HCl under different conditions
and peroxidized to form the *trimer* of acetone then peroxidized . The dimer , trimer , tetramer *are* themselves acetone derived polymers , so the
matter that acetone derived polymers do exist is substantially already proved by AP itself .
The peculiarity of DPPP is that it is a variant on the same theme , but having a reaction scheme made to follow a different course , resulting in a
quite different "polymerized acetone peroxide" variant .
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