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Author: Subject: Diphoronepentaperoxide (DPPP)
Jome
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[*] posted on 5-1-2005 at 09:35


My solution has turned clearer after I evaporated acetone (and some water), that "upper layer" (same sticky substance that is on the jar walls) is hardly visible.

EDIT: Of course thats gotta mean that the tarry shit is no longer soluble when the acetone is evaporated, thats why it seperated out and formed an upper layer.

If I get what you are saying, rosco, then my solution has hardly even begun to decompose? Sounds great :D

[Edited on 5-1-2005 by Jome]




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Matsumoto_Hideki
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shocked.gif posted on 5-1-2005 at 12:52
detvol .. how to prove? ideas?


Well, Joey I think I am going to make a big batch of detcord now that I have proper instrictions and tips from those who are on Rogue science forms.
After seeing the damage a .223 cal shell did @ 1.93g I have do doubt the devol is close to the mark reported by the patent. I took my test plate to a blaster and showed the results off to him. His comment was that the crater from the DPPP side reminded him of a very high velocity explosive. futher evidence of the speed of detonation was the fact that none of the shell casing could be recovered other than a very tiny piece of the primer and rim, also the entire blast area was coated in brass dust about the size of diatomcious earth/cerium oxide polish.. So with this fairly unscientific method of Dvol measure I will try to make some detcord. I will be posting a movie this saturday when I go and test it at the local range.
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[*] posted on 5-1-2005 at 13:03
The colour of the crystals


Could the yellow colour of the crystals be caused by some unreacted precursor that got "coated" in DPPP during the reaction and as such never reacted?



#261501 +(11351)- [X]

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[*] posted on 5-1-2005 at 13:14
Testing the VoD


Hideki
The VoD will be precisely measured by Boomer when he conducts these tests for himself. He made a machine that works fairly accurate. The only real testing you can do is measure and compare the damage to witness plates and other similar test because I doubt you have the necessary tool and equipment. I don’t even have that sort of stuff. Let boomer figure out the exact det vol and in the mean time it is safe to say that DPPP is considerably more powerful and brisance then AP.

You can read about Boomer's machein in the making your own detcord thread at RS.

[Edited on 5-1-2005 by Joeychemist]
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Matsumoto_Hideki
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[*] posted on 5-1-2005 at 14:21
Ah i see what you are talking about..


Yes actually I have just read the article on rogue science. that machine measures the detvol via breaking of two wires via a given length of explosive in a 1m long tube. time between the start and finish of the explosion = the devol m/s

As for the colour Nerro, I am 100% postive that DPPP is in fact yellow since I brought a 5g small sample of this material to around 70c in a hotwater bath and left it for 5 hrs. There was no sublimation of anysort and the sample weighed exactly the same amount as
before. Even after weeks or so the material still won't sublime. I think this is a sure idication that it is in fact DPPP.

[Edited on 5-1-2005 by Matsumoto_Hideki]
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[*] posted on 5-1-2005 at 14:23


Quote:

Forget phorone ! Erase from your mind that DPPP comes from phorone !

DPPP no more comes from phorone than trinitrobenzoic acid comes from benzoic acid .

The structural similarity and similar names is where the similarity ends .

Cast out the phorone demon right now ! Save yourself from this "phorone illusion" ,
or I shall be forced to perform an exorcism to rid us of this pretender ,
this pseudoprecursor who deceives with subtlety and causes confusion
to the washer of test tubes and master of the molecular ;):D

This rant was brought you by reading and rereading the first stumbling half of this mammoth gargantuan thread one too many times :D


In fact I also don't think you're correct about your phorone dihydrogen chloride theory. I don't have much time now to come up with a better explanation myself.

You could prove me wrong though if you were able to prepare the same black liquid from commercial phorone and HCl. :P
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[*] posted on 5-1-2005 at 14:32
What???


Dodoman, what are you thinking teasing us like that "I think you're wrong, but I got to go" WTF? Please share you're thoughts about this?

Hideki, boomer's timer machine is a bit more complicated than that and takes some calculating and a hell of a lot of ingenuity to build. But it is possible.:)
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Matsumoto_Hideki
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mad.gif posted on 5-1-2005 at 14:36
phorone will not form Phorone HCl by itself.


I think we have been over this already, as Phorone is totally insoluable in HCl and refuses to peroxidate.
Please look at rogue science thread on Holy grail organic peroxide. It seems as though you have to form Phorone
from HCl and acetone at high heat then keep reacting the remainder HCl to convert it into Phorone HCl then into finally Pentachlorophorone. Please look at the german patent.
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[*] posted on 5-1-2005 at 14:47


I don't mean to tease anyone but the thing is that I'm having my term exams right now :( and don't have the time to do any testing.
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Matsumoto_Hideki
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mad.gif posted on 5-1-2005 at 16:12
Doodman WTF?


Hey why don't you try the synthesis before you attack all of our hard work, THANX:mad:
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[*] posted on 5-1-2005 at 18:28


Quote:
Originally posted by Dodoman
I don't mean to tease anyone but the thing is that I'm having my term exams right now :( and don't have the time to do any testing.

Yeah right , likely story . Probably wasting your time with failed attempts to make phorone and HCl react to form phorone dihydrochloride in an aqueous system which parallels the reaction conditions :D

Quote:
Originally posted by Matsumoto_Hideki
phorone will not form Phorone HCl by itself.
Under these aqueous reaction conditions I don't think it will form via phorone either because it appears to be an unstable species which
wants to hydrolyze back to being just phorone or possibly something else . So trying to get phorone to form phorone dihydrochloride in this reaction system is
like sending it backwards through its reaction equilibrium to convince it to return to a more unstable form . It's like trying to make it defy gravity and float back down to the bottom layer in the beaker , and be a good little unstable emulsion of the hydrochloride , from which
unhappy home and marriage it demands to be free :D I think the only way we are getting the phorone dihydrochloride to form
in a dispersed "solution" or reactive quasistable microemulsion is that is where it is formed in a nascent state where it exists only according to a certain
half-life , a window in time and concentration where it is phorone dihydrochloride only for awhile and to a limited concentration , in an irreversable condition where it begins hydrolysis soon after formation . Can I prove that this is true ? No , but my own experiment suggests that it is true under the conditions for this particular reaction .
Under different reaction conditions you might be able to happily make phorone react with HCl to form phorone dihydrochloride any time you wish , if you have already formed the phorone by a different path . But the reaction conditions which we see in effect here place constraints upon what is logical to be occurring and what is not . If you have an explanation which seems more plausible , then hey I'm all ears , tell me about it :D

[Edited on 6-1-2005 by Rosco Bodine]
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Matsumoto_Hideki
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wink.gif posted on 5-1-2005 at 18:54
agreed rosco.


Going to make some detchord with DPPP.
hehe. Movie coming this saturday of homemade detcord sheering a tree or thick material in half. hopefully I will get some time to do this....
BTW this is 650g in the bag

100_2622.JPG - 601kB
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cool.gif posted on 6-1-2005 at 00:29


looks like a good yield. Play safe!
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[*] posted on 6-1-2005 at 02:32
DPPP Oxygen Balance?


Maybe I missed reading it, but do we have an oxygen balance worked out for DPPP yet? I'm asking to see whether mixing with MEKP would even out, or worsen its balance...

Also I seem to recall reading that mixing peroxide crystals with contact cement made them safer + into a solid shape + extruded remaining water from the crystals, is this true? and if so does anyone remember in what ratio's?

I mixed a small test tube full of my black liquid with twice that of h2o2, aprox. 3ml total at -10c and then waited a while, I seem to have gotten about 1/2g (unconfirmed, just by looking at coffee filter) of fine yellow crystals, washed with bi-carb and water, and is now drying on newspaper, I've noticed that in a matter of 6 hours, newspaper will suck almost all the water out of anying, if laid on a thick sheet of it. I'm sure lots of people know that....but it makes for drying crystals etc. quicker then just left out in the air.

[Edited on 6-1-2005 by Mickhael]
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[*] posted on 6-1-2005 at 03:35


Quote:
Originally posted by Matsumoto_Hideki
Hey why don't you try the synthesis before you attack all of our hard work, THANX:mad:


I did try the synthesis you'll find the description on page 9 of this post.

Sorry for the inconvenience I've caused you mister Hideki.
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smile.gif posted on 6-1-2005 at 03:41
OB


Quote:
Originally posted by Mickhael
Maybe I missed reading it, but do we have an oxygen balance worked out for DPPP yet? I'm asking to see whether mixing with MEKP would even out, or worsen its balance...


OB? just look at the chemical formula, if you can't get a good idea from that, then there is no hope for you:(

As Rosco has mentioned, a mix of DPPP and MEKP is deffinatly a must try.:D
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[*] posted on 6-1-2005 at 03:55


Ok, I admit I was being lazy and was hoping someone would just give me a number :P...I've got the chemical structure from the first page of the thread...so I'll jsut have to work it out from there, I never took any chemistry in school...so I'm just one step above clueless when it comes to most chemical theory...but I'm learning...slowly...lol
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[*] posted on 6-1-2005 at 05:55


I came up with a mechanism for the prepration of DPPP. The mechanism can explain the ratio of the HCl to acetone and the reason you cann't prepare DPPP from phorone. See the attachment.

Equation 1 and 3 explains the HCl ratio to the acetone and its quite clear that the black oil (resulting from equation 4) cann't be prepared from phorone.

You will need chem sketch to view it.

The equaitons could be a brain fart but I just don't buy the ones in the patent that's what made me start from the begining and try to figure a way out.

Please Rosco tell me what you think of my equations.

Attachment: noname.sk2 (16kB)
This file has been downloaded 1091 times

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[*] posted on 6-1-2005 at 08:03


Dodoman

I don't know what you have been drawing but none of your reactions is right. First of all, your drawing is NOT a mechanism and second, PLEASE go search in literature about acid catalyzed aldol reactions.

Reaction mechanisme according to me:

Aceton + HCl, without H2O2:
1. The enol tautomer of Aceton attacks the protonated form of Aceton, which yields after deprotonation Diaceton Alcohol.
2. Then the enol tautomer of Aceton attacks the protonated form of this Diaceton Alcohol yielding Triaceton Dialcohol after deprotonation.
3. The Triaceton Dialcohol is dehydrated under acidic conditions in two steps to Phorone.
4. This Phorone slowly reacts further with HCl in which HCl adds across the two double bonds forming Triaceton Dichloride (CH3)2CClCH2COCH2CCl(CH3)2.

At the moment H2O2 is introduced, things get a little complicated:
5. Unreacted Phorone reacts rapidly with HCl when radicals are present (H2O2). HCl adds in a Markovnikov-way!! (more stable, easier formed) to the two double bonds, and more Triaceton Dichloride is formed.
6. Cl- is oxydized under acidic conditions by H2O2 and Cl2 is formed.
7. The enol tautomer of Triaceton Dichloride is chlorinated by Cl2 at the alphaposition, this happens only one time under acidic conditions, and the other alphahydrogens are left unaffected. This reactionstep forms (CH3)2CClCHClCOCH2CCl(CH3)2.
8. This intermediate is then attacked by more Cl2 which abstracts a hydrogen atom from one the outer methylgroups, the radical thus formed is stabilized by the neighbouring groupeffect of the tertiary Cl-atom. More chlorine reacts with this radical and the ClCH2-group is formed. This reaction step can take place only two times, one time on both ends of the molecule, probably because of steric hindrence? Anyway, pentachlorophorone is formed ClCH2(CH3)CClCHClCOCH2CCl(CH3)CH2Cl.
9. This pentachlorophorone then undergoes SN2 substitution with more H2O2, releasing Cl- again. After this internal cyclisation follows and at the end of the reaction, two phoronemolecules are interconnected by a peroxo-ether bond (-O-O-) forming DPPP.

I hope this sort of explanation clears things up. I'm pretty sure that i am thinking in the right direction but feel free to criticise if you think you encounter an eror.

[Edited on 6-1-2005 by Swedish Chef]

[Edited on 6-1-2005 by Swedish Chef]
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[*] posted on 6-1-2005 at 09:08


Polymer chemistry is a science unto itself and it is definitely applicable to the reactions we are "guesing" occur here .

I have begun a second sealed bottle experiment to examine some other possible interpretations , variations on the Mackowiak process . Already I have something interesting to report .

To 100 ml acetone is added 125 ml HCl 31.45% and the bottle is sealed . The mixture warms immediately and in 10 minutes has a slightly yellowish color .
3 ml of H2O2 are added , and the color immediately fades , and the mixture has a cloudy white appearance . The gentle exotherm which has been occuring seems
to cease as the mixture stands for an additional 10 minutes , so the sealed bottle is placed into a hot water bath temperature 75 C . 1 hour later the mixture has an orange tea color , and
in another half hour the mixture has darkened further to the very dark concentrated red orange tint which is
almost so dark that no light can pass through the container , ~ 50 mm diameter .

This rate of color development is fully 3 times the rate observed when 3 to 2 moles stoichiometric volumes , of acetone and the same acid were mixed without the addition of the 3 ml of H2O2 . Because two variables have been introduced , with the increased amount of HCl to acetone , along with the addition of a small amount of H2O2 to the mixture after color first appeared , I am uncertain if one or both of these variables is responsible for ramping up the rate of reaction , but it is definitely a 3 times faster reaction with these changes .

[Edited on 6-1-2005 by Rosco Bodine]
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Matsumoto_Hideki
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[*] posted on 6-1-2005 at 09:39
Sounds good Rosco.


Ok, That sounds like a good description of the reaction. It seems like when the dark red- red transulcent colour is reached the solution is still
quite autocatalytic and will still produce the black opac layer we are having the sucess with in mere minutes - hrs after the heat has been turned off. just a thought..

As for the problem of excaping gases during the intintial heating how about using a thick neoprene balloon to trap any acetone and HCl vapours? .... another thought...


Well just thinking here about the colour of DPPP
everyone here seems to be getting the same results when the reaction is complete?
Colour is sulphur yellow and refuses to sublime and room temp... Now that we have pretty much fingured out DPPP what about Diphorone Hexaperoxide?
BTW. I am going to make a 60g butane cylider
shaped charge as well as a length of detcord and take pictures/movies of these in action on Saturday late afternoon.

[Edited on 6-1-2005 by Matsumoto_Hideki]
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[*] posted on 6-1-2005 at 09:40


Could the black oil that forms in the reaction partially consist of mesityl oxide? As I got a black thick oil and dark orange-red liquid when I added my H2SO4 + Acetone mixture into water after 24h in the cold (-10), The orange-red liquid leaves green stains on everything if it dries out. I could try to evaporate the liquid down and see if it yields any crystals (vacuum might be good to remove the oil too..). If I would have refluxed the mixture I should have gotten mesitylene..
Strong bases also seem to form some condensation products (diacetone alcohol) with acetone..
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[*] posted on 6-1-2005 at 09:56
That sounds like phorone!


Well sorry IPN that material is defently phorone. Phorone is a dark green/yellow crystalline material with needlelike crystals.
unfortunatly this is a dead end as you cannot produce a peroxide this way. HCl is the only way that has been sucessful as it forms a Petachloride with Phorone.

[Edited on 6-1-2005 by Matsumoto_Hideki]
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[*] posted on 6-1-2005 at 10:04


Quote:
Originally posted by Matsumoto_Hideki
HCl is the only way that has been sucessful as it forms a Petachloride with Phorone.
Has that been firmly established ? Please give details .

Update on my second sealed bottle experiment . At 4 hours from the initial mixing , the mixture has developed the oily surface sheen , so the mixture has been removed from the heating . I am not happy with the appearance of the mixture . It appears that while there was
success in increasing the reaction rate , the quality of the product does not look as good as the earlier experiment where
milder ratio of HCl to acetone and a slower
reaction rate occurred . There appears to
be some carbonization to this more rapidly reacted mixture . Even though it
is dark in color , it does not have the deep pure color in thin films like the concentrated yellow dyestuff color of the earlier experiment . It is much lower in viscosity as I had hoped , but it just doesn't appear to contain the concentrated "essence" which was the yellow dyestuff like material so evident as being present in the first experiment . The stain is not nearly so intense when a spot test is done on white paper . So the impression I have is that the changes which I implemented were "overkill" in terms of the increase in HCl , whatever may have been the added influence of the small amount of H2O2 . For lack of a better description , the mixture appears to
have been "scorched" by too rapid a reaction rate .

[Edited on 6-1-2005 by Rosco Bodine]
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[*] posted on 6-1-2005 at 11:08
Well I think so..


I was look around for phorone and found production data for the manufacture of it. On an industrial website I found they were using concerated sulphuric acid 98% and Acetone to produce pure Phorone. I will have to go serach again to find it.. However I couldn't find anything on Pentachlorophorone...
The yellow material that IPN reffers to is called xylite oil (Xylitone) and is a byproduct of pure phorone production.

[Edited on 6-1-2005 by Matsumoto_Hideki]

[Edited on 6-1-2005 by Matsumoto_Hideki]
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