Sciencemadness Discussion Board

Diphoronepentaperoxide (DPPP)

 Pages:  1    3  ..  10

Hoffmann-LaRoche - 15-9-2002 at 02:29

Did anyone hear of this compound?
It´s mentioned in german patent DE1951660, and is an organic peroxide that is said to be as brisant as HMX(Vdet=9000m/s) and is surprisingly made of the same things as AP: HCl, H2O2 and Acetone.
First i thought it was a fake, but then i found out the patent really exists...


kingspaz - 15-9-2002 at 03:44

or the patent is a fake...


vulture - 15-9-2002 at 04:01

I have found the patent on the german patent server. Here is a structure I made.
The only problem is that i'd expect the double bonded C's to accept a peroxide bond, but then they can't be double bonded anymore and the other C has to accept a H.

DPPP.jpg - 266kB

I'm wrong!

vulture - 15-9-2002 at 04:16

I made some severe failures in that molecule...please ignore it..I'm working on a new one

Got it

vulture - 15-9-2002 at 04:41

Finally figured out the correct structure.
The left one is the one according to the patent I found. But I feel it must be more like the left one, because I don't see any explanation why the other 2 methyl groups wouldn't form a peroxide bond also... HELP! Philou!;)


vulture - 15-9-2002 at 04:42

Somehow the picture didn't come along....
Sorry for clogging the thread up...

DPPP2.jpg - 30kB

Hoffmann-LaRoche - 15-9-2002 at 06:45

You did a nice job with the jpg....i think i will print that interesting molecule out in poster-size....

Im wondering how this molecule can have such a high brisance while having an extremely bad oxygen-balance, although the molecule is a big one, and this may often contributes to high crystal densities, therefor high detonation velocities...

The bad oxygen balance becomes obvious if considering following decomposition equation:

C18H26O2(O2)5 > 12CO + 6C + 13H2

(additional 18,5 moles O2 required for zero oxygen balance)

Im not familiar with the methods of measuring detonation velocities, but so far, DPPP is by far the most interesting energetic material ive heard of, so i propose to make another brisance test:

If acetone peroxide detonates at around 5000 m/s, and DPPP at 9000M/s, then there has to be a significant difference in the size of shattered particels of the surrounding material.
For example, if one sticks a blasting device with a high detonation velocity in some kind of soil, the shattered parts of the soil have to be much smaller, than using one with much lower Vdet.

So it would be very interesting to compare AP and DPPP to see, wether the 9000m/s could be true....
Patents never lie, especially the european ones(american patent office also patents perpetua mobile), but i find it not very promising, that the patent also says the explosion temperature is 200°C, rather than being 2000°C(maybe a printing error), so im at least careful with this information....


P.S: C`m on!-Give this thread the start it deserves....

Nick F - 15-9-2002 at 07:25

200*C could be the temperature at which it explodes, and not the temperature of the explosion...

vulture - 15-9-2002 at 07:36

HLR, formation of H20 is favourable over that of CO.

Hoffmann-LaRoche - 15-9-2002 at 08:05

vulture)H2O is NOT favoured over CO, the equation has to be right.
Check this:

H2O is at least favoured over CO2...


Nick F)Oops, were is my mind these days!! - You are right.:P

Hoffmann-LaRoche - 15-9-2002 at 08:08

Damn.......thats not my day.
Heres the right link:

vulture - 15-9-2002 at 10:12

I'm sorry, but that is bogus. If it's right what is being stated there, then TNT would not produce carbon upon detonation. It produces carbon because firstly the hydrogen is burned to H2O and no more sufficient oxygen is present to oxidize the carbon.

Also, another flaw in there. Metal additions to an explosive get burned as last, simply because they are not part of the molecule.

Double-damn!!(if you´re right)

Hoffmann-LaRoche - 15-9-2002 at 11:58

well i thought it was a serious site...

do you know a better scientific source?

Gnnnnn, HLR

P.S. has anyone yet synthesized DPPP to compare with AP??-im burning of interest...and i dont have time this week to do it myself.

C6H5N3O6 > CO + C + 5/2H2 + 3/2N2

Hoffmann-LaRoche - 15-9-2002 at 12:39

Carbon is left after decomposition in any case.
So could u please proof what u said, im a little bit confused now..


P.S. Did u really check that site? - It seems to be a navy-site, and it doesnt look like a "bogus"-site at all.

ähh, C7H5N3O6>6CO + C + 5/2H2 + 3/2N2

Hoffmann-LaRoche - 15-9-2002 at 12:43

sorry, but i did some severe bad-concentration-errors in the last equation.....please ignore them.
This one is right.



Polverone - 15-9-2002 at 12:45

This compound does strike me as very interesting. Is anyone here fluent in German? The only parts of the patent that I can understand are the chemical formulas. If somebody will make a nice translation/summary of this patent I will gladly credit you and add this document to the library!

Hoffmann-LaRoche - 15-9-2002 at 12:49

I could translate the most important parts of the patent.
Watch out for the next post.


kingspaz - 15-9-2002 at 13:15

vulture, nice drawing. i would guess it to be quite stable in relation to AP since it doesn't have a cyclic nature, similar to HMTD.
also i have consulted chemistry of explosives and it says in severly oxygen deficient explosives then hydrogen is oxidised first. i would guess this to be due to entropy as one mole of O2 can produce 2 moles of H2O as oposed to 1 mole of CO2 (greater product disorder) thus over ruling C's greater reactivity. but like i siad thats a guess. i can't even remember if C is more reactive.

Here it is!

Hoffmann-LaRoche - 15-9-2002 at 13:23

German patent DE 1951660.


Diphoronpentaperoxid C18H26O2(O2)5

field of invention: the invention refers to an explosive which has special properties that make it suitable especially for mining and as well for military purposes.

Task: The invention wants to make blasting operations cheaper and easier.

Solution: Following cheap substances are required for synthesis:

1part conc. hydrochloric acid(HCl)
1part acetone (CH3COCH3)
2parts 30% hydrogen peroxide(H2O2)

Process of manufacture:

1part of acetone are added to 1part hydrochloric acid, through which acetone polymerizes to phoron; then 2parts of hydrogen peroxide are added, through which two molecules of HCl bond with the two C-double-bonds of the phoron.
In the course of the reaction free chlorine
develops, which bonds with 3 hydrogen atoms of the phoron to give 3 HCl(see drawing) and bonds itself with phoron.
Hydrogen peroxide causes the chlorine atoms to split off the phoron and the peroxide itself bonds with the phoron.
Because of the fact, that one peroxy-bond stays half-opened, one also open phoronperoxide adds to give diphoronpentaperoxide, which precipitates from the solution in crystalline form.

Properties: a)insoluble in water
b)still explosive when heavily contaminated
c)detonation velocity approx. 9000m/s
d)low detonation temperature approx. 200°C
e)does not develop smoke upon detonation, does not smell, no solid residues.
f)ignition by fire, blasting cap or electric
g)does not decompose at long storage
h)yield of manufacturing process approx. 90%

with best regards, HLR

Added to library

Polverone - 15-9-2002 at 16:17

The patent translation that you supplied has now been added to the sciencemadness library. When there is more information available about this substance, I will add it to the existing document.

The patent is not very specific about reaction conditions or times. I have just added one volume of HCl (approx. 31%, not concentrated) to one of acetone. The mixture became cloudy and the flask warmed up a little. I am going to warm this on a hotplate for a while to see if there is any further sort of reaction visible, then chill it in the freezer to see if any phorone crystallizes out (m.p. 27 C according to Then we will see if I will move to the next stage or not...

One thing that just came to mind: when I was young and foolish, I experimented with acetone peroxide, not really knowing what it was, and so did many of my friends. One of these friends once claimed that he had made a batch of acetone peroxide using a huge amount of HCl. He claimed that the mixture grew hot enough to boil, and that when it had calmed down he was left with crystals large enough to be easily visible to the naked eye, and that they had a slight yellowish cast. He also claimed that, unlike other batches of acetone peroxide, this one would explode, unconfined, even in the smallest amounts.

So, did he merely have a unique physical modification of acetone peroxide? Did he perhaps form some of this DPPP as well? Or did he make the whole thing up to amuse me...

madscientist - 15-9-2002 at 16:28

Here's everything I know about phorone (all information from my chemical dictionary).

Formula: (CH3)2CHCOCHC(CH3)2
Density: 0.8791g/cm3 at 20C
Boiling point (760mm Hg): 197.9C
Freezing point: 28.0C
Vapor pressure: 0.38mm Hg at 20C
Properties: Yellow liquid or yellowish green prisms.

madscientist - 15-9-2002 at 16:34

I just consulted several other references. It seems that the melting point of phorone really is 28C. Phorone is very weakly soluble in water (0.1g dissolves in 100mL of water at 50C). It is soluble in ether and alcohol.

That's excellent news!

Polverone - 15-9-2002 at 17:03

About it being yellowish liquid, that is. Because my HCl/acetone mixture on the hotplate has started to turn a golden yellow.

I didn't realize this until I searched today, but DPPP has recently been discussed a tiny amount on the E&W Forum.

Here's what Microtek had to say:


Allright, I'm afraid I got quite un-scientifically impatient to find out more about the diphoronepentaperoxide, hereafter referred to DPPP, so after slowly and carefully reading through the pages, I searched the german patent database and found that the .gifs were copies of those pages. I then made a synthesis as outlined in the patent: 5 mL acetone was mixed with 5 mL part HCl 30%, heat was evolved and very slight bubbling was observed ( I know that it is most likely parts by weight, but as I said I was impatient ).

Once the liquid had cooled, 0.5 mL was transferred to a test tube and 0.5 mL H2O2 40% was added. At first drop by drop, then as nothing untowards was happening, I added the rest.
A white precipitate immediately appeared and the mix was allowed to sit undisturbed for 10 min. After this period the product was filtered off, washed and dried.

Then I started examining the it and found that it smelled exactly like acetone peroxide, but was a fine amorphous powder like HMTD. Upon ignition from flame it flashed like HMTD or AP, but if placed on a piece of Al foil above a flame, the powder melted and then detonated violently. Thus far, everything except morphology pointed at AP, but then I did the impact sensitivity tests. I performed my standard qualitative test which consists of placing the sample in a piece of Al foil which has been folded to form a small envelope. This envelope is then placed on a steel anvil and a carpenters hammer is used to pound the sample. It was quite hard to get the sample to detonate; it took blows consistent with what PETN requires, and when the flat, un-exploded samples still in their envelopes were held into a flame they didn't detonate but only flashed as before.

The final test I did was to pack about .25 gram into a 2 mm pipe attach a fuse, and ignite - no detonation, only flashing which ejected the rest of the fuse. Further testing will follow.

Note that he said that the product he obtained smelled and behaved like acetone peroxide. If it looks like a duck and quacks like a duck...

I am also doubtful that he obtained DPPP since phorone does not rapidly form at room temperature (as my current experiment shows). His unusually impact-insensitive acetone peroxide may actually not be that amazing, since he said that he obtained it as a very fine powder, which is different from the standard physical form as obtained with lower amounts of acid.

Mmmm, today is a great day for mad science.

Density measurement

Hoffmann-LaRoche - 16-9-2002 at 02:18

most likely, the compound has to have a higher density than AP, as it has such a high detonation velocity, and the molecule is simply much bigger!

So: make again a small batch(are the given mixing proportions by weight, or less likely, by volume:mad:?).

It would be best if somebody took the time to make the stoicheometry check using the reaction equations in the patent therefor.

Then, place some of the -supposed to be- DPPP-crystals in a measuring flask-let´s say a 10ml measuring flask, and exactly 5.0 gram of the DPPP, so that we can recalculate the density of the DPPP, when the flask is then later filled up with water from a pipet or a buret.
Dont forget stirring.

density(DPPP)=5,0g/(10mL- ml added water from buret) [g/mL] or [g/cc]


vulture - 16-9-2002 at 06:12

Here's the correct structure.
If you look at this you'll see that first the HCl serves as a catalyst to "rearrange acetone to phorone. Then hydrogen peroxide frees chlorine from the HCl which oxidizes the phorone to phoronedihydrogenchloride. After that more HCl converts it to pentachlorphorone which gets oxidized by the oxygen (EN O > EN Cl) and forms the peroxide bonds where the chlorine was previously bonded.
According to me the hydrogen of the H2O2 will then form HCl with the residual chlorine.

So one could detect succesful reaction by carefully monitoring, because after the phorone will be peroxydized, the pH should drop because of HCl formation.

DPPP final.gif - 3kB

Hoffmann-LaRoche - 16-9-2002 at 06:21

damn.....youre pretty right.....why didnt we come to this earlier!-And again, a nice job on the pictures....what program are u using?


vulture - 16-9-2002 at 06:56

I use ISIS Draw, a program I downloaded for free and it's very simple to work with.

Further info

Polverone - 16-9-2002 at 10:36

This patent seems pretty vague on details. It could be a deliberate omission, so that anybody who wants to replicate the work has to guess at the exact procedures but anyone who infringes the patent can still be prosecuted.

Anyway, the adventure continues:

I found info on the web that indicated that acetone will yield phorone, mesityl oxide, and mesitylene under the influence of strongly acidic or basic conditions. Organic Syntheses online indicated that mesitylene is formed in appreciable quantities only with dehydrating agents (such as conc. H2SO4). Another reference indicated that mesityl oxide would be formed by the action of hydrochloric acid on acetone, but only in small amounts.

I, hoping that my mixture would settle down at some nice equilibrium point, applied moderate heat to the HCl/acetone mixture for a couple of hours. But it passed beyond yellow to yellow-orange and then to orange, and I decided I should finally withdraw the heat.

When the orange liquid was placed in the freezer, nothing crystallized out. A small amount of the cold liquid was mixed with twice its volume of (somewhat concentrated) H2O2. Over the course of an hour there was a small amount of bubbling in the mix and some sort of platelike solid formed in small amounts on the surface of the liquid. The reacting liquid had a somewhat unpleasant solvent-like smell, but it did not smell like HCl, Cl2, or acetone peroxide.

This morning, the small amount of solid that formed had disappeared. I am wondering if I heated my HCl/acetone mix too long and converted the phorone to something else.

I may try making another phorone batch, this time chilling the flask as soon as the liquid starts to get an orange tinge.

Hoffmann-LaRoche - 16-9-2002 at 12:42

I agree with you about the vague patent description of the process.
I came across lots of patents obviously written as vague as possible...

Did you add a small amount of H2O2 in the first reaction?-The patent-drawing of the reaction shows the note of H2O2 being necessary as catalyst.

Maybe it would be better, if only moderate heat (40-50°C)was applied in the first reaction as secondary oxidation reactions possibly get more important....but i`m no expert though.


Hoffmann-LaRoche - 16-9-2002 at 12:55

sorry....forget what i said in the last was just talking out of my stomache.:P

The first reaction?

Polverone - 16-9-2002 at 13:01

The one where phorone is formed? I didn't see that mentioned but didn't look at the patent too closely once I saw that it was all in German. I would be wary of adding H2O2 at that stage because I would expect it to form acetone peroxide, and I don't care to heat a flask containing acetone peroxide (even in solution). But if it's a truly small amount that is required, I might try it. Does the patent specify how much H2O2 to add in the phorone-creation stage, or is it vague there too?

BrAiNFeVeR - 16-9-2002 at 13:29

Well, todayI also took a throw at DPPP.
At the same time, I prepare some regular AP using 20 ml acetone, 12 ml H2O2 (35%) and 8 ml HCl (10%).

I'm not gonna describe the preparation of AP, since that's a dead giveaway ...

To 25 ml acetone, I added 25 ml of 35% HCl (a slightly exothermic reaction occurs), and then I slowly heated this until bubbles reached the surface.
By this time, the solution was nice and yellow ...

I cooled it, in the hope that crystals would ppt out, but no such luck :(

I then took 5 ml of this supposedly phorone solution, placed it in a test tube, and added some snow from the freezer, hoping, that due to it's pretty bad solubility in H2O , I would get crystals.
Again, no luck :(

I took another 5 ml of this yellow solution (evolving HCl vapors btw) and to it, added an equal volume of 35% H2O2. instantly, white crystals started to form, and the test tube heated up a little bit too.
This was left for 2 hours, after wich 90 % of the solution was packed with a very fine crystaline product.
These fine crystals where filtrated, neutralised and dried.
The smell is allmost exactly the same as the (at this time) still crystalising AP.

When hit by a hammer (not very hard) it detonates with the release of the very unpleasant smell of detonated AP.
Which was especially unpeasant in this case, because it indicates that what I have, is mostly regular acetone peroxide, since DPPP would have different detonation products, right ?

So now all my hope lies in getting the phoron out of that solution in a crystaline form, wash it, and peroxidise that ...

Maybe I'll try to dehydrate 5 ml in a dessicator tomorrow in case heat would destroy phorone in some way.

Hoffmann-LaRoche - 16-9-2002 at 15:21

Here are the stoichiometric mixing proportions, which i calculated using the molar amounts in the reaction equations, which are surprisingly much different from the proportions given by the patent:


21,75mL 2-propan-on (D=0,8)+ 70,88mL 30% hydrochloric acid(D=1,2)

which is kept at 50°C for some hours, until the solution turns yellow
(referring to polverone).


68,74mL 30% hydrogen peroxide(D=1,3)
are added to the above mixture and left at room temperature, or i suppose, better on an ice bath for 24-48 hours.

slowly precipitate forms.
dilution with cold water may precipitate some additional DPPP.

Compared to the patent, a mixing ratio of approx. 1:3:3 (acetone:conc. HCl:30%H2O2) results, while the patent says 1:1:2(if the ratios are by volume)


Hoffmann-LaRoche - 16-9-2002 at 15:29

Try adding EtOH or MeOH, as it could well be possible, that phorone is not soluble in alcohol or methanol.
Maybe the phorone/phoronepentachloride precipitates.
Id say it`s worth a try.


madscientist - 16-9-2002 at 15:55

Phorone dissolves in alcohol. It's essentially insoluble in water.

Hoffmann-LaRoche - 17-9-2002 at 02:24

Doesnt anyone have access to beilstein?
- There HAS to be a procedure for it.
Philou, our hero......what´s up?

Furthermore, no one tried to make the peroxidation-step with proper cooling.
I suggest this would give bigger crystals and better yields.
If the crystals are then still that much smaller than AP-crystals, this would be a clear indication that DPPP, and not AP is the major product of the reaction.
The detonated peroxide smells a lot like AP?-Well, why not?-To me it is very likely that AP could be a by-product in the reaction.
Can`t wait for the next weekend, when i can start some similar batches myself.:)


Hoffmann-LaRoche - 17-9-2002 at 05:48

Summary of differences to AP:

1)Phorone-intermediate is yellow and water insoluble, soluble in EtOH, and very likely also in acetone and Et2O

2)Crystals are supposed to be smaller than AP-crystals

3)Purified DPPP is said not to smell

4)It has a giga-brisance for an organic peroxide(only if compressed to near crystal density, for sure)

5)It has a density much much higher than AP (0,8g/cc, if i´m right), this could be measered easily, as i proposed in one of my posts..

6)The peroxidation of the pentachlorphorone yields 10mol HCl per mol DPPP, so the pH will drop SIGNIFICANTLY.
Notice: if u dont start from purified pentachlorphorone, it will be very difficult to see the pH dropping any further when using ordinary pH-indicator, as your solution is already strong acidic.

7) DPPP is very storage stable, and i suppose, because of its high molecular weight, it is not sublimizing like AP.

That´s all so far.


rikkitikkitavi - 17-9-2002 at 09:38

my chemical dictionary states that phorone is formed when acetone saturated with HCl is left standing.

This could mean that it will not work with
HCl in aqeous solution. Maybe the reaction time needs to be extended to...


Hoffmann-LaRoche - 17-9-2002 at 10:11

That´s interesting...this would complicate the process a bit....but no problem so far!
I´ll try that as soon as possible.
A good prep.-method for dry HCl-gas is heating H2SO4 + HCl.
And maybe then, with emphasizis on anhydrous reactants, the acetone could be thouroughly dried by adding by adding small amounts of anhydrous K2CO3 or CaCl2 (ref. CD-Roempp chemistry lex., Thieme 1995).

But the best would still be if somebody could download the procedure(s) from the Beilstein database...


Hoffmann-LaRoche - 17-9-2002 at 10:16

äh.....sorry for the messy equation.....ya know what i mean

madscientist - 18-9-2002 at 18:25

About two-thirds of the way through this thread there is an attempt to synthesize acetone peroxide that is of interest to this discussion.

Hoffmann-LaRoche - 19-9-2002 at 03:20

The post you selected no longer exists. It may have been recently deleted.

Please hit BACK on your browser, then hit REFRESH/RELOAD to get an updated view.

vulture - 19-9-2002 at 10:31

Better keep the kewls ignorant of what they might be making....

DPPP research.....another attempt

Hoffmann-LaRoche - 23-9-2002 at 09:30

Finally, i had some time for experiments.....

1) tried making phorone:

A)50mL of 30% HCl + 50mL acetone, (flask was warming up a bit).
Then heating of the mixture for more than 12 hours: the colour went from yellow to orange and finally it went black(maybe decomposition occured, and carbon was the result..).

B)Then i tried the same again, but this time, i covered the flask with another glass container, so that fewer acetone and other reaction products could volatilize.
After some hours, the outside temperature being quite low, i noticed some crystals on the inside of the covering glass container, which must have sublimized out of the acetone/HCl solution.
Probably phorone?...or just traces of AP which were left in the glass from previous experiments....Has anyone tried to make phorone, and experienced the same??
As phorone seems to be very volatilizable and also seems to be easily devastated to leave only carbon, maybe there is a possibility to recover phorone on a cold surface above the flask...

C)tried the one with dissolving dry HCl gas in acetone.
Well, i made a saturated solution of HCl gas in acetone and i have let stood the flask at 15°C since 3 days.
And again, the colour turned slightly yellow, then golden yellow, and at this moment, it has an orange colour.
Let´s wait ....

2)Tried to make DPPP without isolating phorone first:

mixed 25mL of 30% HCl with 25mL acetone and immediately, an exothermic reaction ocurred.
After the mixture had chilled down, i added 50mL 30% H2O2 and put it into the refrigerator at 5°C.

After a couple of hours, i noticed that the bottom of the flask was covered by a 3mm layer of small crystals.

Then i washed the crystals, which had the same size of AP crystals, with water and dropped a little quantity of them into a lead nitrate solution, which had a measured density of 1,3g/mL,..........the crystals did not sink.

Thus the obtained substance had to have a density between 1,0(sunk in water) and 1,3g/mL.
I dont believe, that a substance with such a low density could have a Vdet of near 9000m/s, so i dont think DPPP was the product.

Furthermore, a yield of 90% was mentioned for the DPPP process, which certainly wasnt the case as raw quantities of reactants were introduced, and only a small layer of crystals could be recovered.

This made me think a lot....if the inventor mentions an overall-yield of 90%, it is very likely that the process is really a simple one, and last but not least, he also mentioned that it is the purpose of the patent, to make blasting operations cheaper; not a single word about distillation operations, none about heating/cooling!

It´s simply a fact that we know too little about phorone and DPPP.


japanese patent

Hoffmann-LaRoche - 23-9-2002 at 10:47

This is a japanese patent, found by rc from the E&W-forum:

PURPOSE:To obtain phorone in high yield by subjecting acetone to aldol condensation in the presence of an alkali catalyst to give mesityl oxide, dehydrating a residual oil an acetone trimer in an acid catalyst such as phosphoric acid base under heating and distilling.
CONSTITUTION:Acetone is subjected to aldol condensation in the presence of an alkali catalyst, mesityl oxide is distilled and separated, a residual oil containing acetone trimer is dehydrated in the presence of 1-10wt.% acid catalyst (preferably phosphoric acid base) under reduced pressure at 50-130 deg.C, preferably 90-120 deg.C so that other acetone trimers are converted into phorone and distilled to give phorone shown by the formula. A reactor is equipped with Dean Stark separator or oil-water separator and formed water is taken out from the reaction system so that equilibrium relationship is transferred to a formation system to give phorone. The acetone trimers are economically not abandoned. Phorone is useful as a raw material for agricultural chemicals, coating compound for ship bottom, antistatic agent, polyamide resin, etc."

The main reaction is 3 C3H6O--->C9H14O+ 2 H2O

Maybe there are other patents too.


Phorone fun

Polverone - 23-9-2002 at 11:49

I've made a couple of other attempts to prepare phorone. Once I added aqueous HCl to acetone and heated as before but only let it react to form a light yellow solution. This material didn't seem to yield anything but ordinary acetone peroxide when combined with H2O2.

Then I did another batch with aqueous acid that I heated until I got a very dark solution. I poured the dark solution into sodium carbonate solution and it lightened considerably. The bulk of the solution went to a pale yellow, and there was some oily substance that floated on the surface of the water without mixing. On prolonged standing some fluffy yellow solid appeared as well.

I meant to try saturating acetone with anhydrous HCl this weekend but I got distracted by other things. It sounds like it gives a similar product in any case. I may try the first part of this Japanese patent, but I don't have vacuum distillation equipment so I can't try all of it.

Phorone fun

Polverone - 23-9-2002 at 11:51

I've made a couple of other attempts to prepare phorone. Once I added aqueous HCl to acetone and heated as before but only let it react to form a light yellow solution. This material didn't seem to yield anything but ordinary acetone peroxide when combined with H2O2.

Then I did another batch with aqueous acid that I heated until I got a very dark solution. I poured the dark solution into sodium carbonate solution and it lightened considerably. The bulk of the solution went to a pale yellow, and there was some oily substance that floated on the surface of the water without mixing. On prolonged standing some fluffy yellow solid appeared as well.

I meant to try saturating acetone with anhydrous HCl this weekend but I got distracted by other things. It sounds like it gives a similar product in any case. I may try the first part of this Japanese patent, but I don't have vacuum distillation equipment so I can't try all of it.

BLAST_X - 23-9-2002 at 13:10

I've tested preparation of DPPP and i can say it`s a very interesting and varied explosive.
You can use it as a primary explosive and as a high energetic secondary explosive.
You can never classify DPPP in the same category as AP or HMTD.
The question is, at which density you use DPPP and at which method you use to ignite DPPP.

To a 1000 ml erlenmeyer flask add 185 ml of 20% HCl (i don`t
have 35% HCl at this time). To a second flask add 100 ml of aceton.
To an third flask add 200 ml of 30% H2O2. Cool all to 5 C.
After cooling, slowly add the aceton to the HCl and stir the mixture
for 5 minutes.(very slight yellow colouring over a few minutes)
The patent don`t say heat at this time and the patent don`t say
some product (poron) should precipitate from the solution at this time.
If you heat or not, the content of AP are always present at end of the synthesis. On the contrary, if you heat to much or to long, the reaction fails.
Cool the mixture to 5 C for 2 hours and stir occasionally.
After standing, set the mixture to magnetic stirring at room
temperature and slowly (over 10 minutes) add the H2O2 to the
aceton/HCl mixture. The temperature can rise over 40 C and
the mixture become a sligth green colouring.
(second reaction-step, formation of pentachlorporon and free
Cl with H2O2 as catalyst)
The DPPP should precipitate on top of the mixture and some fumes bubble of.
You can distinguish this of AP crystalls, which formes in the reaction-mixture and which are a bit larger than crystals of DPPP.
I`ve look at the crystals exactly through a microscope.
(look at attachment DPPP.jpg)

After all H2O2 is adding, continue stirring for 2 hours an more till the liquid on the bottom of the flask are clear and no fumes bubble of.
Filter out the crystals, wash them with 1 L of 10 % sodium bicarbonate solution, and again with water.
Dry crystals of DPPP at room temperature for 48 hours.
The next step are very important to remove all traces of acid and AP in the product, that you can handle safe with DPPP.
Dissolving the crystals in minimum amount of hot ethyl alcohol (60 C),
let cool to 5 C, filter, add a large volume of cold distilled water, let sit for 1-2 hours below 10 C and filter again.
Let dry DPPP at room temperature for 1-2 weeks to decompose and evaporate the rest of AP on the air.
final yield: 65 g
(at this reaction temperature and with delute 20% HCl, i think you can get much more yield with reaction temperatures below 10 C and a longer reaction time, the patent say around 90%)

Be careful with large quantities because DPPP is somewhat sensitive
to friction, shock and heat.

I`ve tested the DPPP in 3 different charges.

1. I`ve made a blasting-cup (hard-paper) with 5 g charge low pressed
DPPP and ignite with a match.
No detonation, only flash, the blasting-cup bursts only.
Consequently, if you ignite DPPP at powdered density or with flame,
it`s flashes only, you can use it as a primary explosive similar
to AP and HMTD, it detonates only at this density when strongly heated.
(very storage stable and lower sensitive to friction and shock)
2. I`ve made a stable blasting cup (hard-paper) with 50 g charge high
pressed DPPP and ignite with a match.
It datonates hazardous and i`d feel strong the detonation pressure
still the distance of over 50 m between the blasting-cup and me.
3. I`ve made a stable blasting cup (hard-paper) with 10 g charge high
pressed DPPP and ignite with a match.
It datonates correctly as well.
Consequently, in high pressed density or under pressure in a
stable blasting-cub - DPPP is a high qualtity and high energetic
explosive, it detonates without a primary igniter.

- somewhat sensitive to friction and shock
- low detonation temperature, ~ 200 C
- density of DPPP are not very high

- required chemicals for synthesis are cheap
- it`s easy to produce (no expensive lab-equipment required)
- large volume of gas and high explosive velocity, ~ 9000 m/s
(conditioned military usage, cut of steel ...)
- storage stable and great chemical stability

DPPP is my new favourite peroxide. It`s safer to handle as AP or HMTD and more powerful and brisant.
It`s a very good primary explosive to ignite very insensitive explosives (hexogen,octogen,TNT,HNIW) or a energetic single explosive.

DPPP.jpg - 4kB

Success with phorone preparation!

madscientist - 23-9-2002 at 20:05

I mixed 35mL of 31% HCl with 25mL of CH3COCH3, and held the temperature at 0C for two hours. Since nothing obvious was happening, I heated it up to 17C for an hour. Still, no signs of reaction. I heated it to 50C for another hour. It's now a beautiful, urine-yellow, and crystals are precipitating! Not in large amounts - they form at the surface of the liquid, sink back into the liquid, re-dissolving. More news surely to come!

madscientist - 23-9-2002 at 20:17

I added 50mL of 27.5% H2O2, after letting the phorone solution cool to 25C. The temperature jumped to 40C, and the solution turned clear - for a moment. It soon turned milky, and within a minute, there was a visible quantity of a white precipitate collecting on the surface of the solution. I probably should mention this - I covered my reaction beaker in which I prepared the phorone with aluminum foil, which was covered with a white solid that had a solvent-like odor, but did not smell like anything I have ever handled before.

DBSP - 24-9-2002 at 07:43

I have some questions about DPPP, what solvents is it suluble in? Can it be used in metal caps etc.

I'll probably try to synthesise it this weekend if I have eneugh time using 30% HCl, 40% H2O2, pure acetone.

Does more concentrated chems increase the yield in this process or does it lower it because of the larger ammounts of heat generated ?

BLAST_X - 24-9-2002 at 14:41

I`cant say the correct density of DPPP
(it exist nowhere information about this compound)
and i don`t have equipment to measure it exactly.
When you calculate, H2O density = 1,0, and DPPP are very light crystals,
[big molecules and high molecular mass, C18H26O2(O2)5],
which going on the surface of the water (AP = density ~ 1,18 [> 1,0] sinking to the bottom),
density of DPPP is < 1,0.
I think density is 0,6 –0,8 g/ml ?
This low density are opposing to the high explosive velocity of DPPP (~9000 m/s)
and similar explosives with vod`s > 8000 m/s (octogen, d ~ 1,9 g/ml).
The most of high explosives with vod`s
> 8000 m/s have a density > 1,6 g/ml.
A another example for low density is tetracene (2,3-naphthacene, 2H8N10O):
d ~ 0,45 g/ml and vod > 4500 m/s.

You can say rough, higher density = higher vod.
(oxygen balance are important also !)
for instance: (vod`s at this density)
octogen, C4H8N8O8:
d ~ 1,9; vod ~ 9100 m/s
tetranitroglycoluril, C4H2N8O10:
d ~ 1,98; vod ~ 9200 m/s
dinitroazofuroksan, C4N8O8:
d ~ 2,0; vod ~ 10k/s

I`ve tested pressed DPPP in a blasting cup without a primary igniter.
A warning before !
When you test a explosive don`t use any metal pipes, cups or matches, with new or unknown substances - under no circumstances !!!
The explosive can form ultra instable isomers and substances with the metal
and the air, which can explode only with the presence of sun-light or with a
touch !!! (look at picric acid or HMTD)
I make safe blasting cups and matches with paper and plastic only, when i test a explosive.
I`ve pressed a charge of 50 g DPPP in a 5 mm hard-paper cup (90x70 mm) careful to high density with a big glas-rod.
To set off the charge, i`ve put a match inside the cap.
A little paper-pipe (3x3x50mm), filled with a fine powdered mixture of KMnO4 + S
in a ratio 1:1.
(look at attachment)
The better way to set off DPPP is certainly electrical, with high temperature without the presence of O2.

DPPP_50g_test_70x90.jpg - 7kB


Physics - 25-9-2002 at 06:45

The sirs, you tried to bleed phorone in the pure state? That if to pour out an intermixture acetone / HCl in a great many of water. (Phorone in water we shall not dissolve)
P.S. Excuse me for mine English.

BLAST_X - 25-9-2002 at 08:02

Fact is, the aceton reacting with H2O
(if you have 20% or 35% HCl, H2O is always present, which are required for the synthesis)
and HCl as a catalyst to a soluble form of Phoron, which don`t precipitate from the solution !
(look at attachment)
I think, when you moderate the reaction in this direction and the Phoron precipitate from the solution,
the synthesis of DPPP fails.

phoron-H2O.jpg - 7kB


Physics - 25-9-2002 at 08:53

I hoped already at the first stage (deriving of phoron) to eliminate any opportunity of synthesis AP. Therefore I want to receive pure phorone (without an impurity of acetone). Certainly after that I again to phoron shall add HCl.

BLAST_X - 26-9-2002 at 05:28

The presence of AP or a other dangerous explosives or peroxide in form of any impureness in the main-product are
a bad thing always.
I think, when everybody make a explosive, it`s dangerous always, but nobody should ignore all the warnings and all the descriptions of them !
When you make AP or a other sensitive peroxide especially.
Everybody see the simple procedures and the high yields of peroxide-synthesis, but the dangerous side are ignored.
Look at the web, how many sites describe the production of more dangerous substances,
for instance:
glycerol tri/tetra-nitrate , AP or picrates
in large amounts.
It`s irresponsible !

Can you conceivably isolate DPPP with adding pure Phoron to a mixture of HCl/H2O2 ?
It`s a expensive way certainly.
I think the better way are, find out a correct possibility to purificate DPPP and destroy all traces of AP correctly.

BLAST_X - 26-9-2002 at 11:24

Try out it, Physics.
You can buy some Phoron
at Sigma-Aldrich,

2,6-dimethyl-2,5-heptadien-4-one, Diisopropylidenaceton
138,2 g/mol
mp = 28,1 C
bp = 198 C
d = 0,9
CAS Number: 504-20-1
Merck Index: 12,7488

Ramiel - 27-9-2002 at 23:16

If you isolate the phorone crystals and remove any trace of organic impurities then it should yeild relitively pure DPPP. So i don't quite see what your problem is.


vulture - 28-9-2002 at 04:35

From Beilstein:

TITLE Catalytic Cyclocondensation of acetone to isophorone

AUTHORS Ramanamurty, K. V.; Salvapati, G. S.

SOURCE Indian J.Chem.Sect.B 1999, 38: 1 24 - 28




CNR 6208963
ABSTRACT Cyclocondensation of acetone involves aldol condensation leading initially to the primary condensation products (PCP), diacetone alcohol and mesityl oxide, which again react with acetone to form phorone, isophorone, mesitylene, etc. Relative selectivities of chromia, γ-alumina, magnesia and calcium oxide catalysts have been studied in a flow reactor at 360-520°C. Alumina and magnesia are found to favour isophorone formation at 360°C with 45 % selectivity but the selectivity steeply falls with the increase in temperature to 520°C due to rise in decomposition products. Primary condensation products are formed more with magnesia; selectivity to mesitylene is more with CaO (ca. 66 % at 400-480°C) and Cr2O3 (50-55 % at 480-520°C).

COPYRIGHT Copyright © 1988-2001, Beilstein Institut für Literatur der Organischen Chemie licenced to Beilstein Chemiedaten und Software GmbH and Beilstein Informationssysteme GmbH. All rights reserved

BLAST_X - 28-9-2002 at 06:34

I don`t have any problem with this.
The question are, be worth the high expenditure, first makeing pure Phoron and at next DPPP, when you use DPPP as a explosive ?
It`s a big rubbish, adding aceton to HCl
to isolate pure Phoron.
The yield are definitely very low.
The major product is this polymerized Phoron
and minor product the solid Phoron.
I`ve read a desciption in a other forum,
to isolate Phoron with high yield in a aldol condensation process in presence of a alkali catalyst and under reduced pressure.

for instance:

I dont`t know, it`s a realistic possibility
with a home-lab equipment ?
Everybody should decide the method by itself.

Seperating AP from DPPP

Hoffmann-LaRoche - 3-10-2002 at 13:53

I remind it being mentioned that phorone dissolves in alcohol; to me it´s very likely that DPPP also dissolves in alcohol, just very similar to other substances and its derivates.
If it does, there would be the possibility to seperate DPPP from AP, which i hope, is not or only badly soluble in alcohol.


Measuremt of density without pyknometer

Hoffmann-LaRoche - 3-10-2002 at 14:08

The most simple method of measuring the crystal density of a water-insoluble substance is to prepare salt solutions and then test wether the produced crystals sink or swim.

An example: prepare a saturated solution of ammonium nitrate, lead nitrate(i tried this and got a solution with a density of about 1,3g/ccm), sodium chlorate or whatever that has a very good solubility and has a high density itself.
The only thing to take care of is to use a measuring flask and a balance that provides good accuracy.
If this is a problem, prepare bigger volumes of solution to minimize the error.

I seek for other salt solutions that perform densities of near 1,5g/ccm and above....


BLAST_X - 3-10-2002 at 15:10

When DPPP or a peroxide dissolves in ethyl alcohol (aceton ?) and it recrystallizing out from the solution by adding H2O, the quality are bad (crystal-structure, clumpy).
As long as no better possibility exist to handle safe with the crude product, it should been so.

DBSP - 8-10-2002 at 09:58

I found this at E&W, might be interesting, not shure though.

You'll probably have to copy/paste

breakthrough in sight?

Hoffmann-LaRoche - 14-10-2002 at 16:22

I want to give an impuls for pushing our research:

We have the patent, which is vague for many parts of the synthesis, sure.

(just to remind anyone: we HAVE a small fine library which is up to grow...)

But we also made several experiments showing that a water-insoluble substance, pure or impure, in any case not containing acetone any more, thus not contaminating the final product of peroxidation with acetone peroxide, can be obtained by heating a mixture of (50ml conc. HCl and 50ml acetone) acetone and HCl for several hours (ideally under reflux) and following neutralization with sodium (bi)carbonate.

It was important not to exceed pH7 by adding too much sodium carbonate or NaOH..., cause it turned out the product re-dissolves not only under acidic conditions but also under strong alcaline conditions.

It has been noted by all forum members who tried to make phorone using this method, that some decomposition that leads to carbon traces in the solution, giving it a dark colour, took also place.

I also tried this and found the final yield of the product to be very low.
A 100ml batch of acetone/HCl resulted in approximately 1-2g.
To get a more pure product, the phorone could be recrystallized from ethyl alcohol(this is not yet tested).

But from my point of view the low yield hasnt a big impact cause the two substances are really dirt cheap, and the later product DPPP is supposed to be used only in small quantities in blasting caps and the like.

The next step should be obvious: dissolving the dried, washed product in HCl to give the chlorinated phorone.
To get a higher yield in the peroxidation step i think it would be better if the pentachlorphorone(by-products excluded here, lets be optimistic...) would be (very carefully!) dried before the final peroxidatoin step.

I think the chlorinated phorone will be a polar substance(due to the high electronegativity of chlorine and the geometry of the molecule), thus better dissolving in 30% aqueous H2O2.

The amounts used in the combined chlorination/peroxidation step can (as always) be played a lot with, only considering the equations from the german patent i calculated the following:

C9H14O + 5HCl + 5H2O2 > C9H13OCl5 + xH2O + yH2O2 > 1/2 DPPP(precipitates) + 5HCl + soandsomuch H2O

(the patents states that nascent chlorine is needed for the chlorination step, so it is actually more than for the peroxidation alone)

From this you can calculate the mass of phorone and the needed volumes of conc. HCl(density is 1,3g/ml) and 30% H2O2 (also 1,3g/ml).

I might have some mistakes in my equations, as this is always possible, and im really really tired.
Give me some feedback.

Could someone calculate this to the end?-I wont make it this time, zzzzzzzzzz


Hoffmann-LaRoche - 14-10-2002 at 16:28

please ignore the part of isolating pentachlorphorone before the peroxidation step, i think this is not really necessary.
I forgot to delete it.

BrAiNFeVeR - 27-10-2002 at 03:30

Well, the sublimation method does NOT work :-(

It's been lying in my lab for more then a month now, and it still smells like AP.

And on quantity ...
There's about 1 gram left of a starting batch of 5 grams !!

So yields are definately not worth having such an amount of sensitive primary lying around for more then a month!!

bonemachine - 28-10-2002 at 01:57

I am ready to try this method anyone had any results?


bonemachine - 28-10-2002 at 01:58

I am just ready to make this compound does anyone had any good results?

bonemachine - 28-10-2002 at 02:00

Forgive me for the double post i thougt the first didn't worked

bonemachine - 28-10-2002 at 03:59

Ok i made a 50/50 solution of HCL and acetone and it heats up quickly. After a wile it forms small crystals at the sides of the container. After being cool i added the H2O2 and now i am waiting.

Is there anything specific about the aperance of DPPP so i can recognise it? Does it have for example a diferent colour or crystal size than AP?

excuse me for bad english.

Reactions of acetone with HCl

BASF - 5-11-2002 at 14:34

I spent two weekends doing this....

1) A) A batch consisting of 30mL 30% HCl and 20mL of commercial acetone in a loosely stoppered flask was heated for several hours until the liquid had a golden yellow colour.
The remaining HCl was neutralized by addition of solid sodium carbonate and i recognized that a yellow-white pptate formed while the liquid cleared up.
The pptate was filtered off and washed with about 500mL of cold water.
Then i dried the pale yellow to white pptate on a water bath(it was actually steam) and weighed it.
Yield of product was 1,5 g.

The product was insoluble in any of the common organic solvents(etOH, hot H2O, acetone, xylene, petrol...).
Soluble in dilute HCl and dilute H2SO4 forming a deep red solution.

B)The same mixing proportions and volumes with extended reaction time.
(Deep red colour of liquid.)
The above process was repeated and 1,7 g of the product were obtained.

C)The same again.
Waited just more till the liquid was a deep dark red, like a blood conserve.
Yield was again 1,7g.

Funny: the powder seems to be an acceptable pH indicator for pH 7: being dark to light red in acidic media, decolourizing at pH 7.

BASF - 5-11-2002 at 15:32

1) 25mL of 30% HCl were added to 75mL of acetone and treated like in C) of the previous post.

Yield was 1,6 g.

2)25mL of dilute H2SO4 with HCl (1:1)were added to 75mL of acetone and kept for 3h on a heating plate at approx. 60°C.
Approximately 60mL of the batch remained due to the loss of acetone by evaporization.

The mix had a light orange-red colour and yielded 0,6g of the abovementioned product.

3)25mL of H2SO4*6H2O(dilute sulfuric acid, saturated with water) were given to 75mL of acetone and heated as above for 3h until the solution had a golden yellow colour.

Yield was 0,2g of a similar product in solubility and optical appearance.

Polverone - 5-11-2002 at 16:11

Interesting. Those yields are terrible, though. Obviously 90% yields aren't attained as easily as the patent would have us think. Are you going to try forming the peroxide, or try to find a better way to make phorone first?

I've searched the ACS journals for information about condensation reactions of acetone to phorone, but the main references are old (late 19th century) and often in German.

DBSP - 6-11-2002 at 04:59

I would just like to point your attention to something an E&W member came up with in the "holy grail organic peroxide" thread.

He might just have a point there.;f=2...

Have a look at the bottom.

BASF - 6-11-2002 at 15:37

I am not very confident that the obtained product contains much phorone as it is non soluble in organic solvents, not yellow or green-yellow, completely solid at temperatures even near 100°C and it only dissolves a little bit with orange to red colour in strong acids such as HCl or H2SO4*6H2O, depending on quantity.

The powder is a very pale yellow to white one with the consistency of flour.

conc. sulfuric acid with acetone

BASF - 6-11-2002 at 16:30

Polverone: If u want u can pass some of the articles to me for translation, i speak german.

25mL of conc. H2SO4 were carefully and slowly given to 75mL of acetone(heated up as with water).
Then the batch was heated at approx. 50°C for 2 or 3 hours till the liquid had again very dark colour.
In thin layers the main content of the flask turned out to be dark red.

Then the black liquid was diluted with double its volume of cold water and neutralized by addition of solid sodium carbonate.
I discovered that very big quantities of sodium carbonate are consumed and it is very time consuming to add the carbonate due to the vigorous reaction.
On the other side, if using 25% ammonia, the neutralization affords less time and relatively low amounts of ammonia, maybe due to the fact that ammonia is better soluble in the acetone-H2SO4 mix and thus enters more easily in the reaction.
Very much stirring and waiting has to be done if solid(solutions of the same would give too big volume) carbonate is used.

I´m not sure wether ammonia also reacts with the reaction products, but i tend to say that this would rather have a negligable effect if the ammonia is not added in excess.

The most interesting thing about this all was the appearance of a small dark green, oily layer(very much like phorone could be, considering the temp was approx. 20°C and the melting point of the product would be decreased by several byproducts) after dilution with water.

I seperated this by filtering(the oily substance was hydrophobic and did not pass the filter as it was always wettened by the aqueous solution running through) and then i could seperate it from the rest of the solid product very easily cause it dissolved in both ethyl alcohol and acetone with orange or black colour, depending on quantity.

I evaporated the acetone and got some mg of an orange to red-coloured non-crystalline layer on the bottom of the flask that smelled exactly like incense.

After that i got a bit "stoned" breathing all those fumes over hours, i decided to come to an end and simply dissolved the small layer obtained with about 20mL of HCl(half of it dissolved), put the black solution(notice the difference in colour to solution in acetone) in another flask and added an equal amount of 30% hydrogen peroxide.

Immediately, from one second to the other, the black liquid cleared up and some white (crystalline?) substance swam on the bottom of the surface.
Now one would fear that such a substance could not have a good density, but considering the overall-density of the peroxidation-mixture, which is at least 1,3g per mL, at least a crystal density equal to acetone peroxide would be possible.

Unfortuneately i had no time left to dry the white product and give it a try on burning "saltpeter-paper", but i will do this as soon as possible and provide u with some photos of the batch.


(The board didnt let me enter as HoffmannLaRoche any more, so now i am BASF)

BASF - 8-11-2002 at 07:37


I read the posts on E&W, but i can say that the inventor definitely didnt mean 9000ft/s instead of m/s!

It is a german invention!-A german would never use ft/s instead of m/s as the metric system is the the most widely used system here.
Furthermore, this would really represent a grave error that the patent office wouldnt tolerate in a patent.

The E&W-thread is not half as informative as the one established here, and is more or less a completely useless disscussion without any progress so far.


vulture - 9-11-2002 at 05:52

After fiddling around with the structure of phorone which seemed very unfavorable to me, I let chemsketch calculate the 3D structure from the original structure in the patent. Surprisingly, the 3D seems quite stable and relatively unstressed for an organic peroxide. The reason the 2D structure looks so strange is that one cannot draw torsion angles in 2D structures which are a key variable to the stability of a molecule.

DPPP according to chemsketch1.jpg - 14kB

vulture - 9-11-2002 at 05:54

Here is the same structure, only rotated around it's axis.

Chemsketch predicts a density of 1,3g/mL for DPPP.....

DPPP according to chemsketch2.jpg - 15kB

BASF - 9-11-2002 at 06:19

My god THATS good news.....1,0-1,3g/mL is the density of the peroxidation product i obtained recently using a product from one of my phorone batches....this really seems to be a fascinating prog you were using.....never thought a simple prog for the home use could calculate densities...


ShockWave - 21-11-2002 at 14:18

Well I have tryed the procedure from Blast_X and it worked fine to me.

The Cristalls that I have are much smaller than AP, And it doesn't smell like AP, now I will let it stand to let the AP evaporate.

ShockWave - 22-11-2002 at 09:15

This is funny.

The Crystalls that I have standing now burns slower than AP, I heard that there is always some AP present in DPPP but AP blinks in light, like real crystalls but my DPPP does not blink at all, It is also less white, and no smoke or smell after burning, the crytalls are very very small.

The wierd thing is that I did not do exactly what Blast_X told.

What I did was this:

10Ml acetone mixed with 10ml 30% Hcl, standing for about 10minutes, no color change just a clear liquid, than I added the 20Ml 30% H202 and kept the temp. below 40c. after the first few ml h202 their was immidiatly a lot of with powder in the glass, When the 20ml h2o2 was added I stirred it very well and waited for 1,5 hours, it looked just like AP, after that, I washed it very well with lot's of water and sodium bi carbonate, I let it dry for 1 day at a warm place, today I did these test and find it very intersting that this powder that I have is so very different compared to AP, If this is pure DPPP, than it is just as easy to make as AP.

And that it burns much slower is an answer why the 5gr from Blast_X did not detonate but just burn.

5gr AP with a fuse ignition would detonate

Microtek - 22-11-2002 at 10:41

Sounds a lot like the results ( and procedure ) from my experiment. I also think that the fact that the product doesn't undergo DDT when ignited with fuse, even if confined lightly, is a strong indication that it is not AP. However, my product sublimed relatively quickly...

ShockWave - 22-11-2002 at 15:19

Well, I just did a evaporate test, at a piece of paper I did a very small amount of AP and at the other end of the same paper I did some "DPPP", and it was above my central heating which was not hot, but warm.

After 2 hours, the "dppp"totally evaporated, and the AP was evaporated just a little !

So the stuff that I have is not DPPP and not AP !

At the picture you can see the paper, to the left is the DPPP which is darker and has smaller crystalls, to the right is the AP, you can see it blinks a little.

dppp_0006.jpg - 59kB

Madog - 22-11-2002 at 15:21

wow! thats weird! did you press that stuff or do impact tests?

vulture - 23-11-2002 at 08:11

Am I correct if i say that what's supposed to be DPPP is amorphous and the AP is crystalline?

Blind Angel - 25-11-2002 at 22:19

250ml Muriatic Acid in 250ml Acetone
Heat up no color change
Added the about 900ml of 3% H2O2 immediately (couldn't fin 30% at the momment)
Reaction (Acetone Peroxyde) precipitate at the bottom
Shaked realy well
The liquid turned yellow and Chlorine disgaged
All the precipitate went on the top and didn't sunk
I've let it stand 2 days then filtered
Did I get DPPP or AP?
And is it possible that AP converted in DPPP if Phorone formed during the shaking?

ShockWave - 26-11-2002 at 00:49

If you want to know if you have DPPP or AP, just do these tests that I did, the evaporate test works fine for me, And tell me, What color is your DPPP and does it blink in bright light?

vulture - 26-11-2002 at 06:08

And is it possible that AP converted in DPPP if Phorone formed during the shaking?

No. The AP won't react with phorone to form DPPP, I don't know where you got it, but chemistry isn't mathematics (Thank God!). Take a look at an AP structure and then at the DPPP structure in this thread.

Peroxidation of commercial phorone

BASF - 26-11-2002 at 07:50

I recently bought 97% phorone at Sigma-Aldrich, which seems to be the only supplier of small quantities.

At first, the phorone was very pure, could easily be melted in a warm water bath and crystallized upon cooling(room temperature) in the form of long yellow needles.

Solubility tests:

-Insoluble in 30% HCl

-soluble in commercial acetone

-exzellent solubility in 98% acetic acid

-Insoluble in commercial ethanol(absolute ethanol needed?)

The phorone does not crystallize at room temperature if surrounded by an aqueous (immiscible) phase.

I tried to peroxidize the phorone(1ml) by first dissolving it in 98% acetic acid (5ml=excess to prevent seperation upon addition of the peroxidation-mix)
and then adding a 1:1 mix of 30%H2O2 and 30%HCl(total of 2ml) in a test tube.

It heated up very strong and i repeated the whole procedure with proper cooling(ice bath), but so far no precipitate occured.
Maybe the DPPP is very soluble even in aqueous solutions of acetic acid, like phorone.

-Or the reaction just failed.
So i added some ml of water to make it seperate along with the rest of unreacted phorone, but nothing remarkable happened.

The last experiment i did was to dissolve phorone in acetone and then tried to peroxidize both.
I was surprised that the phorone seemed to prevent peroxidation of the acetone(no AP-precipitate).


Blind Angel - 26-11-2002 at 09:59

I will try the evaportation test, and my powder is yellowish and don't blink
myabe i just got phorone?

ShockWave - 26-11-2002 at 14:22

Blind Angel

I think you have the same stuff as I have, If you have some AP left than do the evaporate test and see if if the DPPP evaporates faster.

Today I tested the "DPPP" but can not tell if it was stronger then AP, but the stuff detonated and if it is just AP than it is a nice procedure because now you can make AP in less than 5 minutes with a great yield.

Nick F - 26-11-2002 at 14:31

Do a little lead block test. Drill equal sized holes (with a volume of around 0.5cm3) in two blocks of lead. Fill one with CTAP, and one with "DPPP" pressed under the same pressure, initiate both with a few mm of a primary such as lead azide or double salts (you want to be sure that none of either explosive being tested is used up in DDT, so have a "fast" primary that has a short DDT time). If DPPP really is as good as the patent claims, which I doubt, then there will be a significant difference in their effects. If DPPP is not as good as the patent claims, then it will be harder to tell if that's what you have... you'd have to perform several identical tests and take the average expansions.

vulture - 26-11-2002 at 14:37

Nick, IIRC, the Trauzl test is not directly related with detonation velocity.
The sand test seems better to me then. Just use little rocks and see which are broken into the smallest pieces.

I could be wrong though.

Blind Angel - 26-11-2002 at 18:47

I putted some on a sheet of paper than light it up so i detonate. It didn't detonate it just did "Pshhhhh" and the flame got bigger but no "real" explosion got detonated. I still have the yellowish solution from wich i filtrated the product, will try to freeze it (if phorone appears in cold) then will try to heat it to see what happen.

Nick F - 27-11-2002 at 10:42

The VoD is certainly a factor that effects a substance's performance in the Trauzl test, along with energy content, density, gas volume produced, etc (and all these factors have effects on each other, too).
E.g. ethylene glycol dinitrate gives a (water-tamped) standard lead block expansion of 650cm3, glyceryl trinitrate gives one of 590cm3 (COPAE). You can see that EGDN produces a significantly larger expansion, even though GTN is denser by around 0.1g/cm3. This is largely because EGDN has a higher VoD due to its lower vicosity.
But you should certainly be able to tell the difference between a 4km/sec VoD and a 9km/sec VoD(!), especially since the compounds are very similar and are likely to have similar gas volumes.

Blind Angel - 27-11-2002 at 15:33

Do u have further information on this test, myabe more graphical information I dont understand realy well how you can calculate the VoD

BASF - 27-11-2002 at 17:41

It is impossible to calculate the detonation velocity from the trauzl test, but it is possible to compare with other explosives whos vdets are known.
I´d propose making a lead block for 1 or 5g instead of 10g(its not that easy getting so much lead...and after using it, it is toxic waste).
More information on the trauzl test can be found in the cd-roempp-chemistry lexicon(100MB), Thieme Publishing, Germany.
I haven´t seen it on the net so far...but it is the most widely used chemlex here in europe in the schools.
Teachers often allow pupils to copy it.


Blind Angel - 27-11-2002 at 20:41

I searched for Roempp, Rompp, Römpp but still cannot found a readable version (always find non-working .ica file) and more they're in german and i cannot read german, do u have other interesting ressource on this :(
 Pages:  1    3  ..  10