DPPP (Diphorone Pentaperoxide) synthesis results and research forum

Discussion in 'General Science & Technology' started by Hideki Matsumoto, Dec 26, 2004.

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  1. Hideki Matsumoto ñ{ìñÇÃóùâ?ÇÕêSÇÃíÜÇ©ÇÁóàÇ ÈÅB Registered Senior Member

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    alright I am having to move all the info from all the other sites into this research forum and condense it into a single forum.

    Diphoronepentaperoxide C18H26O2(O2)5

    The following patent information was graciously translated from the original German by Hoffmann-LaRoche:

    German patent DE 1951660. 1969
    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:

    1 part of acetone are added to 1 part hydrochloric acid, through which acetone polymerizes to phorone; then 2 parts of hydrogen peroxide are added, through which two molecules of HCl bond with the two C-double-bonds of the phorone.
    In the course of the reaction free chlorine develops, which bonds with 3 hydrogen atoms of the phorone to give 3 HCl(see drawing) and bonds itself with phorone.

    Hydrogen peroxide causes the chlorine atoms to split off the phorone and the peroxide itself bonds with the phorone. Because of the fact that one peroxy-bond stays half-opened, one also open phoroneperoxide adds to give diphoronepentaperoxide, 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%
    -----------------------------------------------------------------

    How DPPP is made from German patent

    1:1 30%-Concentrated HCL to Acetone
    2:1 H2O2

    Theory.. HCl changes Acetone into Phorone (yellow green) and then into Pentachlorophorone which is an oily dark reddish liquid. When H2O2 is added the Cl2 is split away and is replaced by the (O2)5.. in summary :

    " 1 part of acetone are added to 1 part hydrochloric acid, through which acetone polymerizes to phorone; then 2 parts of hydrogen peroxide are added, through which two molecules of HCl bond with the two C-double-bonds of the phorone.
    In the course of the reaction free chlorine develops, which bonds with 3 hydrogen atoms of the phorone to give 3 HCl(see drawing) and bonds itself with phorone.
    Hydrogen peroxide causes the chlorine atoms to split off the phorone and the peroxide itself bonds with the phorone. Because of the fact that one peroxy-bond stays half-opened, one also open phoroneperoxide adds to give diphoronepentaperoxide, which precipitates from the solution in crystalline form."
     
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  3. Hideki Matsumoto ñ{ìñÇÃóùâ?ÇÕêSÇÃíÜÇ©ÇÁóàÇ ÈÅB Registered Senior Member

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    Ok these are my results:
    alrighty, I think I have made DPPP in relatively pure form see this http://community.webshots.com/user/matsumoto_hideki
    what % concentration I am not sure but it looks a hell of a lot like TCAP with the exception that it has a distictive yellow colouration to it. Yellow must = Phorone ?
    My method was via the 1:1 2:1 H2O2 method HCl@35% to Acetone then adding heat taking this liquid down that black-red colour (VERY DARK) and then letting this liquid sit for a few days to a week in the open to cool and let some of the unreacted acetone to vapour off. I then took this liquid and chilled it for several hours in a freezer at -25c ie) below -5c is good enough! The Peroxidation is the hard part since the moment the peroxidation occurs the heat really being to climb rapidly, there is a putrid smell of Cl2 coming off the reaction which is a good sign. This indicates that the Cl2 is being replaced by (O2)5 ... I find you have only a few secs between the formation of YELLOW precip and the secondary reaction which intitiates a complete boil over... I did manage to controll the heat by sitting it in a super cooled mix of slat/ice. temp was around -8c or so..
    So as soon as you see the precip form wait 3-5 secs then nutralize the reaction with Ammonium Hydroxide. I would also reccomend the use of a thermometer as you'll have a complete temp analyisis of the reaction. The reaction is best below 40c any warmer than thisc ie) beyond 50c and I find the Phorone converts over into acetone, HCL and water vapour...
    Precip is yellow - to cream colour and has way more power than AP! I have a few movies of AP and DPPP going off in the same amounts and the results are clearly visible. DPPP also seems to detonate in much smaller quantities than AP does and doesn't seem to sublime at all at room temp. My first cople batches had a little bit of a fruity acetonish smell to them, I do think this has somthing to do with TCAP being precipiated in the solution along with the DPPP.


    ---- my second batch (...for posting purposes)
    Pentachlorophorone is produced via same method as stated above and let to sit in a arm place 30-40c for 1 week.
    an oily dark-red liquid with the consistency simular to motor oil was produced with an EVIL odor.. extreamly heavy pungent semi metallic) odor

    I then used Sodium Hydroxide (Xgrams) to nutralize the left over HCl... to my amazement most of it was gone.. YAY

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    apon peroxidation the solution was placed into a cold water bath and same characteristic odor of Cl2 was noticed and the solution began to immediatly lighten to a yellow colour.
    very fine yellow crystals formed without any whitish-yellow precip. the precip was almost exactly 90% of the entire container vol. WOW !!
    I have yet to test this particular material as it is drying..
    More pics coming soon
     
    Last edited: Dec 26, 2004
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  5. Hideki Matsumoto ñ{ìñÇÃóùâ?ÇÕêSÇÃíÜÇ©ÇÁóàÇ ÈÅB Registered Senior Member

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    DPPP mystery is cracked !! THE KEY FOR MAKING DPPP IS THE DISTILLING OF THE BLACK_RED LIQUID INTO THE MOST CONCENTRATED YOU AN MAKE IT.. Should have a concistancy of lite motor oil.
    DPPP has a plate like pentagramlike crystal structure and is (dark yellow orange) almost umber coloured. kinda reminds me a bit of (wulfenite)
    My synthesis was correct and WOW I even have pics and video of a micro amount deflagrating and one of a melting- to semidetonation. It deflagrates at an amazing speed as well. at least 3x faster than TCAP does in a small amount. DPPP also is totally smelless when it detonates and has a tiny amount amount of soot was seen in the deflagration.. however when it actually detonates no soot is formed... interesting. As the patent says it also detonates when contaminated ... I mix 50% with very fine saw dust an it detonated like AP... but with the smell of hot wood... cool .. i wonder if you mixed it with sandalwool dust you could get a kind of explosive insence going?

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  7. James R Just this guy, you know? Staff Member

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    Please do not post recipes for explosives on sciforums.
     
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