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Author: Subject: HMX by way of nitration of dpt
BASF
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thumbup.gif posted on 4-6-2003 at 10:48
HMX by way of nitration of dpt


Surprisingly, i found this ref. on totse...

They have it from "the preparatory manual of explosives".

It is a low-yield process which has not found industrial application(thus wasn´t patent too), but is very interesting as it does NOT call for Ac2O or P2O5.

The DPT-precursor(3,7-dinitro-1,3,5,7-tetraazabicyclo[3.3.1]nonane) is made by introducing hexamine dinitrate to cold sulfuric acid. The yield of this process is said to be very low, which seems to be the major drawback of this synthesis.

If anyone has the book i´d be glad if he could post the procedure.
(the excerpt is a little bit vague on the mixing proportions, especially on the DPT-synth).

Also, the original ref. of the book, which the retarted guys of totse left blank, would be great ... but this would be birthday and christmas together, i think.

HLR




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BASF
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thumbup.gif posted on 6-6-2003 at 10:01


Thanks a lot !

5% yield for DPT is not impressive, but it´s science, isn´t it ?

:):D:P




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[*] posted on 7-6-2003 at 08:59


I haven't read the whole thing yet so i don't know if it mentioned this.
Don't you think that this method is a total waste of cyclonite (destroying it with ammonia) just to get a very small amount of HMX? I think it would make much more sense to separate them.
This can be done by treating the crude product with dimethyl sulfoxide which will dissolve the HMX and it can then be easily filtered out.
You can recrystalize the separate products to purify them.
You could also use the ammonia to destroy the small amount of cyclonite present in the separated HMX without wasting the shit load of RDX which has been extracted.
Does nitration of DPT yield a larger percentage of HMX impurity than the normal nitration of hexamine? If so that would be a good method to make your rdx more powerful. :)
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[*] posted on 7-6-2003 at 09:10


That's a very interesting document, thanks!



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Krypton
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wink.gif posted on 9-6-2003 at 22:02


BASF,

from what bad reel of film have you
downloaded this document ? ;)




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BASF
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[*] posted on 10-6-2003 at 05:06


? however, i was just fascinated by the fact this method works without Ac2O or P2O5...
BTW, i would never put an eye on totse...i was doing a google search...:P


Quote:

This can be done by treating the crude product with dimethyl sulfoxide which will dissolve the HMX and it can then be easily filtered out.
You can recrystalize the separate products to purify them.
You could also use the ammonia to destroy the small amount of cyclonite present in the separated HMX without wasting the shit load of RDX which has been extracted.


That´s exactly how i imagined it, only using the cheaper acetone.

:P




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[*] posted on 10-6-2003 at 05:45


Are you sure HMX is insoluble in acetone? That would be better. :)
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[*] posted on 10-6-2003 at 09:12


The solubility of HMX in acetone is not very good.
But the one of RDX is.:D;):)

Acetone has been proposed for that purpose in numerous patents. They recommended using hot acetone, then cooling down or alternatively adding water, til you get about 50% acetone.

Hmm...just can´t remember exactly, sorry.

[Edited on 10-6-2003 by BASF]




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[*] posted on 11-7-2003 at 20:15


I remember a patent(cant remember the number though)which talks about the seperation of HMx and RDX.The HMX is first disolved/filtered with hexanol and then the RDX is taken out by acetone.Suposedly this goes to like 98%.
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kingspaz
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[*] posted on 13-7-2003 at 14:20


would using conc. phosphoric acid to dehydrate the HDN increase the initial yield?

not sure if thats any good at dehydrateing but its in my mind so i must have picked it up from somewhere...




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[*] posted on 17-7-2003 at 05:59


Wouldn´t the phosphoric acid also act as a buffer, to certain extent?
If so, then maybe this would increase the RDX/HMX-ratio towards HMX, due to lower acidity(this was mentioned in one of the above patents).




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