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Author: Subject: A substitute to acetic anhidride for RDX manufacture
menchaca
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[*] posted on 10-11-2003 at 13:50
A substitute to acetic anhidride for RDX manufacture


Hello again I´ve read in megalomanias´s a way to make RDX from ammonium nitrate and paraformaldehide but in this method acetic anhydride is needed, i think as a dessicant; My question is: is possible to use concentred sulphuric acid instead of it?what other chemical could i ue instead of it? It is almost impossible for me get it because is a very watched chemical here. Thanks !!!!!
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Marvin
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[*] posted on 11-11-2003 at 00:22


As I understand it, sulphuric acid will cause an RDX synth to fail.
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froot
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[*] posted on 12-11-2003 at 05:43


This link: (http://groups.yahoo.com/group/21stCenturySurvival/message/23...)
At the end he says that acetic anhydride is used in the common HNO3/hexamine method to improve 'iffeciency'. If this is true, anybody know the quantities, procedure and yeilds for this method?




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[*] posted on 12-11-2003 at 12:11


in most nitrations where acetic anhydride is used in presence of HNO3, it's used to form acetyl nitrate - a strong nitrating agent
but I'm not a chemist so I can't tell you what it does in the E method (where it is obviously no HNO3)

H2SO4: RDX decomposes very quickly in presence of sulfuric acid. that's why it is not used in any of the methods

the methods involving HNO3 and Ac2O are the Bachmann's method and method KA. both use hexamine dinitrate, ammonium nitrate, Ac2O and concentrated HNO3.
very interesting ways if you can get hold of Ac2O - little usage of conc. HNO3 and high yields :D

forget about method E - low yield and dangerous without BF3
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froot
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[*] posted on 13-11-2003 at 22:52


Well 'click!!'. So that's what Ac2O is, I was wondering if it was Actinium oxide!! 'Umm dudes where do you buy that?'
Thanks man.
Do you have any idea on where I can find typical ratios? I've searched the place flat.


[Edited on 14-11-2003 by froot]




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[*] posted on 14-11-2003 at 09:22


There is a ratio on Megalomania's site. It doesn't reduce well, but its 260mL Ac2O to 105g Ammonium Nitrate to 38 grams Paraformaldehyde.

The Ac2O could be a bit hard to come by. Buying it at least. The synthesis isn't the easiest thing to do either, but not the hardest either. Theres a thread about that here somewhere. It is basically forbidden by the Government for its use in drug manufacture mostly. Converts morphine into heroin or something like that. You can use it to make asprin too. We did that in chem class one year. Having to use it to make asprin, and just seeing all that Acetic Anhydride go to waste make me feel dirty for not being able to do something constructive with it.
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Nevermore
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[*] posted on 14-11-2003 at 09:30


I wonder if AcO method would work with low % HNO3 or act by just increasing the yeld of 100% HNO3...:o



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[*] posted on 14-11-2003 at 11:05


Exactly what I'm asking about Nevermore. I'm familiar with the Meglomania's para/AN/Ac2O method, even tried it but with no real success. After reading that site I mentioned above I've been searching for some kind of Ac2O/HNO3 method.

I don't think a lower conc. HNO3 with Ac2O would work, mainly because the water in the HNO3 would hydrate the Ac2O. You might end up with mainly HDN.
The acetyl nitrate being a strong nitrating agent that was mentioned above sounds interesting.
I'm not sure what the equation for the reaction is but if H2O is a by-product then maybe Ac2O helps keep the reaction dehydrated forming acetic acid as a by-product instead. I'm assuming that water is a no-no for good yields.




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[*] posted on 14-11-2003 at 13:33


Well, if with the AcO is requested to use conc HNO3 anyway, i suppose is not worth the work of getting AcO, but just to distill off some 100% HNO3 then perform the synth with that, unless there is really a big difference with AcO!



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[*] posted on 14-11-2003 at 14:30


Acetylnitrate is a VERY hazardous nitrating agent as it tends to explode violently for no reason.

If there's no way around it it should be made and consumed in situ.

I have a more detailed procedure if you're interested.




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[*] posted on 15-11-2003 at 00:37


I can source acetic anhydride but it's very expensive. Something like an equivalent of $40 for 500ml. But if it does increase yields substantially then it may be worth a try. I hate distilling HNO3 and if I do get absolute 100% it's pure luck. So good yields to me is crucial.
Vulture I'm very interested.

With regards to a substitute for Ac2O I suppose we can brainstorm all sorts of chemicals. Like is there such a thing as citric acid anhydride?? Would citric nitrate be a good nitrating agent?




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[*] posted on 15-11-2003 at 02:03


Quote:
Originally posted by vulture
Acetylnitrate is a VERY hazardous nitrating agent as it tends to explode violently for no reason.
sure it's not stable at all, but I think no one here ever thought about separating it and storing for further use...
it's just that sort of thing that appears in the middle of the equations for a more complicated reaction

BTW the mix of 100% HNO3 and acetic anhydride was also used in aerial bombs in WW2...
but this shouldn't be a problem unless you like putting blasting caps in the reaction vessel :D

and don't heat it to high temperatures as it is (Ac2O is flammable and if you put 2 and 2 together...)
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[*] posted on 17-11-2003 at 13:52


<blockquote>quote:<hr>and don't heat it to high temperatures as it is (Ac2O is flammable and if you put 2 and 2 together...)<hr></blockquote>
also acetyl nitrate detonates above 55°C !
benzoyl nitrate has (rarely) been used as a nitrating agent.




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[*] posted on 28-11-2003 at 19:53


""also acetyl nitrate detonates above 55°C ! ""

Excuse stupidity pls.

IT JUST DETONATES?!?!

NOT DDF (DEFLAGRATE TO DETONATE)???




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[*] posted on 30-11-2003 at 20:55


it obviously makes DDT (deflagration to detonation transition)



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[*] posted on 3-1-2004 at 06:10
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Today at the hardware I found a rather strange chemical. On the one side it says '98% concentrated sulfiric acid' - a powder??
On the other it says it's amido sulfonic acid
I think that when mixed with water it forms H2SO4.
Maybe not for RDX but could this be an interesting water scavenger in nitration reactions?




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[*] posted on 3-1-2004 at 15:58


Quote:
Originally posted by froot

With regards to a substitute for Ac2O I suppose we can brainstorm all sorts of chemicals. Like is there such a thing as citric acid anhydride?? Would citric nitrate be a good nitrating agent?


1) No.
2) Citric acid is a fairly fragile molecule, and would be ripped apart by nitric acid.
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