An+sulfuric for nitro esters - Archive file

[zaibatsu]

radar
Frequent Poster
Posts: 63
From: Redding California
Registered: DEC 2000
posted January 10, 2001 08:58 PM
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Do any of you know a method in which i can do I can do a simple ester nitrification with just sulfuric acid plus ammonium nitrate and then add my material being nitrated? Like for example meriol or nitro glycerine or EGDN? Thanks

sadsakjoel
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Posts: 170
From:
Registered: OCT 2000
posted January 14, 2001 06:05 AM
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hello, what is EGDN?

Mr Cool
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Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted January 14, 2001 06:20 AM
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EGDN = ethylene glycol dinitrate. It's like nitroglycerin, but a bit more storage stable, a bit less sensitive, and a bit more toxic. I think the power is about the same.
The only time I use that sort of method is when I make nitrocellulose, but I use KNO3 not NH4NO3. If you're interested in that recipe, say so and I'll type it out here. I think you need to do it at a slightly higher temperature, which might not be good for NG or EGDN.

Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted January 14, 2001 06:21 AM
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Did you mean to say metriol (= methyl nitrate)? Or is this a different thing I haven't heard of?

Mr Cool
Frequent Poster
Posts: 991
From: None of your bloody business!
Registered: DEC 2000
posted January 14, 2001 11:53 AM
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Sorry, I was confused in my last post. Myrol = methyl nitrate. I suppose you were talking about making metriol trinitrate?

[frogfot]

Nitrating cotton with sulfuric acid/KNO₃ (or other nitrate)?
Wouldn't there be problems to make this nitrating mixture homogen, or will KNO₃ totally dissolve?
I'm asking this because i find it hard to cover cotton with nitrating mix even when using usuall method (nitric/sulfuric acids).

It seems that non-homogen mix can lead to partial nitration or even cause some "hotspots".

[Sparky]

Mr Cool, I am interested in your procedure to make nitrocellulose with KNO3 and H2SO4, could you type it out? I have read the available threads on nitrocellulose but haven't found any satisfactory method using KNO3 which has been shown to work. SWIM tried the Sam's procedure but it doesn't seem to work. Maybe she screwed it up.

[kingspaz]

procedure that will give a complete nitration of cellulose (using pure cotton wool pads):

0.5g cellulose
5g conc. H2SO4
2g of NH4NO3 or 2.5g KNO3

1. add nitrate salt to sulphuric acid taking care to add it slowly in small amounts and not letting the temperature exceed 50*C.
2. add the cellulose to the acid and squash it down under the surface making sure it is all covered with the nitrating mix.
3. using a hot water bath and a cold water bath keep the temperature of the mix between 38 and 42*C (ideally 40*C)
4. leave the mixture to nitrate for 40 minutes at the temperature then pour the mixture into cold water of atleast 3 times the volume of the mix.

to purify:
1. 3 washes with hot water each of 30 minutes.
2. wash with hot bicarb solution for 30 minutes.
3. add to a fresh bicarb solution and leave to sit overnight (12hrs).
4. wash with hot water again.
5. wash with a hot 10% urea solution for 30 minutes.
6. wash with hot water again for 30 minutes and then remove the NC and let it dry.

the above process should make the NC reasonably safe to store.

frogfot, yes hotspots are a problem but they can be avoided by using ammonium nitrate as the nitrate source. even when the mixture temperature is very low the ammonium sulphate will not crystalise out into solid crystals but just thicken the mixture making hotspots alot less likely to occur.