I'm gonna get kicked all the way to the Moon, but whatever.

I am doing some nitroglycerin. I know the process, since the reaction itself is pretty basic. I know that it is an electrophilic substitution and that it releases a hell lot of energy. I've handled that with an ice bath and by doing the respective stoichiometry. I add around 5 ml of glycerol every 10 minutes.

All of that works great, until I have to do the wash. I've learned how to do washing and extractions from MIT's OCW. Nitroglycerin is insoluble in water, so I require water to wash the mixture and pull out the acid. <- There's the problem. When I'm doing the wash, the temperature rises and a runway reaction begins.

Any advice, besides the usual: "Just… don't"?

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    $\begingroup$ It's one thing if you take the risk for yourself of synthesizing nitroglycerin. There's nothing we can do about that here, and that sorta covers the "Just ... don't" part you mention yourself. But don't expect anyone to step in and actively aid you in this. Especially given that you don't appear to be a trained chemist, but rather someone who does some whacky home brewing ("I learned how to do ..."). That's like telling a drunk lunatic who wields a gun how to turn the safety off because he couldn't figure that out himself. $\endgroup$ – Antimon Oct 13 '12 at 13:03
  • $\begingroup$ Just… don’t, unless you have adequate mentoring and equipment. $\endgroup$ – F'x Oct 13 '12 at 16:01
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    $\begingroup$ Did you think ahead on how you could safely store such amounts of nitroglycerine? It is very shock-sensitive and becomes even more unstable over time. Do you have a container that would survive the explosion of the amount you want to produce? Can you guarantee that nobody else can accidentally get to the stuff and blow themselves up? $\endgroup$ – Mad Scientist Oct 13 '12 at 17:13

Just do a decantation. Simply discard the acid layer and then do the wash.

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    $\begingroup$ How did you determine that? More details would be useful… $\endgroup$ – F'x Oct 13 '12 at 21:11
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    $\begingroup$ The nitroglycerine is insoluble in water (even though it is hygroscopic) and it's density is higher than water's and lower than the $H_2SO_4$ and the $HNO_3$. It forms a layer which can be decanted before adding water to pull out the acid. $\endgroup$ – Fiire Oct 14 '12 at 2:07

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