quicksilver
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Nitroglycerin Extraction
The extraction of Nitroglycerin from existing sources would be of great benefit for ultra small scale experiements where the nitration of a few drops
of glycerin is time consuming.
A simple, consistent source of high grade Nitroglycerin is double base smokless powder. Having used a variety of solvents with DBSP to obtain
nitrocellulose laquer in various viscosities it seems quite challenging to extract the Nitroglycerin without also breaking down the NC.
I believe I thought I had found the answer however in ethyl acetate. the solvent does not appear to breakdown the NC if exposed to DBSP during a short
time frame (a wash through a paper filter). However diphenylamine is VERY soluable in ethyl acetate. The two popular brands of canister powder that
have large percentages of Nitroglycerin also have large percentages of diphenylamine.
The whole purpose of the exercise is to have small amounts of pure Nitroglycerin and not having even a stabilizer there to influence results of
experiments, etc.
Any thoughts on methods of extraction?
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Rosco Bodine
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Anhydrous denatured alcohol should pull a lot of the nitro out of high nitro content double base , after a good long soaking ....probably several days
. Methanol or isopropanol might also do the trick . Maybe neutralize
the alcohol extract with white vinegar sufficient to form the acetate of diphenylamine , and slowly air evaporate
the alcohol and water until the nitro precipitates , rinse it with a small amount of distilled water , and harvest it
with a pipette . Then you will have the few drops of nitro needed for soaking cotton in a spark gap detonator useful for high ordering the remaining
double base .
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Boomer
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Got a *good* vacuum source? Distillation should work, and might leave most of the stabilizers in the flask, together with the unwanted NC.
And Rosco, I dont think he wants it to det the remaining double base. He's advanced anough to rig up a cap + booster without going through this
hassle...
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quicksilver
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 HA - Don't give me too much credit. Roscoe has had to hold my hand through
simple re-crystalization proceedures that I should have found in the same journal that I found the synth in..... But thank you for the vote of
confidence.....Now I have some further questions....
If a vacume lowers the boiling point, etc of a distiltion is safety a factor (to the point of needing some sort of blast shield, etc) in using same
where I have only the temp of point of explostion (I don't want to loose my glassware, of course), I could set up a board or something but is it too
close in temp?
Methanol did result in a breakdown of the NC when I tried it but it did not run together with the NG! (Several hour exposure @ 25 C) This could be
workable but the idea of using a distiltion rig appears to be a good one due exactly to the vacume lowering the boiling point -> My question is
continually around the safety factor....under a vacume of .5 m methanol should move over through the condenser to the collection vessel at about 130 C
- am I cutting it too close? Have either of you guys ever done something like this and if so what happened? Do you all think this is just an
unworkable concept from the standpoint of safety?
Thinking out loud, the safety issue and the setup of a distilltion rig is close to the same work as a simple nitration. Maybe I was looking for an
easy answer where none existed. It sure would be nice to have a fast, cheap, clean source of NG however.
[Edited on 28-8-2006 by quicksilver]
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Rosco Bodine
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I would certainly recommend against distillation of NG and a few other highly energetic nitro or nitroester cpds .
When you get vapors of materials such as this
within the confines of equipment and under distillation conditions , what you may ordinarily observe as stability
for the liquid at the same temperature is not necessarily so for the vapor at reduced pressure . A more finely
dispersed form of the material is far more reactive and
far more dangerous , exponentially more dangerous
to handle in this case I would expect , than the liquid ,
and the vapor is in contact with the liquid , so if the
vapor goes , not only may the apparatus be destroyed by its ignition/detonation , but it may also bring about the detonation of the liquid . I would
never attempt this
except in a barricaded apparatus remotely operated ,
using equipment regarded to be expendable .
The danger is exponentially greater than for a simple nitration . My advice here is don't do it .
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Nick F
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"It sure would be nice to have a fast, cheap, clean source of NG however."
I still don't see why simply making your own won't be much faster, MUCH cheaper and probably much cleaner than extraction from DBSP...
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Rosco Bodine
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When I first saw this thread it actually went straight to a
sort of McGyverish proposition of how to accomplish
a high order capable device using fewest chemicals ,
and OTC components , and it reportedly can be done by getting some of the " soup " from a high nitro content double base and using it to fabricate a
spark gap det that utilizes coaxial cable crimped to a metal tube containing cotton soaked with the soup and a capacitive discharge source like a
disposable camera flash circuit .
Some of the first detonators actually worked on this principle , before mercury fulminate came along .
So it seems that this could be done without having to buy any acids or nitrates or glassware , really the most basic sort of OTC improvisation using
minimal components . In that context it makes sense to
go the extraction route . I have never tried it myself
for confirmation , but see no technical reason why it shouldn't work .
[Edited on 28-8-2006 by Rosco Bodine]
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Boomer
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To be honest, I would not distil it either unless remotely. And with "good" vacuum I mean a professional pump, not an ass-pirator. Still I read it
*can* be done, but with a vacuum so low it boils at say 50C and the condenses fed with a freezing mix. What is called for here, 0.1mm Hg or what
(grin).
Doing a batch the usual way is *much* easier of course, and probably safer too. I recommend that, unless this is just to test a concept like Rosco
stated.
BTW what about the old tale about "cooking" nitro out of dynamite by boilling the sticks in water? Anybody tried this with a modern variety - the guhr
version will excrete oil in hot water, no doubt, but a gelled type?
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quicksilver
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A story from my sordid youth....
A very long time ago I had found some older sticks in a mine (I live in quite a rural area even today) and knowing the danger of same, did not touch
them. My friend at the time who was younger than me thought of disposing of them so we could continue to explore the shaft and he put what was left of
the cardboard carton in a wheelbarrow in which was a lot of water. The sticks wept after a long period (couple of days) as we had to walk by the
wheelbarrow to get inside the mine. Ihe amount of NG was quite large and could easily be picked out with a spoon. It may have been 75%, I had no way
of knowing as the carton was badly messed up. The brand was "RED-something-something" and was in a diamond shape. the sticks were wide, about 2" in
diamiter. The absorbant material could have been AN as not much was left in the muck from the sticks in water. I did remember that the amount of NG (I
knew even back then what the basic composition of commercial explos were) was quite large. I knew that if the NG were disturbed we could be in serious
trouble but the fellow I was with said that his was the safeist course of action (I think back on that and shake my head). We were only students at
the time but I remember that the amount of NG on the suface was enough to be remarkable. Also in recolection was the fact that since there was some
wax staining still on the stick surface they may have not been as old as the carton made them appear. However they were breaking apart from exposure.
The weeping seperation concept was a simple one as the absorbant is often water soluable (i.e. diatomatous earth, HN4NO3, NaNO3, saw dust, etc).
DBSP often as a glaze of graphite. This makes seperation a bit more difficult without some stirring or movment to remove the glaze. This does not
occur in some products and there are some with a high NG content that are very simple in composition. The idea for this is about 40% NG which appears
to be most of the very fast pistol powders: Bullseye, AA #2, - the best is an imported Finnish powder with nearly 50% NG. This whole thing seems
workable if one needs only a few grams at most. Diphenyamine is less soluble in methanol then I originally thought. Ethyl centralite also has low
solubility in solvants that thin with water, etc. The only other materials are a tiny bit of polyester and rosin.
[Edited on 29-8-2006 by quicksilver]
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