dasgoose21
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Pulling TACN from saturated solution
Okay so Im going to start from the top with my issue. Every time I have made TACN I would just take the solution and let evaporate until I obtained
somewhat of a crystalline paste. From there I would use multiple washings with reagent grade acetone to achieve complete dryness. Quite frankly I'm
done with wasting large amounts of expensive acetone to make sure my product is dry, so I've tried thinking of ways to precipitate the TACN from
solution and from there I can filter and let air dry, with the final stage being one last dehydration in an acetone bath. Does anyone know what I can
do to precipitate my tetra from a fairly concentrated solution? 
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AndersHoveland
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Perhaps you should use pure methanol as the solvent to make the TACN in the first place. Then make an NH3 gas generator (which is not so difficult).
The less water you begin with, the easier it will be to remove the water later.
The only problem with this route is that the methanol creates a flammability hazard. Ideally, the best thing to do would be to use the proper
glassware apparatus to distill out the methanol (recollecting it for later use), and to use an electric hot plate.
The absolute WORST thing you could do is to attempt boiling out all the methanol over a gas stove top in your kitchen. Methanol is very poisonous, and
boiling it inside will fill the building with fumes. Done over an open flame, there is a near certainty that the vapors would lead to flash back and
ignite the methanol in solution.
Another complication/hazard is that TACN fairly easily decomposes under heat, for example if the wet crystals are heated in a test tube over a flame.
The decomposition can be fairly violent (though not actually a detonation). Take care not to let the reaction solution boil dry, and WEAR PROTECTIVE
EYE GOGGLES !! Turn off the heat as soon as any crystals begin to precipitate out. Further crystals likely will precipitate out as the remaining
methanol cools. (ideally, the best way to remove the remaining methanol would be under reduced pressure) At this point, you could allow the remaining
hot/warm methanol to be allowed to evaporate out in a well ventilated area. However, it is probably not a good idea to let it be exposed to air for
too long because TACN is a deliquescent substance. Further crystals of TACN could be crystallized out by putting the solution in a freezer.
[Edited on 21-3-2013 by AndersHoveland]
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Fantasma4500
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the method i always used was this:
20 mL 25% NH4OH
10g NH4NO3
and then add copper metal, this process took long time, but i guess you could make CuCO3*2Cu(OH)2, then add that to NH4NO3
NH4NO3 + CuCO3 (simplifying it) > (NH4)2CO3 + Cu(NO3)2
the ammonium carbonate would under slight heating produce ammonia and water, so it shouldnt really affect it much
the solution should be cooled down and the volume doubled up with acetone
for acetone, you can mix up vinegar with calcium carbonate (you can find a few things made of CaCO3 in nature if im not wrong) or Ca(OH)2
out of this you will get calcium acetate, about 160*C or some it releases acetone, this is quite easy to distill, and you end up with CaCO3 after this
process, so its reusable..
for evaporating the solution off abit use a very wide container of some sort, that should make the time many times less as it evaporates faster the
larger surface used
also distilling out the acetone would help, and to minimize the drying time for the crystals put it in a piece of cloth and squeeze out the water by
twisting the cloth.. then again spread crystals out on a very wide area and the process should go quite fast this way..
if you doubt the method with CaCO3 would work (its just a theory) you could possibly electrolyse a solution of NH4NO3 and NH4OH, but again, ammonia +
electrolysis could potentially give NCl3
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