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Author: Subject: Cocrystalization
Hey Buddy
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[*] posted on 13-7-2023 at 14:50


Quote: Originally posted by dettoo456  
@underground NMP or another polar aprotic like DMF and DMSO might work. NQ has been verified to be soluble in NMP and DMSO and if the polarity trend follows, then ETN might be aswell


I have a bunch of DMSO used for skin absorption of pharmaceuticals for animals, but Ive never used it as a solvent, is DMSO soluble in water? How would one recrystallize an ETN/NQ cocrystal from DMSO? I could try it


Okay, I tested DMSO in a petri dish. It fully dissolves NQ quickly with stirring around 30 C. Same with ETN. Adding water drops out a fine white suspension. I would assume the DMSO is miscible with the water and it is very fine NQ/ETN coming out of solvent. if thats the case, it's pretty awesome. I suppose the DMSO/water can be washed away from precipitate in a filter. I assume DMSO is unreactive with any of the common energetics. , should wash away without too much is issue. It is like a thin gel at 20C and becomes a little thinner at 30 C, it becomes very thin when water is added. Why is DMSO not used in energetics more often? I suppose it is expensive but not outrageous.

I will try NQ in a 1:1 mole ratio with ETN. The dump it into water and see how it filters...

[Edited on 14-7-2023 by Hey Buddy]
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[*] posted on 13-7-2023 at 17:49


48 mmol DMSO dissolves 48 mmol of ETN/NQ. It took about 15 minutes at 30C stirring 311rpm to dissolve. It could likely take more ETN/NQ with an increased stir time. I'm not going to add more but I think it would handle more. Going to drop water into solvent 1:1 or until precipitation then vacuum filter and wash with water. It is ~2.5g NQ to 7.25g ETN.
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[*] posted on 13-7-2023 at 18:44


It appears to work. There is a uniform crystal of a little smaller than table salt, and the volume of the two materials as a cocrystal is considerably reduced. The dmso requires a massive amount of water to wash out. I at first used equal mass dmso to water which caused some precipitation, but it first comes out like a syrup. So I kept it on stirring and added as much water as would fit in the beaker. The filtered, put back in a beaker, added more water, stirred decanted, rinse, repeat. It would be better to dissolve in a small beaker then dump in a large beaker of water while stirring. Any dmso that isn't diluted enough water holds the dissolved EM like a gum. DMSO cause anything dissolved to be directly absorbed through the skin into the blood stream so gloves are absolutely necessary when using dmso. I would consider it a bit hazardous for that reason, but if precaution is used it seems to be incredibly effective at creating a dense cocrystal.

UPDATE: After looking at this the next day, there is definitely still two materials. The DMSO made them smaller in volume and there is some cocrystallization, but only partial. Not a homogenous cocrystal, I don't know much about crystallization theories. Perhaps it is favored at some lattice ratio interval, and the favored ratio is cocrystallized while the excesses rejected. Regardless, dmso does dissolve both ETN and NQ. I think aspNO3 actually made denser NQ but it was dissolved at higher temperature.

[Edited on 14-7-2023 by Hey Buddy]
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[*] posted on 19-7-2023 at 10:42


Besides DMSO, most solvents seem to work for only ETN or NQ. Perhaps though, we could use that to our advantage. I could try crashing a solution of ETN in methanol into NQ in hot water, or vice-versa. Even with strong stirring it probably would just separate into two layers that slowly crystallize their respective solutes. And even if it did work, I couldn't imagine it having a great density.

[Edited on 19-7-2023 by Sir_Gawain]




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