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Author: Subject: synthesis of Propylene carbonate
elementcollector1
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[*] posted on 6-6-2015 at 23:41


Interestingly, *something* dissolved. I originally started with bright yellow CeCl3 flakes. When these were added to the propylene carbonate, they were bleached white - which is supposedly the color cerium chloride is supposed to be. If that's the case, I'm assuming the yellow color is from CeOCl, which seems to dissolve rather easily into the propylene carbonate (forming a greenish-yellow solution). The solution did not appear to be electrically conductive, but that may be because the amounts of CeOCl responsible for the yellow color were too low to establish any kind of actual current. I'll see if I can hydrolyze some of the white, 'pure' stuff tomorrow, and see if that CeOCl dissolves as well.

This is mainly a test to see whether the RE salts will dissolve to any appreciable extent in propylene carbonate, before I move on to trying to electrowin them. Therefore, water quantity isn't that important - for now.




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[*] posted on 17-12-2015 at 17:14


Update on the above: The white stuff appears to be quite flocculent, and has broken up into small grains which do not stick together anymore. The supernatant liquid is a deep golden yellow in coloration, unchanged from when I last left it.

I get the feeling that the yellow color is not worth trying to isolate cerium from at this stage - if so, how do I purify the propylene carbonate for reuse?

I have a vacuum pump that can reach 5 Pa (apparently), but I don't know what the BP of propylene carbonate is at that pressure, and I'm afraid it might simply not condense under such an intense vacuum. I've heard of 'bleeder' pieces being introduced into distillation setups to raise the pressure a bit, but I don't know how to do this. Any advice?




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[*] posted on 18-12-2015 at 12:45


solvents? if propylene carbonate is miscible with benzene (i checked it is) then water may separated phases salt in one, carbonate/benzene in the other. Unless you'll find you have a complicated mix, but how hydrophilic can propylene carbonate be?

anyway if you get it cold enough it will condense, look at pluto

[Edited on 18-12-2015 by halogen]

ah, yes, You see? miscible with benzene, ethyl acetate, etc., partly miscible with water. not micible with hexane. that's interesting.

https://books.google.com/books?id=oJy5wdzi0yUC&pg=PA178


[Edited on 18-12-2015 by halogen]




F. de Lalande and M. Prud'homme showed that a mixture of boric oxide and sodium chloride is decomposed in a stream of dry air or oxygen at a red heat with the evolution of chlorine.
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[*] posted on 18-12-2015 at 20:03


According to a nomograph, the BP of propylene carbonate at 5 Pa should be somewhere around 30.5 C. If that's the case, ice water should condense it, yes? Not sure how great the difference in temperatures needs to be to prevent too much vapor entering my vacuum pump.

Benzene is something else to try, if I can get my hands on it. For now, I'll stick with the resources I have.




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