6dthjd1
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sulfur chloride-drying precursors
When passing chlorine gas into molten sulfur from chlorine that is produced from TCCA+ HCl., is it absolutely essential to dry the chlorine in order
to obtain a reasonable yield?
I have tried twice to pass chlorine into molten sulfur and have failed generally to obtain a reasonable yield or a yield that is somewhat quick to
occur. I am currently hypothesizing that I need to heat my sulfur even more.
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Tdep
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Mood: PhD is done! It isn't good but it's over lol
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To get this reaction to happen at all, i've found you need to distil off the sulfur chlorides as they form. Its quite a complicated setup, but that's
what you need. The drying will impact yield but not a whole heap if it isn't perfect. I doubt that's where your problem lies.
A chlorine generator, run through some CaCl2 or sulfuric acid, then into the heated reaction flask, then have your distillation setup coming off that.
No need for column or getting a reflux going or whatever, but you need to collect the product and pump in the chlorine at the same time. Good luck, it
is pretty bloody awful
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6dthjd1
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Here is my setup:
![IMG_1315[1].JPG - 2.9MB](https://www.sciencemadness.org/whisper/files.php?pid=536406&aid=70634)
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Tdep
National Hazard
Posts: 516
Registered: 31-1-2013
Location: Laser broken since Feb 2020 lol
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Mood: PhD is done! It isn't good but it's over lol
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Ah its the same glassware I use. Long live the claisen adaptor. Although a sideways Allihn condenser triggers me a bit, but if that's all you have
then you work with what you got I guess.
Ok so there could be a couple of things going on here. The fact that that's a layer of sulfur over everything (oh god, the memories) implies that you
are distilling some sulfur chloride but it is then being decomposed by the water. Putting some drying in the chlorine would help yes. Everything in
the photo also looks wet, so if the humidity is high or it literally rains on your setup, that wont help either.
My suggestion would be to get that Vigreux column, plug the end with cotton wool and then loosely pack in with some dry CaCl2. The stick it in the
Claisen adapten, (clamp it) and continue on.
Other areas to improve likely are the heating, but perhaps also the chlorine rate. If you put a lot of heat in but not enough chlorine, you'll just
start to boil off the sulfur (~450 degrees C) and that may be what you're seeing with the sulfur over the setup. Put some drying in there and overdo
the chlorine.
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6dthjd1
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Do you have any idea as to how vigorous the chlorine addition rate should be?
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