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Author: Subject: Preparation of S2Cl2
deltaH
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[*] posted on 2-12-2017 at 23:39


When I was a child I used to make chlorine gas by dripping 98% sulfuric acid onto pool grade calcium hypochlorite granules. The gypsum product acts as a desiccant. The reaction is rapid. It's a miracle I made it to adulthood, others say I never did :D

2CaOCl + 2H2SO4 => 2CaSO4.H2O(s) + Cl2(g)

[Edited on 3-12-2017 by deltaH]




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Feriman
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[*] posted on 19-3-2019 at 11:52


Why my final product is so dark?
I used HCl + Hypochlorite Calcium garnular as Cl generator.
I added some sulfur and redistilled product and got a lighter (edit:red) liquid instead of very dark red first one.
Is it useful to distill again for get more pure product? simple or vacuum?which is better?

[Edited on 19-3-2019 by Feriman]

[Edited on 20-3-2019 by Feriman]
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clearly_not_atara
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[*] posted on 19-3-2019 at 13:36


The dark red is probably SCl2, which is red; S2Cl2 is yellow-orange.

The product has a strong tendency to degrade, so it is best used quickly. It may be possible to improve the storage by storing it under some kind of solvent which won't dissolve it -- alkanes are the most likely candidate, although decamethylcyclopentasiloxane, if available, has a unique reputation as an especially poor solvent for many compounds. Other permethylcyclosiloxanes have similar properties. Joints on the storage flask should probably be wax-coated to prevent sticking.

[Edited on 19-3-2019 by clearly_not_atara]




[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 19-3-2019 at 22:01


Quote: Originally posted by clearly_not_atara  
The dark red is probably SCl2, which is red; S2Cl2 is yellow-orange.

The product has a strong tendency to degrade...

So if I leave it some days doest it convert to S2Cl2? How long it takes?

+EDIT: I reflux it for 1hr but no change in color :(

[Edited on 20-3-2019 by Feriman]
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[*] posted on 22-3-2019 at 10:41


Adding sulfur is more than sufficient for converting SCl2 to S2Cl2. I'm not sure what is causing the red coloration, but if I had to guess, maybe there was some iron in the sulfur and you have FeCl3 in the sulfur chloride? FeCl3 has an annoying habit of coming over during some types of distillation, due to its tendency to form diatomic molecules with Lewis acids (particularly FeCl3*AlCl3).



[Edited on 04-20-1969 by clearly_not_atara]
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[*] posted on 23-3-2019 at 08:44


Polysulfides are red. It could be that.



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[*] posted on 23-3-2019 at 22:39


How could polysulfides possibly form? There is nothing in the flasks that could form polysulfides.
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[*] posted on 24-3-2019 at 00:08


I wasn't thinking of ionic polysulfides, but more along the lines of long chains of sulfur atoms. (SxCl2)



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[*] posted on 26-3-2019 at 09:21


Is it possible to dissolve sulfur in Sulfur Chloride solution(that I prepare by this method) for make more Sulfur Chloride,instead of melting sulfur?
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[*] posted on 26-3-2019 at 10:26


SxCl2 + Na2Sy = S(x+y) (long chain of S)+ 2NaCl,
will this work?




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clearly_not_atara
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[*] posted on 26-3-2019 at 10:37


Quote: Originally posted by Feriman  
Is it possible to dissolve sulfur in Sulfur Chloride solution(that I prepare by this method) for make more Sulfur Chloride,instead of melting sulfur?

One friend reports success with this method.

Quote:
SxCl2 + Na2Sy = S(x+y) (long chain of S)+ 2NaCl,
will this work?

https://en.wikipedia.org/wiki/Allotropes_of_sulfur#Solid_cyc...

[Edited on 26-3-2019 by clearly_not_atara]

[Edited on 26-3-2019 by clearly_not_atara]




[Edited on 04-20-1969 by clearly_not_atara]
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draculic acid69
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[*] posted on 27-3-2019 at 02:48


Scl2 can apparently be made by heating NaCl + s8 together like a destructive distillation.im keen on trying it with nabr but upon googling it I probably won't now as it's so unstable and I have no use for it compared to s2cl2 or scl2.no point in going through that much stink unless there's an immediate need for it.thionyl chloride for example.
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[*] posted on 27-3-2019 at 04:17


Quote: Originally posted by draculic acid69  
Scl2 can apparently be made by heating NaCl + s8 together like a destructive distillation.im keen on trying it with nabr but upon googling it I probably won't now as it's so unstable and I have no use for it compared to s2cl2 or scl2.no point in going through that much stink unless there's an immediate need for it.thionyl chloride for example.


Kind of unsure about what you are referring to that is unstable, the SCl2 or a route with NaBr. The SX2 will disproportionate back into S2X2, and will continue to do so since S2X2 is stable.

S2X2 would be nice to have on hand as it can be used for some of the same reactions that calls for SOCl2. I have a liter of Br2 that has been waiting for some time to experiment with S2Br2, and acid bromide/anhydride formation. I have even recrystallized about 800g of sulfur for these experiments.

[Edited on 27-3-2019 by Loptr]




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[*] posted on 31-3-2019 at 10:36


Is reaction between sulfur chlorides and air moisture an exometric reaction?
Because when I opened lid of the container which I keep my product in it,I feel exited warm air from that.
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[*] posted on 31-3-2019 at 11:07


The NaBr route produces an unstable gaseous compound is what I was referring to.
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