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Author: Subject: Chlorination of Sulphur
gdflp
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[*] posted on 25-3-2015 at 13:42


Quote: Originally posted by Molecular Manipulations  
Nice, 31% yield ain't bad for such a simple apparatus.

How are you calculating that, based off of theoretical formation of SCl2? I'm getting a number around 56% yield, am I missing something?
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[*] posted on 25-3-2015 at 13:47


Me Tired, you're probably right, I'll check my work later but I'm sure I made some error.



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[*] posted on 25-3-2015 at 14:35


Ah. I filtered it after the reaction finished, as there appear to be some small yellow grains in my 'pure sulphur'.

The weights are accurate though (so my 0.01 dig scales say).

When i stuffed the product in that 25ml RBF there immediately appeared a few yellow blobs.

I assumed there was some water in there, and the SCl2 reacted with that to make Purest Yellow Blob.




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[*] posted on 25-3-2015 at 14:44


This is a seriously cool procedure. I am tempted to try it myself.
The problem is that I have no need for sulfur dichloride whatsoever. I have no idea what I might do with it when done.
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[*] posted on 25-3-2015 at 14:52


gdflp is being generous : i work it out as 55.63% yield.

It looks great and will get dumped into some linseed oil to see if White Factice can be had.

Happy happy.




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[*] posted on 25-3-2015 at 14:53


Chlorinate organics? That's its main use.



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[*] posted on 25-3-2015 at 15:10


Sulphonate so the papers says.

The idea seems to be to cross-link the oily stuff to make it gel, then harden.

I cannot pretend to have much of a clue as to the mechanics of that.

Edit:

The Objective is to make a synthetic rubber (factice) from some oil.
I tried sulphur & olive & sunflower oil, and it failed (sticky tar, no rubbery stuff).

For White factice the papers say to use SCl2 hence this experiment.

My expectation is a White tar, rather than a Brown one.

Future experiments will tell.


[Edited on 25-3-2015 by aga]




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[*] posted on 25-3-2015 at 16:26


Definitely something I'd like to try too. Favoriting this thread for now, and hopefully I'll be able to make time in the next couple weeks to try it out. But I might want to wait until I get some ampoules...
Looks like a great procedure though, aga. Even if it isn't the most precise and clean method for making sulfur dichloride, it's quite approachable and doable. I really look forward to trying it.




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[*] posted on 10-8-2015 at 08:28


Having had some luck with S2Cl2 in factice making, i stumbled on a one-line reference to CS2 doing the same trick :

http://www.sbioinformatics.com/design_thesis/Carbon_Disulfid...

A bit of reading says that CS2 is Nasty, but then, every chemical is called nasty.

Apparently heating carbon and sulphur at high temps yields some CS2.

Does anyone have any experience with Carbon Disulphide and/or any thoughts on it ?

[Edited on 10-8-2015 by aga]




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[*] posted on 10-8-2015 at 08:43


I thought this might be a worthwhile mention.

If you heat an excess of TCCA ground finely with sulfur a red-orangish liquid starts to distill off. I ran a few test tube scale experiments have obtained about 120 mL of this liquid that seems to also contain some solids that settle to the bottom. The reaction seems to begin at the time the sulfur starts to melt. A lot of gas is given off, so this needs to be directed somewhere. I heat the flask with a propane torch to ensure the reaction goes to completion.

I have not worked this up to isolate the product and get a boiling point, so it could be anything, however, it seems to be a very quick way of producing a lot of liquid within a minute or so, so if the major product is S2Cl2, then its a quick way to get enough for an experiment. It's still sitting in a stoppered test tube waiting for me to get around to it.

An interesting thing happened after the experiment. I was using a latex tube to leading into a beaker to help wash the gases being generated. This latex tube turned grey and hardened upon exposure to the reaction vapors and resembles nothing of latex any longer. Is this perhaps vulcanized latex rubber? Rubber stoppers also swell very badly when exposed to the vapors.

I hope to get back around to this and conduct experiments in a more methodical manner, but I just lack the time right now.

The downside to this is that a mass begins to form in the flask as the reaction progresses. I am assuming this is cyanuric acid. It's a bit of a pain to clean, but isn't difficult.

[Edited on 10-8-2015 by Loptr]

[Edited on 10-8-2015 by Loptr]

[Edited on 10-8-2015 by Loptr]
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[*] posted on 10-8-2015 at 08:49


That sounds like a very quick shortcut to disulphur dichloride !

Drip a little into water and see if it instantly dumps elemental sulphur out.




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[*] posted on 10-8-2015 at 08:50


Quote: Originally posted by aga  
That sounds like a very quick shortcut to disulphur dichloride !

Drip a little into water and see if it instantly dumps elemental sulphur out.


It does and gives off HCl.
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[*] posted on 10-8-2015 at 08:53


Excellent discovery Loptr.

Chlorination with Cl2 gas takes a lot longer than a few minutes.




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[*] posted on 10-8-2015 at 09:17


Quote: Originally posted by Loptr  
If you heat an excess of TCCA ground finely with sulfur a red-orangish liquid starts to distill off.

See making SCl2 From TCCA-Na2S,possible or not?
and posts in the other disulfur dichloride thread.




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[*] posted on 28-3-2016 at 15:43


If anyone in aus us having trouble finding good sulphur they have elemental sulphur at bunnings in very section it states 99+% I'll get the name of it soon its fine granules easily crushed to a powder
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[*] posted on 28-3-2016 at 18:54


Fertilizer bloody spell check and fat fingers lol
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