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Author Topic: sulphur chloride  (Read 128 times)

hypnos

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sulphur chloride
« on: October 22, 2009, 01:54:38 AM »
hey can anyone help me with making/buying sulphur (mono)chloride? i have some silver acetate and want to try the AA synth-- a few things also--

where can i get,find,make anhydrous ether? is it essential?--when i distilling the ether it says to "remove the last traces using DRY hydrogen" is this REALLY neccessary" :-\
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zajcek01

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Re: sulphur chloride
« Reply #1 on: October 22, 2009, 06:08:55 AM »
I will try it some day using procedure similair to the one found on wikipedia.
http://en.wikipedia.org/wiki/Sulfur_dichloride

Chlorine gas will be bubbled trough molten sulfur, then distilled.

What procedure will you use for the production of AA? Will it be similair to the one on rhodium's archive?
Ether can be found in starter spray for diesel cars (last resort), It can be made from ethanol and excess sulfuric acid (distillation).
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no1uno

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Re: sulphur chloride
« Reply #2 on: October 22, 2009, 09:55:14 AM »
Here is some of the information which is easily available online in regard to your question vis-a-vis how to prepare Sulfur Monochloride (S2Cl2)

If you want, have a look at the reference request thread where Java just provided the answers to your questions vis-a-vis the reaction between it and GAA

Now, UTFSE and help yourself to the rest ::)
"...     "A little learning is a dang'rous thing;
    Drink deep, or taste not the Pierian spring:
    There shallow draughts intoxicate the brain,
    And drinking largely sobers us again.
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styphnate

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Re: sulphur chloride
« Reply #3 on: October 22, 2009, 08:38:23 PM »
I'll through in my 2 cents on this reaction:

It sucks.  Now, I have never used S2Cl2, but I haveused its bromine counterpart with silver acetate.  In my exoerience, my product was contaminated with nasty black tar and acetic acid, even after distillation.  Some AA was probably present, given the distinctivce smell, but I don't see any decent way to purify the product in decent yield.  I would suggest you go another path.  Perhaps thionyl chloride or tosyl chloride?

hypnos

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Re: sulphur chloride
« Reply #4 on: October 23, 2009, 12:36:06 AM »
hmmmm, it was TFSE that gave me the idea in the first place!!!! ::)  sorry if i seem slack to some of you--i'm pedalling as fast as i can :P

one of the "problems' i have is with nomenclature ( names/naming) of chemicals depending on which source i am looking at esp. if its 80+yrs old  ???

my ideas came from "preparing anhydrides"--i love these old links(thanx heisenberg/java) 8)

by
    William Smith Denham
J. Chem. Soc., Trans.1909, 95, 1235- ...
...  preparation of anhydrides
William Smith Denham and Hilda Woodhouse     
J. Chem. Soc

 but i sometimes have a bit of trouble with them (esp.names-outdated maybe?) and hence difficult to find and clarify with TFSE!!    but hey i am here to learn and share ;D

i have about 50 gms of silver acetate which only yesterday i was looking at thinking "' hmmmm? what am i going to do with you?" and an hour later i 'accidentally' found this synth

styphnate check it out--the is no distillation (initially at least) i wonder what type of solution i will have after 'decomposition' of the product after 3 days in the fridge!! will i need to distill to seperate?

i dont know--does anyone?

but first things first......s2cl2-- and i dont know how i can safely use chlorine gas without a lot more lab equipment than i have right now :(

"the two things you can give away and never lose, are what you know, and how you feel...."

no1uno

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Re: sulphur chloride
« Reply #5 on: October 23, 2009, 07:57:56 AM »
Hydrochloric acid onto hypochlorite (or any bleach in fact) will give chlorine gas - dry it by passing it through CaCl2 or via H2SO4

You don't need much at all to make chlorine gas, just don't breath the shit in or you'll have the same hacking cough a lot of people I don't know here probably also have :P - also a marked predisposition to chest infections, colds etc.

A syringe full of HCl put through a hole in a 2-hole stopper - pass a tube through the other - use permanganate/bleach/whatever as the oxidant - pass the tube into the bottom of a jar containing CaCl2 (for preference - H2SO4 is not so easy to get here), then another tube from the lid thereof passing to where you want your gas (big tip - use glass whenever your tube is going to outlet Cl2 gas - even get it from eyedroppers)...

A couple of glass jars with rubber stoppers, some aquarium tubing, an eyedropper tube and a syringe...

PS I'd also suggest you do this FAR away from anyone you don't want smelling weird shit
"...     "A little learning is a dang'rous thing;
    Drink deep, or taste not the Pierian spring:
    There shallow draughts intoxicate the brain,
    And drinking largely sobers us again.
..."

Vesp

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Re: sulphur chloride
« Reply #6 on: October 23, 2009, 10:19:40 PM »
From my experience the chlorine doesn't need to be dried, and once you have a little bit of SCl2 you can dissolve sulfur in it, reflux and add chlorine to produce as much SxCl2 as you would like - excess sulfur will lead to S2Cl2, while excess chlorine will lead to SCl2

I've produced ~50mls but I know it would not be hard to produce more using this method.

Reflux condenser and flask are difficult to separate after, and it is difficult to store.
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no1uno

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Re: sulphur chloride
« Reply #7 on: October 27, 2009, 07:45:46 AM »
Insofar as producing the S2Cl2, Len1 has an illustrated practical guide, you really cannot do better than to follow it. The rest as they say, is up to the experimenter - YOU... Maybe check whether S2Cl2 is soluble in any chlorinated solvents/Glacial acetic acid, maybe read the various papers and ask questions based upon specific portions thereof... The community could probably help you modify a synthesis route, can't say I'm overly excited about spoonfeeding anybody one but
« Last Edit: October 27, 2009, 07:48:15 AM by no1uno »
"...     "A little learning is a dang'rous thing;
    Drink deep, or taste not the Pierian spring:
    There shallow draughts intoxicate the brain,
    And drinking largely sobers us again.
..."

hypnos

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Re: sulphur chloride
« Reply #8 on: October 28, 2009, 04:34:22 AM »
faaaaaaaark!! i just got 'timed out' on another largish reply.... :'(  yeah thanx no1uno it was the method of bubbling gas i needed coz i have never done so before--like many things in life

there are 'easy ways' and 'hard ways' so i very much appreciate your input :) 8),,please forgive my ignorance  :-[

 as they say,,"the best thing about banging your head against the wall,,,,,is stopping!"
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Vesp

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Re: sulphur chloride
« Reply #9 on: October 31, 2009, 02:46:19 AM »
Quote
faaaaaaaark!! i just got 'timed out' on another largish reply.... Cry 

Sorry about that! I don't know what is going on - perhaps when you loggin you can control how long it takes to time out?
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hypnos

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logout
« Reply #10 on: November 01, 2009, 11:39:12 PM »
na matey not your fault...mine..i just use the autologout function and then forget i have :-[ hmmmmmmm????
"the two things you can give away and never lose, are what you know, and how you feel...."
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