Chemical Forums

Please login or register.

Login with username, password and session length

Sponsored links

Pages: [1]   Go Down

Author Topic: I need help knowing what happened to my sulfur dichloride  (Read 8527 times)

0 Members and 1 Guest are viewing this topic.

mnakhla

  • Regular Member
  • ***
  • Mole Snacks: +1/-3
  • Offline Offline
  • Gender: Male
  • Posts: 60
I need help knowing what happened to my sulfur dichloride
« on: June 02, 2008, 05:15:27 PM »

           I made sulfur dichloride by melting sulfur and directly halgonating it with chlorine.. the yellowish molten sulfur gradually formed into a cherry red liquid that had yellow fumes (other than the chlorine) coming off of it... so i was happy that i had achieved to the compound that i was trying to make, or atleast i think i made sulfur dichloride, but as it was being funneled into another container it instantly reformed sulfur and solidified inside the funnel, flask and container...

I had not read anywhere that such a thing would happen... and really im wondering if the small amount of sulfur dichloride that was formed dissolved the  rest of the remaining sulfur and made a super saturated soultion or.. what exactly happened??

could someone please help explain  to me what happened?


thanks Mina
Logged
Im a freak and Im quite fond of it

limpet chicken

  • mad scientist
  • Full Member
  • ****
  • Mole Snacks: +49/-27
  • Offline Offline
  • Gender: Male
  • Posts: 738
  • Vote Limpet for supreme emperor of the new order
Re: I need help knowing what happened to my sulfur dichloride
« Reply #1 on: June 03, 2008, 09:54:24 AM »

It hydrolyses fairly quickly in moist air to S and HCl.
Logged
The light blinds
So behold darkness as our new light
In our darkness we can see
So with others blindness
We take flight.

mnakhla

  • Regular Member
  • ***
  • Mole Snacks: +1/-3
  • Offline Offline
  • Gender: Male
  • Posts: 60
Re: I need help knowing what happened to my sulfur dichloride
« Reply #2 on: June 03, 2008, 10:25:11 AM »

wow that quickly.. i had read that it would do that in water but i would have never thought of it occurring that quickly ... it seems i have to find away to make it with out transfering it from bottle to bottle


thanks
Logged
Im a freak and Im quite fond of it

constant thinker

  • mad scientist
  • Sr. Member
  • *****
  • Mole Snacks: +85/-45
  • Offline Offline
  • Gender: Male
  • Posts: 1273
Re: I need help knowing what happened to my sulfur dichloride
« Reply #3 on: June 04, 2008, 01:16:03 PM »

Since your problem seems to mainly be with moisture in the air...

Air conditioning dries out air, or do this in the winter if you live in an area that actually gets a winter.

You do have a problem with ventilation though if you use air conditioning to dry out the air because you'd have to be in a closed environment. A fume hood could dodge this problem though I guess.
Logged
"The nine most terrifying words in the English language are, 'I'm from the government and I'm here to help.' " -Ronald Reagan

"I'm for anything that gets you through the night, be it prayer, tranquilizers, or a bottle of Jack Daniels." -Frank Sinatra

AWK

  • Global Moderator
  • Sr. Member
  • ***
  • Mole Snacks: +357/-108
  • Offline Offline
  • Gender: Male
  • Posts: 4858
Re: I need help knowing what happened to my sulfur dichloride
« Reply #4 on: June 04, 2008, 06:46:20 PM »

It hydrolyses fairly quickly in moist air to S and HCl.
???
write down a reaction of your hydrolysis
Logged
AWK

AWK

  • Global Moderator
  • Sr. Member
  • ***
  • Mole Snacks: +357/-108
  • Offline Offline
  • Gender: Male
  • Posts: 4858
Re: I need help knowing what happened to my sulfur dichloride
« Reply #5 on: June 04, 2008, 06:55:34 PM »

           I made sulfur dichloride by melting sulfur and directly halgonating it with chlorine.. the yellowish molten sulfur gradually formed into a cherry red liquid that had yellow fumes (other than the chlorine) coming off of it... so i was happy that i had achieved to the compound that i was trying to make, or atleast i think i made sulfur dichloride, but as it was being funneled into another container it instantly reformed sulfur and solidified inside the funnel, flask and container...

I had not read anywhere that such a thing would happen... and really im wondering if the small amount of sulfur dichloride that was formed dissolved the  rest of the remaining sulfur and made a super saturated soultion or.. what exactly happened??

could someone please help explain  to me what happened?


thanks Mina

Sulform forms many compounds with chlorine: SCl2, SCl4 and serie of SXCl2 where x is from 2 to about 100. They easily hydrolyse,
SCl4 + 2H2O = SO2 + 4HCl (fumes)
but also disproportionate (then much of sulfur can be recovered), eg
4S4Cl4 = 4S2Cl2 + S8
Logged
AWK

limpet chicken

  • mad scientist
  • Full Member
  • ****
  • Mole Snacks: +49/-27
  • Offline Offline
  • Gender: Male
  • Posts: 738
  • Vote Limpet for supreme emperor of the new order
Re: I need help knowing what happened to my sulfur dichloride
« Reply #6 on: June 05, 2008, 07:06:37 AM »

Sorry AWK, I should have balanced an equation for that, but at the time, I just got back from my mates 18th birthday party, in no state do work it out:P
Logged
The light blinds
So behold darkness as our new light
In our darkness we can see
So with others blindness
We take flight.

johnuk

  • New Member
  • **
  • Mole Snacks: +1/-0
  • Offline Offline
  • Posts: 3
Re: I need help knowing what happened to my sulfur dichloride
« Reply #7 on: June 09, 2011, 02:02:44 AM »

Sulphur Dichloride decomposes at it's boiling point; which is just 59C.

The melting point of sulphur is 115C. So, if your dichloride was in prolonged contact with the molten sulphur, it will have accelerated the decomposition.

I think I'll have a go at making it with a pipette; packed with sulphur, with chlorine going in at the top and hopefully the dichloride coming out the bottom.

If you wanted to entirely avoid hydrolysis, you'd do this in sealed up glassware. For instance, if the pipette method works, you could swap the pipette for an air condenser / column and fit a flask to the bottom with one of the ports going off to a bubbler, for any excess chlorine to leave through, then purge it all out with dry air, nitrogen or argon so it's entirely dry in there before starting to make the dichloride. Which would hopefully drip out of the vertical column and into the flask.

As I get annoyed seeing people suggest methods as fact without having tried them, I'll make it clear that I haven't actually tried the pipette idea; I've just seen it being done with things like iodine packed in with chlorine going over to make iodine trichloride

Logged

johnuk

  • New Member
  • **
  • Mole Snacks: +1/-0
  • Offline Offline
  • Posts: 3
Re: I need help knowing what happened to my sulfur dichloride
« Reply #8 on: June 22, 2011, 05:07:27 AM »

I've since run a preparation of disulphur dichloride by bubbling the chlorine into around 25mls of molten sulphur over the coarse of 24h. The chlorine was dried by first passing it through sulphuric acid. I was continually distilling off the product as it was formed.

I received back what looks to be a near full yield of the chlorides. The receiving flask was around the correct mark and the elemental sulphur all disappeared from the boiling flask.

This method, however, is not suitable alone if you wish to produce either the the disulphur dichloride or the sulphur dichloride.

When in the boiling flask, there is an excess of sulphur present, which will lead to disulphur dichloride (distillable). On leaving the flask, it is still warm and now in contact with an excess of chlorine. This leads to the formation of sulphur dichloride on the way out, as my receiving flask came out cherry red. But, as the disulphur dichloride is cooling and leaving, it's unlikely all of it will transform to sulphur dichloride. I suspect the result is a mixture of both. I have measured things such as it's density using class A volumetric glass and a 0.01mg balance. It is dead on the centre for both of the chlorides. The boiling point recorded during the constant distillation was also between the two.

There are a few ways to solve the problem.

1.) Take the product and redistill it with some powdered sulphur in the flask. Provided there is an excess of elemental sulphur present, the sulphur dichloride will decompose to disulphur dichloride and a yellow liquid should be the result.

2.) Take the product and bubble excess chlorine through it, which should convert any disulphur dichloride to sulphur dichloride.

3.) Rather than trying to distil the result off in the first place, reflux it whilst bubbling through excess chlorine, which should result in a flask of only the sulphur dichloride.

4.) There a method involving solvents for producing the disulphur dichloride. The sulphur is combined with chloroform, which boils below the melting point of sulphur. The chloroform will dissolve a small amount of the sulphur. Chlorine is bubbled through. The chloride is formed and dissolves into the chloroform. Provided there is excess sulphur present when the bubbling is stopped, the chloride in the solvent will be disulphur dichloride. Because the sulphur never melts, it is supposed to be a lot easier to clean up, as the sulphur can be removed by simply pouring it out. The, still solid, sulphur excess can then be removed by filtration. The solvent is removed by distillation and then the disulphur dichloride can be distilled to remove the traces of sulphur left dissolved in the solvent.

Both are hydrolysed by water, so all of this benefits from having a constant positive pressure on the glass and preferably some form of drying or trap on the exit to prevent water back tracking into the results. The chlorides are not aggresively reactive with the atmosphere, but they do fume when disturbed. For example, when sitting in an open flask, mine did very little. But fumes appeared as I picked some up with a pipette to measure it's density and such. The fumes are acid gas decomposition products. The product smells of chlorine, sulphur, has a stinging quality to it due to the acid gases produced on decomposition and there is a slight 'rotten' smell to it, as we might expect from hydrogen sulphide. But the latter is vastly diminished by comparison to the smell of a reaction directly involving hydrogen sulphide; which absolutely wreaks of stagnant drains and sewers.

On turning the heat off under my boiling flask (the chlorine generator had expired), there appeared to be elemental sulphur still left. The next day, this seemed to have disappeared from the walls, leaving a few drops in the bottom. On rinsing the glass with water, this also disappeared. A waxy opaque coating was left. What I had seen remaining was likely sulphur chlorides, which had then decomposed to micronic elemental sulphur and sulphur oxides. These were left in the boiling flask because it is impossible to recover 100% during a distillation due to the volume of dead space in the glass and the films left on the walls.

As the chlorides can dissolve sulphur, it is possible they are capable of carrying at least a small percentage of it over to the receiving flask with themselves. Disulphur Dichloride also looks similar to molten sulphur in terms of colour.
« Last Edit: June 22, 2011, 05:20:24 AM by johnuk »
Logged
Pages: [1]   Go Up
 

Mitch Andre Garcia's Chemical Forums 2003-Present.

Page created in 0.057 seconds with 23 queries.