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Author: Subject: Elemental sulfur from sulfates?
Junk_Enginerd
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[*] posted on 8-9-2019 at 00:00
Elemental sulfur from sulfates?


Hey

Sulfur is starting to become quite a chore to get a hold of where I'm at. It's not impossible yet though, so note I don't need suggestions on how to find it.

Mostly out of curiosity, I was thinking of ways it could be synthesized from what I do have. My main sulfur containing cheap bulk chemicals would be iron sulfate and gypsum.

I've read around a little here and done some random googling and found a couple of ways from FeS2 to sulfur, but none from sulfates...

There's got to be a route for this right?

I suppose I could just outright calcine the iron sulfate to SOx and pipe it through hot activated charcoal to reduce it, but that'll be labourous and messy as fuck. I don't know how I'd separate charcoal from sulfur either. Maybe melting the sulfur... What other ways might exist?

An electrochemical process would be neat for me, if that's a way. I've got half decent equipment in that area, but not the chemical know how to figure out how to use it here.
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Deathunter88
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[*] posted on 8-9-2019 at 00:16


Well to separate sulfur from impurities a great way is to dissolve it in toluene or xylene. Not sure it would be practical to calcinate large amounts of most sulfate salts though.
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[*] posted on 8-9-2019 at 03:29


Quote: Originally posted by Deathunter88  
Well to separate sulfur from impurities a great way is to dissolve it in toluene or xylene. Not sure it would be practical to calcinate large amounts of most sulfate salts though.


Allright, good tip. I have xylene so that works.
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wg48temp9
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[*] posted on 8-9-2019 at 03:59


Calcium sulfide can be produced by the carbon reduction of the sulphate I guess that iron sulfide could be produced by the same process.

Sulfides can be used to produce hydrogen sulfide which can be burnt in a limited supply of air or oxidized in solution to produce sulfur.

Sulfur can be separated from carbon very easily as carbon is not volatile at any reasonable temperature while sulfur boils at about 450C and also sublimes at low temperature. meaning it can be distilled or sublimated from the carbon.




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Alkoholvergiftung
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[*] posted on 8-9-2019 at 04:33


You dont Need to burn the H2S Gas you only Need it to bubble througt MgSO4 solution or FeSO4 or over moist Gypsum. You get Metall Sulfid and lot of Sulfur.
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[*] posted on 8-9-2019 at 10:52


Quote: Originally posted by Alkoholvergiftung  
You dont Need to burn the H2S Gas you only Need it to bubble througt MgSO4 solution or FeSO4 or over moist Gypsum. You get Metall Sulfid and lot of Sulfur.

Really?
How?
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AJKOER
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[*] posted on 8-9-2019 at 13:40


The action of highly electropositive zinc metal with H2SO4 does apparently create some H2S gas! Source: See for example, https://chemiday.com/en/reaction/3-1-0-985 . See also comments at https://books.google.com/books?id=Dv_F03cdKPUC&pg=PA429&... .

Shaking an aqueous solution of H2S with H2O2, or some chlorine gas, or add a small amount of hypochlorous acid, or even chlorine bleach (but not in excess), will liberate elemental sulfur. Reactions:

H2O2 + H2S --> 2 H2O + S (s)

Cl2 (g) + H2O = HCl + HOCl

H2S + HOCl --> S (s) + H2O + HCl

H2S + NaOCl (aq) --> S (s) + H2O + NaCl (aq)

But, do avoid an excess of, for example, HOCl owing to:

S + 2 HOCl --> SO2 + 2 HCl

And, in further excess, even back to sulfate!

[Edited on 8-9-2019 by AJKOER]
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teodor
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[*] posted on 9-9-2019 at 02:49


Quote: Originally posted by AJKOER  
The action of highly electropositive zinc metal with H2SO4 does apparently create some H2S gas!


Thank you AJOKER for this information! Because I always thought the smell of H2S from this reaction is because of some impurities, like with Fe. Also the "Inorganic Reactions in Water" contains another interesting information.
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[*] posted on 9-9-2019 at 03:51


Quote: Originally posted by teodor  
Quote: Originally posted by AJKOER  
The action of highly electropositive zinc metal with H2SO4 does apparently create some H2S gas!


Thank you AJOKER for this information! Because I always thought the smell of H2S from this reaction is because of some impurities, like with Fe. Also the "Inorganic Reactions in Water" contains another interesting information.


I also noticed smell of H2S when I reacted zinc and H2SO4 and it surprised me.

Quote: Originally posted by AJKOER  
The action of highly electropositive zinc metal with H2SO4 does apparently create some H2S gas! Source: See for example, https://chemiday.com/en/reaction/3-1-0-985 . See also comments at https://books.google.com/books?id=Dv_F03cdKPUC&pg=PA429&... .


In this book is answer to my recent question about reaction of thiocyanate with zinc/nascent hydrogen. Thank you very much!

[Edited on 9-9-2019 by Bedlasky]
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teodor
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[*] posted on 9-9-2019 at 04:20


So, is it possible to reduce, say CaSO4 by Zn and heating? Because there is another thread about converting CaSO4 to something useful and couple of new threads about getting CaS. It seams that Zn could be an options for all of them. Considering the melting point of Zinc it could be much better route than reducing with carbon.

[Edited on 9-9-2019 by teodor]
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Alkoholvergiftung
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[*] posted on 9-9-2019 at 05:31


unionised
They used the waste Sulfides from the leblace Prozesse for the H2S Generation.They lit it throught pipes filled with Gyps at red hot temperature
CaSO4 + 4H2S = CaS + 4H2O + 4S.

If you use Ironsulfate it will go at roome temperature.

Weldon used an suspention of Ironoxyde or Manganoxyde and bubbled H2S and air inside.
Calciumsulfide was also made by mixing gyps and charcoal and formed briks out of it and burned it like clay briks. 1g gyps on 0,15 if it had crystall water in it and 0,2 without.
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[*] posted on 9-9-2019 at 06:50


CaSO4 and aluminum is used as a heat booster in some thermite reactions (I did this for silicon thermite). That reaction produces calcium sulfide, which reacts with water to release copious amounts of H2S. So zinc would probably also work, if you can find powdered Zn.
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Boffis
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[*] posted on 9-9-2019 at 07:53


Historically barium hydroxide was produced by the "Black ash process" where barium sulphate was reduced with coke dust and the resulting crude barium sulphide leached with hot water. Air was then drawn through the hot, filtered barium sulphide solution. Oxidation of the sulphide solution gave the desired barium hydroxide solution and a precipitate of sulphur. If carried out close to boiling point the sulphur clumps together and was easily removed by filtration. I see no reason why you couldn't do this with baked plaster of paris and charcoal instead of baryte and coke.
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[*] posted on 9-9-2019 at 08:15


Quote: Originally posted by Alkoholvergiftung  

If you use Ironsulfate it will go at roome temperature.


At room temeprature ferrous sulfate react with H2S only at basic conditions to produce FeS.

[Edited on 9-9-2019 by Bedlasky]
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[*] posted on 9-9-2019 at 16:17


Not from sulfates, but from sulfites (including the readily available "hypo", or sodium thiosulfate). This might work, but I have not seen it described before.

I remember once long ago someone challenged me to prove that carbonates have carbon in them. So I reacted some NaHCO3 with a dilute acid to produce CO2. Then I lowered a burning magnesium ribbon into the CO2. The magnesium reduced the CO2 to C, and I was left with carbon (along with magnesium oxide).

So maybe the same thing would work with SO2, which could be produced by treating sulfides (as well as the readily available "hypo" - sodium thiosulfate) with a dilute acid.

Equation would be
SO2 + 2Mg -> S + 2 MgO

The enthalpy of formation of CO2 is -394 KJ/mol, whereas for SO2 it is -297 KJ/mol. So I would guess that the SO2 would be easier to reduce than CO2. But I don't have the chemicals handy to test this myself at this time.

Certainly, the sulfur produced would be vaporized. It would likely sublime onto the walls of the container of CO2.

Probably not real practical, but the original author did mention curiosity, so thought I would chime in with this idea.

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[*] posted on 9-9-2019 at 23:16


Quote: Originally posted by hodges  
So maybe the same thing would work with SO2, which could be produced by treating sulfides (as well as the readily available "hypo" - sodium thiosulfate) with a dilute acid.


If you acidified sodium thiosulfate you'll get sulfur in solution.

S2O32-+2H+--->SO2+S+H2O

But reaction is more complex. Sulfates, polythionates and hydrogen sulfide are also formed in this reaction.
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teodor
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[*] posted on 10-9-2019 at 02:09


I am curious, is it possible to disproportionate SO42- and OH- somehow to get S2O32-? Because we have reaction like this

4S+8NaOH = Na2SO4+3Na2S+4H2O

(dry process)

and the equilibrium possible is driven by evaporation of H2O. So, if we start with Na2SO4 and Na2S (or NaOH) and H2O can we get some oxysulfate anion (between SO42- and S, like S2O32-)?
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Alkoholvergiftung
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[*] posted on 10-9-2019 at 06:44


hodges
I ve read an early production way was to bubble H2S throught H2SO3 yields immedatly fine Sulfur powder.

Bedlasky Ive searched again and it was Iron III sulfate with the Sulfid Sulfur reaction.
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teodor
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[*] posted on 10-9-2019 at 06:50


Actually there are sooo many ways to get a sulfur powder from H2S, actually when you try to get H2S sometimes you get just a sulfur powder ... Many oxidizers will work on H2S but I never saw H2S as something affordable that I can use if I have no access to sulfur.

So, I propose routes in which you mix (poly)sulfide with some oxidizer and acid and you get S directly without bothering with H2S which requires either descent equipment or huge optimism to work with.
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draculic acid69
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[*] posted on 11-9-2019 at 00:47


Trying to get elemental sulfur from sulfates sounds like a long way around to get something you can get at any hardware store.in my opinion it's a bad starting point.
And anything utilizing h2s is soooooo dangerous.so unnecessarily dangerous
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teodor
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[*] posted on 11-9-2019 at 03:16


Oh, I forgot about the most obvious route to get sulfur from sulfates. From wikipedia:

"Native sulfur is synthesised by anaerobic bacteria acting on sulfate minerals such as gypsum in salt domes."

And I think with a proper culture of bacteria making sulfur at home should be not more complex than making alcohol or bread.

Also, if you like to travel: "Elemental sulfur can be found near hot springs and volcanic regions in many parts of the world, especially along the Pacific Ring of Fire; such volcanic deposits are currently mined in Indonesia, Chile, and Japan."

So, if it will disappear from your hardware store one day I believe you know what to do :)

[Edited on 11-9-2019 by teodor]
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Alkoholvergiftung
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[*] posted on 11-9-2019 at 06:36


Ive read that the chemical factory Griesheim made Soda via Sodiumsulfate and straw and piss.The waste product was elemental sulfur If you want to go the bacterial route. :)

[Edited on 11-9-2019 by Alkoholvergiftung]
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[*] posted on 11-9-2019 at 08:57


I think sticking with a SO2 method instead of H2S is the safer and better way to do. You could generate SO2 rather consistently by hot sulfuric acid and copper on a regular hot place. Then reduce the SO2 over carbon, zinc or magnesium. sulfur should be easy to extract using xylene or toluene. It does sound laborious though.
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draculic acid69
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[*] posted on 11-9-2019 at 17:38


If you can find the actual bacteria that they use that would be the best way but how hard is it to get?is it even available to the public? A lot of companies use strains of bacteria they've spent many years breeding and modifying.
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[*] posted on 11-9-2019 at 17:56


Sodium thiosulfate plus hydrochloric acid is a simple method to produce sulphur,
but
sulphur should be available in massive quantities in any country that refines crude oil.




CAUTION : Hobby Chemist, not Professional or even Amateur
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