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otonel
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[*] posted on 24-1-2011 at 14:54
Antimony Sulfide


I can make antimony sulfide from sulfur and antimony casting pieces by melting together?
I don`t find on the internet how to make that chemicals and i need to use in priming mixture
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Xenoid
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[*] posted on 24-1-2011 at 17:21


The "black" form of Sb2S3 can be produced by heating antimony and sulphur together.
The "orange" form can be produced by bubbling H2S through an acidified solution of antimony trichloride;

2SbCl3 + 3H2S --> Sb2S3 + 6HCl

The orange form converts to the black form on heating.
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[*] posted on 13-2-2011 at 04:34


My try to make Sb2S3 by adding S to melting Sb is failed,the result was a black mixture from grey Sb and black residue of melting sulfur
Best result i have with tin sulfate making with melting process
About the method to produced by bubbling H2S is not easy for me
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[*] posted on 13-2-2011 at 11:18


Add a hot solution of sodium thiosulfate -photographer's hypo -to a hot solution of SbCl3 containing enough HCl to avoid hydrolysis. Do so with good ventilation, as H2S is formed. A dark precipitate of Sb<sub>2</sub>S<sub>3</sub> will be formed; doing the reaction at temperatures below 40to 50 C gives the red form of the sulfide, while adding too much thiosulfate dissolves some of the sulfide being formed.
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Lion850
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[*] posted on 19-11-2020 at 22:20


I had a go at making antimony sulphide more or less based on patent Patent CN102259912B

https://patents.google.com/patent/CN102259912B/en

although I must stress 'loosely' as I did not have all the exact compounds specified.

- 5.1g Sb2O3 and 18g concentrated HCl placed in a beaker, stirred and heated (patent called for Sb2O5 but I did not have any).
- Once hot (not boiling) the oxide dissolved reasonably fast, into a clear solution.
- Add 3g tartaric acid and stir till dissolved.
- Let solution cool to below 50 and then add equal volume of water. At this point the solution became cloudy, with a white ppt. I dont think this was supposed to happen, I probably added too much water or the temperature should have been lower before adding the water?
- Filter the solution, obtaining a clear filtrate and a little bit of white remainder.
- Dissolve 7g Na2S in 30ml water (patent calls for ammonium sulphide but I did not have).
- Drip the Na2S solution into the SbCl3 solution with fast stirring.
- An orange suspension quickly formed. Initially there was no H2S smell, but when about 75% of the Na2S solution was added it suddenly started to make bubbles of H2S as more was added. I assumed this was the point where all the SbCl3 was displaced and the Na2S was started to react with the excess acid, so stopped adding Na2S.
- Transfer to large beaker and add 400ml water, stir, let settle, decant, add water, stir, settle, decant.
- Transfer remainder to vacuum filter and wash again in funnel.
- In solution the volume of the remainder looked huge, not so much once filtered and recovered to a crucible.
1.jpg - 444kB

- Dry the product on a steam bath until the weight was stable. Pulverize in a mortar.
- 3.6g of soft orange-brown powder recovered. This is a yield of roughly 50% based on the initial amount of Sb2O3.
2.jpg - 369kB

Cleaning: This stuff is fine and sticks to everything. Best way I found was to wash with water, then clean with paper towel, then rinse with concentrated HCl. And get a whiff of H2S a few times as the acid reacts with the antimony sulphide.

It is mentioned online that a golden color is also achievable. I think this reaction will yield many different color shades depending on ratios, temperatures, starting materials, stirring rates etc.








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[*] posted on 20-11-2020 at 00:28


I actually think that you have a nice result. Yield probably could be a little better, but your product looks nice. I myself made Sb2S3 many times, but never took the effort to isolate it and dry it. I also purchased Sb2S3, but that is the crystalline black material. The black material is much less reactive than the orange material, that's why I made the orange compound several times as a basis for other experiments. The black crystalline solid appears to be only marginally interesting. It seems to have applications in pyrotechnics, but I don't do that and then not much remains to be done with the black material.

I do not understand why the patent calls for Sb2O5. Isn't that a mistake? Sb2O5 is oxidizing and if you dissolve that in acid, you get antimony(V) in solution, which will oxidize sulfide to free sulfur. Your product then will be strongly contaminated with sulfur. So, you did the right thing to start with Sb2O3. Btw., I have some Sb2O5, and this stuff is MUCH more inert than Sb2O3. Dissolving even a tiny bit of this compound in conc. HCl takes ages, even when boiling and fuming you workspace with HCl.





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Lion850
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[*] posted on 20-11-2020 at 01:16


Woelen thanks for your comments. The patent also says the product is antimony pentasulphide (Sb2S5) which may be why they are starting with the pentaoxide?

What is the purpose of adding tartaric acid, is that to keep the pH low and prevent hydrolysis of the SbCl3?
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[*] posted on 20-11-2020 at 02:02


The patent still looks strange to me. Whether Sb2S5 is a real compound or a very intimate mix of Sb2S3 and S seems to be still a subject of debate. Sb2S5 is orange, just like Sb2S3. I actually do have some orange Sb2S5, just as a lab curiousity, and I keep it around as a display sample.

Tartrate ion forms a very specific complex ion with antimony. Sb(3+) entities are coordinated to tartrate ions in this complex, with the H-atoms stripped off from the hydroxyl groups. This complex increases the solubility of antimony in water and makes hydrolysis less of a problem. The potassium salt of this complex is available commercially. It is a very strong emetic and still is used for this purpose in some cases.

Look at this beautiful official IUPAC name for this commercially available salt:

:P dipotassium 3,6,10,13-tetraoxo-2,7,9,14,15,16,17,18-octaoxa-1,8-distibapentacyclo[10.2.1.1¹,⁴.1⁵,⁸.1⁸,¹¹]octadecane-1,8-diuide

A little more info can be found here: https://en.wikipedia.org/wiki/Antimony_potassium_tartrate




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joseph6355
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[*] posted on 28-5-2022 at 09:55


Any recommendations for synthesizing Antimony Sulfide from elementar Antimony?
I'm thinking of welding steel bar stock in a cube shape, filling it with Sulfur and Antimony and heating it to 750°C-ish. Regarding this method, I've got two questions:
1. Antimony Sulfide reacts with oxidizers under heat. Wouldn't such mixture rupture the container when it reacted upon heating?
2. If so -- and to prevent that -- I could top up the containing with an additional excess of Sulfur and compress it prior to welding in order to leave little to no air inside. But upon heating wouldn't the mixture expand or something and cause the same problem?

Last thing I want is to breathe in a toxic cloud of Antimony. I'm too young to have cancer :D.

[Edited on 28/5/22 by joseph6355]




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[*] posted on 29-5-2022 at 02:45


I'm fairly sure that Sb2S3 will react with steel.
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joseph6355
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[*] posted on 1-6-2022 at 16:27


Quote: Originally posted by unionised  
I'm fairly sure that Sb2S3 will react with steel.

How could one make Sb2S3 from Sb and Sulfur then? It has to be heated inside of something that can withstand those temperatures, right?




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clearly_not_atara
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[*] posted on 1-6-2022 at 16:56


Sulfur reacts at high temperatures with every metal except gold. So you would need something that forms a passivating layer, because inertness to sulfur ain't happening. You also need a flow process, because sulfur at 750 C has a vapor pressure of dozens of atmospheres. Oh, and the reaction is reversible, so you'll want finely divided antimony. Oh, and be sure to contain the exhaust with good cooling, because sulfur's autoignition temperature is just 260 C. I think you could use alumina ceramic components with gold "solder".

This sounds very hard. Are you sure you wouldn't rather react the antimony with chlorine and use the easy method? I honestly cannot think of a single reaction conventionally performed using sulfur gas.




[Edited on 04-20-1969 by clearly_not_atara]
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SplendidAcylation
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[*] posted on 2-6-2022 at 03:07


Quote: Originally posted by clearly_not_atara  
I honestly cannot think of a single reaction conventionally performed using sulfur gas.



There's always the old preparation of carbon disulfide! :P

P.S. where did you get your time machine?
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