Exploration of metal sulfide syntheses and the dissolution process of antimony sulfide in phosphonium-based ionic liquids

Ionic liquids (ILs), especially task-specific ILs, are capable of dissolving various solids at moderate temperatures without the need for special reaction vessels. Direct synthesis of binary sulfides of B, Bi, Ge, Mo, Cu, Au, Sn, In, Ti, V, Fe, Co, Ga, Ni, Al, Zn, and Sb in [P 66614 ]Cl was tested a...

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Published in:Dalton transactions : an international journal of inorganic chemistry 2022-03, Vol.51 (1), p.479-486
Main Authors: Grasser, Matthias A, Pietsch, Tobias, Brunner, Eike, Ruck, Michael
Format: Article
Language:English
Subjects:
Aluminum
Amorphous materials
Antimony
Chemical synthesis
Copper
Copper sulfides
Crystallization
Dissolution
Germanium
Gold
Hydrogen sulfide
Ionic liquids
Ions
Iron
Melting points
Molybdenum
Nickel sulfide
Tin
Titanium
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Summary:Ionic liquids (ILs), especially task-specific ILs, are capable of dissolving various solids at moderate temperatures without the need for special reaction vessels. Direct synthesis of binary sulfides of B, Bi, Ge, Mo, Cu, Au, Sn, In, Ti, V, Fe, Co, Ga, Ni, Al, Zn, and Sb in [P 66614 ]Cl was tested at 100 °C, i.e. below the melting point of sulfur. Under these conditions, substantial sulfide formation occurred only for nickel (Ni 3 S 4 , Ni 3 S 2 , NiS) and copper (Cu 2 S, CuS). Sb showed no formation of crystalline sulfide, but after addition of EtOH, an orange material precipitated which was identified as amorphous metastibnite. Subsequently, the dissolution of antimony sulfide (Sb 2 S 3 ), the main source of antimony production, in the phosphonium-based ILs [P 66614 ][OAc] and [P 66614 ]Cl at 100 °C was studied in detail. The dissolution proceeds without H 2 S evolution, and amorphous Sb 2 S 3 can be precipitated from these solutions. Heating Sb 2 S 3 in the Lewis-acidic IL [BMIm]Cl·4.7AlCl 3 led to the crystallization of [Sb 13 S 16 Cl 2 ][AlCl 4 ] 5 , which contains a new quadruple heterocubane cation. Antimony sulfide (Sb 2 S 3 ) can be dissolved in phosphonium-based ionic liquids (ILs) and re-precipitated in amorphous form. The reaction with a Lewis-acidic imidazolium-based IL results in the formation of quadruple-heterocubane cluster cations.
ISSN:1477-9226
1477-9234
DOI:10.1039/d1dt04165g