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A kind of method for synthesizing metal sulfide by carbothermal reaction

A metal sulfide, carbothermal reaction technology, applied in the preparation of sulfide/polysulfide, aluminum sulfur compounds, chemical instruments and methods, etc., can solve harsh experimental conditions, difficult to achieve large-scale realization, titanium tetrachloride Difficulties and other problems, to achieve the effect of short process flow and simple process

Active Publication Date: 2022-07-19
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method avoids the use of hydrogen sulfide gas, but operational difficulties with titanium tetrachloride remain
[0005] It can be seen that the current preparation methods of titanium sulfide are either expensive in raw material sources, or harsh in experimental conditions, or difficult to realize on a large scale
Moreover, the same difficulty generally exists in the preparation of a large number of metal sulfides such as Zr, Ta, Nb, etc.

Method used

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  • A kind of method for synthesizing metal sulfide by carbothermal reaction
  • A kind of method for synthesizing metal sulfide by carbothermal reaction
  • A kind of method for synthesizing metal sulfide by carbothermal reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) According to titanium dioxide (with TiO 2 Calculated) / activated carbon (calculated by C / ) sublimated sulfur (calculated by S) weigh about 30g of the mixture according to the material ratio of 1:2:2.2, take ethanol as a dispersant, mix by ball milling and dry it for later use.

[0034] (2) Take 1-5g of the mixed powder and press it into a cylindrical test piece with a mold with a diameter of 20cm under a pressure of 20Mpa, and then put the pressed test piece into a corundum tube and vacuum seal. The sealed reactor was placed in a vertical muffle furnace, the temperature was raised to 1000° C. for 20 hours, and cooled with the furnace to obtain titanium sulfide.

Embodiment 2

[0036] (1) Titanium dioxide (with TiO 2 Calculate) / activated carbon (calculated by C / ) sublimation sulfur (calculated by S) weigh 13.39g of titanium dioxide, 4.02g of activated carbon, 12.59g of sublimated sulfur according to the mass ratio of 1:2.1:2.35, take ethanol as a dispersant, pass After mixing by ball milling, dry for use.

[0037] (2) Take 1-5g of the mixed powder and press it into a cylindrical test piece with a mold with a diameter of 20cm under a pressure of 20Mpa, and then put the pressed test piece into a corundum tube and vacuum seal. The sealed reactor was placed in a vertical muffle furnace, and the temperature was raised to 1200° C. for 10 hours, followed by cooling in the furnace to obtain titanium sulfide.

[0038] The titanium dioxide and the product obtained in step (2) are respectively subjected to XRD detection, and the obtained diffraction pattern is as follows: figure 1 and 2 It is shown that the product obtained by the reaction is titanium sulfid...

Embodiment 3

[0040] (1) Al2O3 (with Al 2 O 3 Calculate) / activated carbon (calculated by C / ) sublimation sulfur (calculated by S) weigh 12.34g of aluminum oxide, 4.5g of activated carbon, 13.16g of sublimated sulfur according to the mass ratio of substances 1:3.1:3.4, take ethanol as The dispersant is mixed by ball milling and dried for later use.

[0041] (2) Take 1-5g of the mixed powder and press it into a cylindrical test piece with a mold with a diameter of 20cm under a pressure of 20Mpa, and then put the pressed test piece into a corundum tube and vacuum seal. The sealed reactor was placed in a vertical muffle furnace, and the temperature was raised to 1650° C. for 10 hours, followed by cooling in the furnace to obtain aluminum sulfide.

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Abstract

The invention discloses a method for synthesizing the sulfide of metal M by carbothermal reaction, wherein M is Ti, Zr, Hf, Cr, Mo, W, V, Nb, Ta, Fe, Co, Ni, Mn, Cu, Zn, Si, Ge, Pb, Sn, Ag, Au, Pt, Pd, Rh, Ir, Ru, Os, Re, Al, B, Ga, In, Tl, Sc, Y, U, One or more of lanthanide series and actinide series. The metal oxide is uniformly mixed with carbon and sulfur in a certain proportion, and the mixture is reacted in a high temperature vacuum environment to prepare the solid sulfide of metal M. The method starts from metal oxides, the raw materials used are cheap and easy to obtain, the production process is simple, safe and feasible, and the reaction speed is fast, which provides a new method for mass production of metal sulfides.

Description

technical field [0001] The invention relates to a method for synthesizing metal sulfides based on carbothermal reaction, and belongs to the technical field of material preparation. Background technique [0002] Metal sulfides have many special properties and uses, but except for a few metal sulfides that have natural mineral resources, most metal sulfides need to be artificially synthesized. The existing forms of these metals in nature are mainly oxides. Since the combining ability of sulfur and metals is often weaker than that of oxygen, the traditional methods for preparing metal sulfides of metal sulfides are often complicated and expensive. The following is a brief introduction to the synthesis of titanium sulfide. [0003] In the early stage of synthesis of titanium sulfide, the direct chemical method or vapor deposition method was used. For example, in the patent U.S. Pat. No. 4,007,055, British Pat. Sulfur is used as a raw material, and titanium sulfide is prepared ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/20C01F7/70C01G23/00
CPCC01B17/20C01G23/007C01F7/70C01P2002/72C01P2004/03
Inventor 金先波谭明胜王志勇吴长胜
Owner WUHAN UNIV
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