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A method for synthesizing metal sulfides by gas/molten salt interfacial reaction

A metal sulfide and interfacial reaction technology, applied in chemical instruments and methods, tantalum compounds, titanium compounds, etc., can solve the problem of lack of batch preparation methods for large-sized flake materials, and achieve safe and feasible production processes, high yields, and raw materials. cheap effect

Active Publication Date: 2016-03-30
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is also a lack of batch preparation methods for such large-scale flake materials.

Method used

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  • A method for synthesizing metal sulfides by gas/molten salt interfacial reaction
  • A method for synthesizing metal sulfides by gas/molten salt interfacial reaction
  • A method for synthesizing metal sulfides by gas/molten salt interfacial reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) analyze soda ash metal chloride in 300 DEG C of pre-drying, take by weighing NaCl7.2g after drying and KCl9.1g as molten salt medium, mix; Add 3.2g anhydrous sodium sulfide and mix and put into graphite crucible; Put the graphite crucible into the figure 1 In the shown quartz container, protect by argon, raise the reaction temperature at 2°C / min to 300°C for 2 hours, then raise the temperature to 500°C at 2°C / min and keep it for 2 hours, and finally increase the reaction temperature at 3°C C / min rises to 700 DEG C of reaction temperature, imports titanium tetrachloride 3.9g by high-purity Ar gas flow, and the reaction times is 5h;

[0036] (2) Cool the quartz container to room temperature, add secondary water to soak and filter, and the obtained solid is washed with acetic acid (2mol / L), washed with water, filtered, and dried in vacuum to obtain a golden yellow titanium disulfide product.

Embodiment 2

[0038] (1) Analysis of soda alkali metal chlorides is pre-dried at 300°C, and takes by weighing dried NaCl7.9g and KCl10g as a molten salt medium, and mixes; add 3.5g of anhydrous sodium sulfide and mix and put it into a graphite crucible; crucible into the figure 1 In the shown quartz tube reactor, the argon protection is applied, the reaction temperature is raised to 300°C at 2°C / min and kept for 2h, then raised to 500°C at 2°C / min and kept at 2h, and finally with 3 DEG C / min rises to 750 DEG C of reaction temperature, imports titanium tetrachloride 4.3g by high-purity Ar air flow, and the reaction times is 5h;

[0039] (2) Cool the quartz tube reactor to room temperature, add secondary water to soak and filter, and the obtained solid is washed with acetic acid (2mol / L), washed with water, filtered, and vacuum-dried to obtain a golden yellow titanium disulfide product.

Embodiment 3

[0041] (1) Analysis of soda alkali metal chloride is pre-dried at 300°C, takes by weighing dried NaCl45g and KCl57g as molten salt medium, and mixes; add 20g of anhydrous sodium sulfide and mix and put it into a graphite crucible; put the graphite crucible into Such as figure 1 In the shown quartz container, protect by argon, raise the reaction temperature at 2°C / min to 300°C for 2 hours, then raise the temperature to 500°C at 2°C / min and keep it for 2 hours, and finally increase the reaction temperature at 3°C C / min rises to 800°C of reaction temperature, imports titanium tetrachloride 24.5g by high-purity Ar gas flow, and the reaction times is 8h;

[0042] (2) Cool the quartz container to room temperature, add secondary water to soak and filter, and the obtained solid is washed with acetic acid (2mol / L), washed with water, filtered, and dried in vacuum to obtain a golden yellow titanium disulfide product.

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Abstract

The invention discloses a method for synthesizing metal sulfide by a gas / molten salt interface reaction. The method comprises the following steps: adding soluble metal sulfide M1S which serves as a raw material in an alkali chloride or fluoride molten salt medium, uniformly mixing, and putting the mixture in a closed reactor A; heating until solid is completely molten in inert gas protection, introducing a halide gas of metal M at 500-1000 DEG C above the liquid surface, carrying out a gas / molten salt interface reaction on the halide gas of metal M with M1S so as to prepare a solid-state sulfide of the metal M, wherein M is Ti, Zr, V, Nb and Ta. The interface reaction is beneficial to generation of flaked sulfide of the metal M, the generated flaked sulfide constantly sinks due to density difference, so that the reaction is carried out constantly. Raw materials used in the method are low in price and easily available, the production process is simple, safe and feasible, and the reaction speed is high, so that a novel method is provided to massive production of metal sulfide, especially laminar metal sulfide.

Description

technical field [0001] The invention relates to a method for synthesizing metal sulfides based on a gas / molten salt interface reaction, belonging to the technical field of material preparation. technical background [0002] Titanium disulfide (TiS 2 ) is a typical transition metal dichalcogenide, which is an n-type semiconductor with little metalloid properties and is stable in air at room temperature. TiS 2 With hexagonal close-packed CdI 2 structure, six S atoms in each unit cell form an octahedron, and Ti is located in the center of the octahedron, forming a TiS 6 Octahedrons, which are combined by covalent bonds; S-Ti-S "sandwich" layered structural units formed in the c direction. Titanium disulfide is composed of S-Ti-S unit sheets combined by weak van der Waals force, so it is easy to peel off to obtain a single-layer or superstructure. [0003] TiS 2 The layered structure makes it have many unique properties, such as: similar to graphite, TiS 2 It can be used ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G1/12C01G23/00C01G35/00
Inventor 金先波谭明胜王志勇
Owner WUHAN UNIV