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Synthesis method of silicon disulfide powder

A synthesis method and technology of silicon sulfide, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems of low efficiency, high cost, and difficulty in realizing industrialized production, and achieve environmental friendliness, low cost, and easy industrialization implementation. Effect

Inactive Publication Date: 2019-12-03
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to be heated at high temperature, the efficiency is low, the cost is high, and it is difficult to realize industrial production

Method used

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  • Synthesis method of silicon disulfide powder

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Effect test

Embodiment 1

[0025] Under the protection of a nitrogen atmosphere, lithium sulfide and silicon tetrachloride were uniformly mixed at a molar ratio of 2:1, transferred to a reactor and sealed. Heat to 140°C at a heating rate of 2°C / min, and keep the temperature for 5h. After the reaction was completed, the temperature was lowered to room temperature, and excess silicon tetrachloride was recovered by distillation at 100°C. Add the solid product in the reactor to benzene, through solid-liquid separation, obtain a benzene solution containing silicon sulfide, recover benzene by distillation at 120°C, and dry the solid in it at 100°C to obtain silicon sulfide powder . figure 1 The X-ray diffraction pattern of its product can only characterize the X-ray pattern of lithium chloride. According to the law of conservation of materials, there must be silicon sulfide in the product.

Embodiment 2

[0027] Under the protection of an argon atmosphere, lithium sulfide and silicon tetrachloride were evenly mixed at a molar ratio of 1:1, transferred to a reactor and sealed. Heat to 100°C at a heating rate of 0.5°C / min, and hold for 100h. After the reaction was completed, the temperature was lowered to room temperature, and excess silicon tetrachloride was recovered by distillation at 60°C. Add the solid product in the reactor to benzene, through solid-liquid separation, obtain a benzene solution containing silicon sulfide, recover benzene by distillation at 85°C, and dry the solid in it at 100°C to obtain silicon sulfide powder .

Embodiment 3

[0029] Under the protection of a nitrogen atmosphere, lithium sulfide and silicon tetrachloride were uniformly mixed at a molar ratio of 2:3, transferred to a reactor and sealed. Heat to 300°C at a heating rate of 20°C / min, and hold for 1h. After the reaction was completed, the temperature was lowered to room temperature, and excess silicon tetrachloride was recovered by distillation at 80°C. Add the solid product in the reactor to benzene, through solid-liquid separation, obtain a benzene solution containing silicon sulfide, recover benzene by distillation at 90°C, and dry the solid in it at 100°C to obtain silicon sulfide powder .

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Abstract

The invention discloses a synthesis method of silicon disulfide powder. The synthesis method comprises the following steps: (1) under protection of an inert atmosphere, lithium sulfide and silicon tetrachloride are uniformly mixed and transferred to a reactor, and sealing is performed; (2) the mixture in the reactor is heated and a reaction is carried out for a certain period of time under heat preservation conditions; (3) after the reaction is completed, the temperature is reduced to room temperature, and an excess of silicon tetrachloride is recovered; and (4) the solid product is separatedby using a solvent to obtain the silicon disulfide powder. The synthesis method of the silicon sulfide powder has the characteristics of simple process, low cost, and easy industrialization production.

Description

technical field [0001] The invention belongs to the technical field of material synthesis, and in particular relates to a method for synthesizing silicon sulfide powder. Background technique [0002] Silicon sulfide is an inorganic compound with the chemical formula SiS 2 , belonging to the orthorhombic or tetragonal crystal system, stable at normal temperature and pressure, and decomposed into SiO when exposed to moisture 2 and H 2 S. At present, there are few synthetic methods related to silicon sulfide. Japanese patent (publication No. JPS62252310A) discloses a method for obtaining silicon sulfide by reacting sulfur vapor or hydrogen sulfide gas with boiling silica. This method requires high-temperature heating, which has low efficiency and high cost, and is difficult to realize industrialized production. Therefore, it is of great significance to develop a new, efficient and environmentally friendly synthesis method for silicon sulfide. Contents of the invention ...

Claims

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Application Information

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IPC IPC(8): C01B33/00
CPCC01B33/00C01P2002/72
Inventor 梁初潘良斌王俊豪黄辉张文魁甘永平夏阳张俊
Owner ZHEJIANG UNIV OF TECH
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