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Method for synthesizing titanium disulfide by mechanical ball milling

A technology of titanium disulfide and synthesis method, which is applied in the fields of titanium sulfide, chemical instruments and methods, inorganic chemistry, etc., which can solve the problems of low safety, danger, and time-consuming preparation, and achieve the effect of high operational safety

Pending 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

The above methods have the disadvantages of slow reaction rate and low safety.
[0003] Titanium disulfide can be used as a negative electrode material in lithium batteries. It takes a long time to prepare under high temperature conditions and has certain risks. Therefore, it is necessary to develop a simple, efficient and safe synthesis method.

Method used

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  • Method for synthesizing titanium disulfide by mechanical ball milling

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] The lithium sulfide was dried in a vacuum oven at 100 °C for 12 h. Under the protection of an argon atmosphere, uniformly mix 0.65g of lithium sulfide and 0.78ml of titanium tetrachloride into a ball mill jar. The ratio of the total weight of grinding balls to the total weight of materials is 30:1. Under room temperature conditions, the ball milling tank was continuously ball-milled at a speed of 400r / min for 8 hours, and the obtained mixture of titanium disulfide and lithium chloride was then added with ethanol to wash and filter to separate the titanium disulfide, and after washing with water, put it in Titanium disulfide can be obtained after drying in an oven at 80°C. The XRD figure of embodiment 1 reaction generation product is as figure 1 shown.

Embodiment 2

[0026] Lithium sulfide was dried in a vacuum oven at 80 °C for 24 h. Under the protection of an argon atmosphere, uniformly mix 0.65g of lithium sulfide and 0.78ml of titanium tetrachloride into a ball mill jar. The ratio of the total weight of grinding balls to the total weight of materials is 50:1. Under room temperature conditions, the ball milling tank was continuously ball-milled at a speed of 350r / min for 12 hours to obtain a mixture of titanium disulfide and lithium chloride, and then the excess titanium tetrachloride was recovered by distillation, and finally ethanol was added to wash and filter the titanium disulfide It is separated, washed with water, and dried in an oven at 90°C to obtain titanium disulfide.

Embodiment 3

[0028] The lithium sulfide was dried in a vacuum oven at 70 °C for 36 h. Under the protection of an argon atmosphere, 0.65g of lithium sulfide and 1.56ml of titanium tetrachloride were uniformly mixed and added into a ball mill jar. The ratio of the total weight of grinding balls to the total weight of materials is 60:1. Under room temperature conditions, the ball milling tank was continuously ball-milled at a speed of 500r / min for 36 hours to obtain a mixture of titanium disulfide and lithium chloride, and then the excess titanium tetrachloride was recovered by distillation, and finally ethanol was added to wash and filter the titanium disulfide It is separated, washed with water, and dried in an oven at 85°C to obtain titanium disulfide.

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Abstract

The invention discloses a method for synthesizing titanium disulfide by mechanical ball milling. The titanium disulfide is prepared from the steps that titanium tetrachloride and lithium sulfide are used as raw materials, titanium disulfide powder and titanium tetrachloride are added to a sealed ball milling tank according to a certain ratio under inert gas shielding, operation is performed for aperiod time in a certain rotating speed at a room temperature, after the ball milling reaction is completed, a removed mixture is distilled, filtered, washed and dried, and the titanium disulfide is obtained. The method is simple in process and high in safety.

Description

technical field [0001] The invention belongs to the field of material synthesis, and in particular relates to a method for synthesizing titanium disulfide by mechanical ball milling. Background technique [0002] Titanium disulfide is a metallic conductor with a layered structure, and it is easy to intercalate metal lithium, so titanium disulfide can be used as an ideal electrode material in batteries, or replace graphite as a catalyst for the reaction between alkali metal or alkaline earth metal elements. container material. At present, the methods for preparing titanium disulfide mainly include: (1) using the iodine transport method to synthesize and grow titanium disulfide crystals by using a three-temperature zone process, [Tang Houshun, preparation of a layered material titanium disulfide single crystal. Fudan University, 1982]; (2) pass the hydrogen sulfide of dry bath into the α-chloronaphthalene solution of boiling titanium tetrachloride, make hydrogen sulfide and t...

Claims

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Application Information

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IPC IPC(8): C01G23/00
CPCC01G23/007C01P2002/72
Inventor 梁初孙鑫曾称福夏阳张俊黄辉张文魁甘永平
Owner ZHEJIANG UNIV OF TECH
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