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Mechanical ball milling synthesis method of phosphorus pentasulfide powder

A technology of phosphorus pentasulfide and phosphorus pentachloride, which is applied in the direction of phosphorus sulfur/selenium/tellurium phosphorus compounds, can solve the problems of low product quality, complicated preparation process, and high energy consumption, and achieve low cost, efficient synthesis method, and environmental protection. friendly effect

Active 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 existing synthesis process of phosphorus pentasulfide has defects such as complex preparation process, low product quality and high energy consumption. Therefore, it is of great significance to develop a new, efficient and environmentally friendly synthesis method of phosphorus pentasulfide

Method used

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  • Mechanical ball milling synthesis method of phosphorus pentasulfide powder

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Comparison scheme
Effect test

Embodiment 1

[0026] Under the protection of an argon atmosphere, 0.75g of lithium sulfide powder and 1.32g of phosphorus pentachloride were evenly mixed and then added to a ball mill jar. Then put the balls into the ball mill jar and seal it. The ratio of the total mass of grinding balls to the total mass of materials is 40:1. Under the condition of room temperature, the ball mill jar was continuously ball milled at a speed of 500 r / min for 24 hours. After the reaction, under an argon atmosphere, the solid product in the ball mill tank was taken out and added to toluene for solid-liquid separation, and the separated solution was distilled at 150°C to recover liquid toluene and solid phosphorus pentachloride. Add the remaining solid into acetone, separate the solid from the liquid, and dry the solid at 80°C to obtain phosphorus pentasulfide powder. figure 1 The X-ray diffraction pattern of its product can only characterize the X-ray spectrum of lithium chloride. According to the law of co...

Embodiment 2

[0028] Under the protection of an argon atmosphere, 1.78g of lithium sulfide powder and 4.9g of phosphorus pentachloride were uniformly mixed and then added to a ball mill jar. Then put the balls into the ball mill jar and seal it. The ratio of the total mass of grinding balls to the total mass of materials is 60:1. Under the condition of room temperature, the ball mill jar was continuously ball milled at a speed of 100 r / min for 100 h. After the reaction, under an argon atmosphere, the solid product in the ball mill tank was taken out and added to toluene for solid-liquid separation, and the separated solution was distilled at 110°C to recover liquid toluene and solid phosphorus pentachloride. Add the remaining solid to acetone, separate the solid from the liquid, and dry the solid at 80°C to obtain phosphorus pentasulfide powder

Embodiment 3

[0030] Under the protection of an argon atmosphere, 0.37g of lithium sulfide powder and 1.3g of phosphorus pentachloride were uniformly mixed and then added to a ball mill jar. Then put the balls into the ball mill jar and seal it. The ratio of the total mass of grinding balls to the total mass of materials is 20:1. Under room temperature conditions, the ball milling tank was continuously ball milled at a speed of 300 r / min for 100 h. After the reaction, under an argon atmosphere, the solid product in the ball mill tank was taken out and added to toluene for solid-liquid separation, and the separated solution was distilled at 120°C to recover liquid toluene and solid phosphorus pentachloride. Add the remaining solid into acetone, separate the solid from the liquid, and dry the solid at 80°C to obtain phosphorus pentasulfide powder.

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Abstract

The invention discloses a mechanical ball milling synthesis method of phosphorus pentasulfide powder. The preparation method comprises the following steps: (1) adding phosphorus pentachloride and lithium sulfide powder into a sealed ball milling tank under protection of an inert atmosphere; (2) mounting the ball milling tank onto a ball mill at room temperature, and carrying out a ball milling reaction at a certain rotation speed for a certain time; (3) taking out the solid product from the ball milling tank under an inert atmosphere after the reaction is completed, and recovering excess phosphorus pentachloride; and (4) separating the remaining solid product to obtain the phosphorus pentasulfide powder. The preparation method of the phosphorus pentasulfide powder has the characteristics of simple process, low cost, and easy industrial production.

Description

technical field [0001] The invention belongs to the field of material synthesis and relates to a method for synthesizing phosphorus pentasulfide powder by mechanical ball milling. Background technique [0002] Phosphorus pentasulfide is an inorganic compound with the chemical formula P 2 S 5 , is a yellow and yellow-green crystalline substance, stable when dry, but easily hydrolyzed into phosphoric acid and hydrogen sulfide when exposed to water. With the development of automobile, petroleum, pharmaceutical and other industries, the demand for high-quality phosphorus pentasulfide powder is increasing year by year. The synthetic method of existing phosphorus pentasulfide mainly is a liquid phase method (Li Gang, the preparation method of phosphorus pentasulfide), and liquid elemental sulfur (sulfur) and phosphorus (yellow phosphorus) are fed into the reactor by stoichiometry to react, and the reaction product obtained is passed through Purify by distillation, and then cool...

Claims

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Application Information

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IPC IPC(8): C01B25/14
CPCC01B25/14
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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