Method for preparing lithium phosphate powder

A lithium phosphide and powder technology is applied in the field of preparing lithium phosphide powder, which can solve the problems of low product purity, poor batch performance, and difficulty in realizing industrialized production, and achieve the effect of high purity and good product batches.

Active Publication Date: 2015-05-20
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This type of method requires high temperature heat treatment, high energy consumption, and the product has disadvantages such as low purity and poor batch quality, making it difficult to realize industrial production

Method used

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  • Method for preparing lithium phosphate powder

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Experimental program
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Effect test

Embodiment 1

[0026] The red phosphorus powder was dried in a vacuum oven at 80°C for 6h. Under the protection of an argon atmosphere, 0.31 g of red phosphorus powder and 0.24 g of lithium hydride powder 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 40:1. Under the condition of 25° C., the ball milling tank was continuously ball milled at a speed of 500 r / min for 32 hours, and the obtained powder was lithium phosphide powder. figure 1 Its corresponding XRD diffraction pattern, compared with the standard card, shows that the obtained product is pure phase lithium phosphide, and no other impurities exist.

Embodiment 2

[0028] The red phosphorus powder was dried in a vacuum oven at 60°C for 10 h. Under the protection of nitrogen atmosphere, 4.6g of red phosphorus powder and 2.6g of lithium hydride powder were uniformly mixed and then added to the 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 80:1. Under the condition of 48° C., the ball milling tank was continuously ball milled at a speed of 450 r / min for 24 hours, and the obtained powder was lithium phosphide powder.

Embodiment 3

[0030] Dry the white phosphorous powder in a vacuum oven at 75°C for 12 hours. Under the protection of an argon atmosphere, 3.1 g of white phosphorus powder and 2.8 g of lithium hydride powder 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 60° C., the ball mill jar was continuously ball milled at a speed of 500 r / min for 32 hours, and the obtained powder was lithium phosphide powder.

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Abstract

The invention discloses a method for preparing lithium phosphate powder. The method comprises the following steps: (1) drying phosphorus powder; (2) mixing the dried phosphorus powder and lithium hydride according to a molar ratio of 1:(2-4) under inert atmosphere protection, adding the mixed powder into a sealed ball-milling tank, and performing ball milling for 2-48 hours under the conditions of the temperature of 0-60 DEG C and the rotating speed of 100-500 revolutions per minute; and (3) taking out the powder from the ball-milling tank under an inert atmosphere after the ball-milling reaction is ended, thereby obtaining the lithium phosphate powder. The method for preparing the lithium phosphate powder disclosed by the invention has the characteristics of simple process, low cost and simplicity in industrial production.

Description

(1) Technical field [0001] The invention relates to a method for preparing lithium phosphide powder. (2) Background technology [0002] Lithium phosphide is a reddish-brown inorganic compound with the chemical formula Li 3 P, belongs to the hexagonal crystal system, Na 3 As structure with a density of 1.43g cm -3 (298K), easily deliquescent in the air, reacts with water to form PH 3 . At present, there are few preparation methods for lithium phosphide, and the most common preparation method is to use vacuum or protective atmosphere (commonly used H 2 , CO as the carrier gas), the metal lithium powder and red phosphorus powder or phosphorus vapor are directly combined under high temperature heating conditions. This type of method requires high-temperature heat treatment, consumes a lot of energy, and has the disadvantages of low purity and poor batchability of the product, making it difficult to realize industrial production. (3) Contents of the invention [0003] The...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/08
CPCC01B25/08
Inventor 夏阳方如意梁初张文魁黄辉陶新永甘永平
Owner ZHEJIANG UNIV OF TECH
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