Prepn process of germanium dioxide powder

A germanium dioxide and powder technology is applied in the field of preparation of inorganic catalysts, which can solve problems such as agglomeration, difficult hydrolysis process, bonding growth, etc., and achieve the effects of reducing content, avoiding agglomeration, and promoting rapid progress.

Inactive Publication Date: 2007-11-07
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the use of stirring paddles in the hydrolysis process, insufficient stirring often leads to the difficulty of completely carrying out the hydrolysis process, and a small amount of GeCl 4 wrapped in GeO 2 powder, meanwhile, the GeO produced by hydrolysis 2 The powder will appear agglomeration, cohesion and growth

Method used

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  • Prepn process of germanium dioxide powder
  • Prepn process of germanium dioxide powder
  • Prepn process of germanium dioxide powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] high purity GeCl 4 solution, GeCl by volume 4 :H 2 Slowly add O=1:9 ratio to electronic grade deionized water for hydrolysis, and feed while stirring. The feeding speed is 30ml / min; the stirring speed is 1000 rpm; the hydrolysis process temperature is controlled at 10°C; after the feeding is completed, the stirring paddle continues to stir, the stirring speed is 800 rpm, the ultrasonic oscillation frequency is 40KHz, the oscillation power is 100W, and the time is 20min; 2 The particles were washed with water and dried at 180°C for 8 hours to obtain GeO with a central particle size of 5 μm. 2 powder.

Embodiment 2

[0018] high purity GeCl 4 solution, GeCl by volume 4 :H 2 Slowly add O=1:7 ratio to electronic grade deionized water for hydrolysis, and feed while stirring. The feeding speed is 30ml / min; 10°C; after the feeding is completed, the stirring paddle continues to stir, the stirring speed is 800 rpm, the ultrasonic oscillation frequency is 40KHz, the oscillation power is 50W, and the time is 30min; 2 The particles were washed with water and dried at 180°C for 8 hours to obtain GeO with a central particle size of 6 μm. 2 powder.

Embodiment 3

[0020] high purity GeCl 4 solution, GeCl by volume 4 :H 2 The ratio of O=1:7.5 is slowly added to electronic grade deionized water for hydrolysis, while stirring, the feeding speed is 50ml / min; the stirring speed is 1000 rpm; the temperature of the hydrolysis process is controlled at 5°C; after feeding, the stirring paddle continued to stir, the stirring speed was 700 rpm, the ultrasonic oscillation frequency was 40KHz, the oscillation power was 80W, and the time was 20min; 2 The particles were washed with water and dried at 180°C for 8 hours to obtain GeO with a central particle size of 6 μm. 2 powder.

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Abstract

The preparation process of small size GeO2 powder includes the following steps: adding high purity GeCl4 solution in the volume ratio between GeCl4 and H2O of 1 to 5-9 into electronic level deionized water to hydrolyze in the addition speed of 30-150 ml/min while stirring in 500-1400 rpm to react at 0-15 deg.c; further stirring in 500-1000 rpm after finishing addition for 15-30 min while ultrasonic vibration in the frequency of 40 KHz and power of 50-100 W; washing produced GeO2 particle with electronic level deionized water and stoving at 150-180 deg.c to obtain small size GeO2 powder.

Description

technical field [0001] The present invention relates to the preparation of a kind of inorganic catalyst, particularly a kind of germanium dioxide (GeO 2 ) powder preparation method. Background technique [0002] original GeO 2 The powder is mainly used to reduce Ge metal, so there is no special requirement for its particle size. GeO produced by existing processes 2 The powder particles are relatively large, generally around 30 μm. Due to the use of stirring paddles in the hydrolysis process, insufficient stirring often leads to the difficulty of completely carrying out the hydrolysis process, and a small amount of GeCl 4 wrapped in GeO 2 powder, meanwhile, the GeO produced by hydrolysis 2 Powder will appear agglomeration, cohesion growth phenomenon. GeO obtained by laser particle size analyzer 2 The powder particles are about 30μm, and the <10μm particles are about 30%. [0003] With the development of society, GeO 2 The catalytic performance of GeO has been rap...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G17/02B01J23/14
Inventor 方峰蒋建清邵起越董岩涂益友夏兰
Owner SOUTHEAST UNIV
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