Preparation method for high-purity alumina

A kind of alumina, high-purity technology, applied in the field of high-purity alumina preparation, can solve the problems of insufficient purity of alumina powder, easy blockage of pipelines, difficult transportation, etc., to reduce preparation costs, good working conditions, and preparation The effect of simple process

Inactive Publication Date: 2012-06-13
DALIAN JIAOTONG UNIVERSITY
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  • Abstract
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Problems solved by technology

[0004] At present, there are two main methods for preparing high-purity alumina in my country. One is the thermal decomposition method of aluminum carbonate amine. The purity of alumina powder prepared by this method cannot reach the level of 5N. The other method is to use aluminum isopropoxide Alumina powder is prepared by hydrolysis. Although this method can obtain very high-purity powder, aluminum isopropoxide solidifies at room temperature during the preparation process, and it is easy to block the pipeline during operation and difficult to transport. It needs to be hydrolyzed at a temperature above 80°C Hydrolysis at high temperature, the hydrolysis process is difficult to control and other disadvantages

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  • Preparation method for high-purity alumina
  • Preparation method for high-purity alumina
  • Preparation method for high-purity alumina

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Experimental program
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Effect test

Embodiment 1

[0027] Take 0.5kg of metal aluminum with a purity of 99.996%, 4kg of sec-butanol, HgCl 2 Add 0.1g to the synthesis kettle, heat to 90°C under reflux conditions, react for 6h, and the reaction ends. The resulting mixed solution was filtered and pumped for vacuum distillation at 190° C. and 10 mmHg vacuum to obtain aluminum alkoxide in a liquid state at room temperature. Slowly add 6.67kg of sec-butanol with a water content of 15wt% to the aluminum alkoxide under stirring conditions at room temperature. The molar ratio of aluminum alkoxide to water is kept at 1:3. Distill under high pressure to distill off excess alcohol to obtain aluminum hydroxide powder. Calcined at 1200° C. for 3 hours to obtain alumina powder with a purity of 99.999%. Such as figure 2 As shown in a, each diffraction peak is the characteristic diffraction peak of alumina. The aluminum oxide powder was analyzed by atomic spectroscopy quantitative analysis technology, and the test results are shown in Tabl...

Embodiment 2

[0029] Get 0.75kg of metal aluminum with a purity of 99.996%, 4.5kg of sec-butanol, HgCl 2 Add 0.3g into the synthesis kettle, heat to 90°C under reflux conditions, react for 6h, and the reaction ends. The resulting mixed solution was filtered and pumped for vacuum distillation at 190° C. and 10 mmHg vacuum to obtain aluminum alkoxide in a liquid state at room temperature. Slowly add 13.33kg of sec-butanol with a water content of 15wt% into the aluminum alkoxide under stirring conditions at room temperature. The molar ratio of aluminum alkoxide to water is kept at 1:4. Distill under high pressure to distill off excess alcohol to obtain aluminum hydroxide powder. Calcined at 1200° C. for 3 hours to obtain alumina powder with a purity of 99.999%. Such as figure 2 As shown in b, each diffraction peak is a characteristic diffraction peak of alumina.

Embodiment 3

[0031] Take 1.25kg of metal aluminum with a purity of 99.996%, 3.75kg of sec-butanol, HgCl 2 Add 0.2g into the synthesis kettle, heat to 90°C under reflux conditions, react for 6h, and the reaction ends. The resulting mixed solution was filtered and pumped for vacuum distillation at 190° C. and 10 mmHg vacuum to obtain aluminum alkoxide in a liquid state at room temperature. At room temperature, 33.33 kg of sec-butanol with a water content of 15 wt% was slowly added to the aluminum alkoxide under stirring conditions, and the molar ratio of the aluminum alkoxide to water was kept at 1:6. Distill under high pressure to distill off excess alcohol to obtain aluminum hydroxide powder. Calcined at 1200° C. for 3 hours to obtain alumina powder with a purity of 99.999%. Such as figure 2 As shown in c, each diffraction peak is a characteristic diffraction peak of alumina.

[0032] Table 1

[0033]

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Abstract

A preparation method for high-purity alumina powder includes: preparing aluminum alkoxide in liquid state at the room temperature by means of reaction of metallic aluminum with sec-butyl alcohol, using the reduced pressure distillation method for purifying, and preparing the high-purity alumina powder by means of hydrolyzing, reduced pressure distillation and calcinations. Using the method to prepare high-purity alumina powder has the advantages of simple preparation process, no pollution, low energy consumption, fine operating conditions, zero emission and the like. The alumina powder prepared by the method is applicable to the field of catalysts and can also be applied to the fields of laser crystals, sapphires, transparent alumina ceramics, sodium lamps, metal halides, high-grade abrasives and the like.

Description

technical field [0001] The invention relates to a method for preparing high-purity alumina, which belongs to the technical field of catalyst preparation. Background technique [0002] A preparation technology of high-purity alumina powder, which uses organic synthesis method to synthesize metal alkoxide which is liquid at room temperature by using metal aluminum and organic alcohol, and prepares high-purity alumina powder through purification, hydrolysis, hydrothermal treatment, vacuum drying and calcination body. The invention has the characteristics of no pollution in the technological process, easy transport of the synthesized alkoxide, good uniformity of the hydrolysis process, convenient and controllable alcohol recovery, good dispersibility of the product powder, controllable particle size and particle size distribution, and the like. [0003] With the rapid development of high-tech industry, the demand for high-purity alumina powder is increasing day by day, and the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/42
Inventor 王晶
Owner DALIAN JIAOTONG UNIVERSITY
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