Preparation method of highly pure alpha-aluminum oxide

An alumina, high-purity technology, applied in the field of metal-organic compound synthesis, can solve problems such as the troublesome recycling of aqueous isopropanol, the difficulty in preparing metal aluminum powder, and the high price of n-hexanol, achieving no environmental pollution and toxic residues, saving The effect of equipment investment and energy saving

Inactive Publication Date: 2010-12-22
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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  • Summary
  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

German Condea Company produces high-purity SB alumina (such as US4590289) with metal aluminum powder and n-hexanol, and has built an industrial device of 10,000 tons / year, and the products sell well all over the world. However, this process technology has difficulties in the preparation of metal aluminum powder. Disadvantages of expensive n-hexanol
The use of isopropanol and metal aluminum to prepare high-purity alumina has also achieved good results at home and abroad. However, due to the high melting point of aluminum isopropoxide, it is difficult to purify by distillation, and the hydrolyzed aluminum isopropoxide is recycled. More troublesome (eg GB825972, CN85100218)

Method used

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  • Preparation method of highly pure alpha-aluminum oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0014] Put 27g aluminum ingot, 1.33g anhydrous aluminum trichloride and 50g n-butanol (water content less than 0.2%) in a 1L four-necked flask with condenser. After refluxing for 1h, add 260g n-octanol and 24g n-butanol Mix alcohol with alcohol, reflux for 1h, and filter while hot. The filtrate was put into a 2L four-neck flask with a reflux condenser and a water separator. After the temperature reached 80°C, 400g of deionized water at 80°C was added to the hydrolysis reaction for 4h, the alcohol was separated, and 500g of deionized water was added. The temperature was raised to 95°C, refluxed and aged for 14h, the remaining alcohol was distilled off, and dried at 120°C for 6h to obtain 60g of white alumina. After XRD, differential thermal and atomic absorption analysis, it was proved to be high purity α-alumina·H 2 O.

Embodiment 2

[0016] Put 27g aluminum ingot, 1.33g anhydrous aluminum trichloride and 50g n-butanol (water content less than 0.2%) in a 1L four-necked flask with condenser. After refluxing for 0.5h, add 390g n-octanol and 61g n-butanol. Mix butanol with alcohol, reflux for 0.5h, and filter while hot. The filtrate was put into a 2L four-necked flask with a reflux condenser and a water separator. After the temperature reached 90°C, 400g of deionized water at a temperature of 90°C was added, the hydrolysis reaction was carried out for 4h, the alcohol was separated, and then 500g of deionized water was added. Reflux and age for 12 hours, distill out the remaining alcohol, and dry at 120°C for 6 hours to obtain 60 g of white alumina powder. After XRD, differential thermal and atomic absorption analysis, it was proved to be high purity α-alumina·H 2 O.

Embodiment 3

[0018] Put 27g aluminum wire, 1.3g anhydrous aluminum trichloride and 50g n-butanol into a 2L four-necked flask. After reaction for 0.5h, add 390g n-octanol and 61g n-butanol mixed alcohol and reflux for 2h. The following operation is the same as the example 1. Hydrolysis temperature is 80℃, time is 4h, aging temperature is 100℃, time is 12h, drying temperature is 120℃, time is 6h.

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Abstract

The invention provides a preparation method of highly pure alpha-aluminum oxide, belonging to the technical field of metal organic compound synthesis. The preparation method comprises the following steps of making metal aluminum having purity of more than 99.5% react with mixed alcohol to prepare aluminum alkoxy, and then hydrolyzing, aging and drying the aluminum alkoxy to obtain highly pure alpha-aluminum oxide. The invention overcomes the purification difficulty when the aluminum alkoxy is prepared by low-carbon alcohol and the shortages of low reaction efficiency when the aluminum alkoxy is prepared by high-carbon alcohol; the alpha-aluminum oxide with the purity as high as 99.9% can be obtained by controlling the mixing alcohol proportion and the hydrolysis condition; and the invention simplifies the preparation technique of the highly pure alpha-aluminum oxide and has high preparation efficiency and low preparation cost.

Description

Technical field [0001] A method for preparing high-purity α-alumina belongs to the technical field of metal organic compound synthesis. The preparation method uses metal aluminum and a mixed alcohol of C5-C8 alcohol and n-butanol as reactants, anhydrous aluminum chloride as a catalyst to synthesize aluminum alkoxide, and then hydrolyze aluminum alkoxide to obtain aluminum hydroxide, which is aged and dried Then α-alumina is obtained. The alcohol produced after hydrolysis and aging can be recycled. This method has no environmental pollution and toxic residue. The product is widely used in the field of catalyst carriers and materials. Background technique [0002] High-purity alumina is an important material for catalyst carriers, integrated circuit substrates, transparent phosphors, functional single crystals, precision instruments and aviation functional devices. The research and development of high-purity alumina preparation methods have been carried out for many years, and in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/42
Inventor 辛秀兰徐宝财周雅文高玉李董黎明赵进吴爱萍
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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