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Preparation method of high-purity hydrated alumina

A technology of pure hydration and alumina, which is applied in the field of metal-organic compound synthesis, can solve problems such as the troublesome recycling of hydrous isopropanol, the difficulty in preparing metal aluminum powder, and the high melting point of aluminum isopropoxide, so as to achieve short hydrolysis aging time and save Equipment investment and energy consumption, the effect of easy filtration

Inactive Publication Date: 2011-07-13
BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

German Condea Company uses metal aluminum powder and n-hexanol to produce high-purity SB alumina (such as US4590289), and has built an industrial device of 10,000 tons per year. The products sell well all over the world, but this process technology has difficulties in the preparation of metal aluminum powder
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 and longer response time (eg GB825972, CN85100218)

Method used

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Experimental program
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Effect test

Embodiment 1

[0015] Put 27g of aluminum ingots, 1.33g of anhydrous aluminum trichloride and 50g of n-hexanol (water content less than 0.2%) in a 1L four-neck flask with a condenser tube, and after reflux for 0.5h, drop 256g of n-hexanol into the flask and react under reflux 1h, filtered while hot. The filtrate was put into a 2L autoclave at a temperature of 80°C, and after adding 400 g of deionized water at a temperature of 80°C, the system was sealed. Raise the temperature to 120°C, perform hydrolysis for 2 hours, separate the alcohol, then add 500g of deionized water at 95°C, raise the temperature to 115-180°C, age for 5h, evaporate the remaining alcohol, and spray dry to obtain 60g of white alumina. After XRD, differential thermal and ICP-MS analysis, it is proved to be high-purity α--Al 2 o 3 ·H 2 O.

Embodiment 2

[0017] Put 27g of aluminum ingots, 1.33g of anhydrous aluminum trichloride and 50g of n-hexanol (water content less than 0.2%) in a 1L four-neck flask with a condenser tube, and after reflux for 0.5h, add 307g of n-hexanol and react for 0.5 h, filter while hot. The filtrate was put into a 2L autoclave at a temperature of 80°C, and after adding 400 g of deionized water at a temperature of 80°C, the system was sealed. Raise the temperature to 115-180°C, perform a hydrolysis reaction for 2 hours, separate the alcohol, then add 500g of deionized water at 95°C, raise the temperature to 120°C, age for 4 hours, evaporate the remaining alcohol, and spray dry to obtain 60g of white alumina. After XRD, differential thermal and ICP-MS analysis, it is proved to be high-purity α--Al 2 o 3 ·H 2 O.

Embodiment 3

[0019] Put 27g of aluminum wire, 1.3g of anhydrous aluminum trichloride and 50g of n-hexanol into a 2L four-neck flask, and after reacting for 0.5h, add 256g of n-hexanol, reflux for 2h, filter while it is hot, and put the filtrate into a refrigerator with a temperature of 90°C In a 2L autoclave, add 400 g of deionized water at a temperature of 90° C., and then seal the system. Raise the temperature to 130°C, perform hydrolysis reaction for 2 hours, separate the alcohol, then add 500g of deionized water at 95°C, raise the temperature to 130°C, age for 3h, evaporate the remaining alcohol, and spray dry to obtain 60g of white alumina. After XRD, differential thermal and ICP-MS analysis, it is proved to be high-purity α--Al 2 o 3 ·H 2 O.

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Abstract

The invention provides a preparation method of high-purity hydrated alumina, belonging to the technical field of metal organic compound synthesis. In the preparation method, metal aluminum with the purity more than 99.5% and C5-C8 high-carbon alcohol react to prepare alkoxy aluminum, and the alkoxy aluminum is subjected to high-pressure hydrolysis, ageing and drying to obtain the high-purity hydrated alumina. The invention overcomes the defects of difficult purification when the alkoxy aluminum is prepared from low-carbon alcohol and difficult recovery and use of the low-carbon alcohol. By adopting the conditions of high-temperature and high-pressure hydrolysis and ageing, reaction time can be obviously decreased and the alumina with the purity up to 99.9% can be obtained; and the preparation method provided by the invention ensures that the high-purity hydrated alumina is prepared with a simplified process, high efficiency and low cost.

Description

technical field [0001] The invention discloses a preparation method of high-purity hydrated alumina, which belongs to the technical field of synthesis of metal organic compounds. The preparation method uses metal aluminum and C5-C8 alcohol as reactants and anhydrous aluminum chloride as a catalyst to synthesize aluminum alkoxide, and then hydrolyzes aluminum alkoxide under normal pressure or high pressure to obtain hydrated alumina after aging and drying. Alcohol produced after hydrolysis and aging can be recycled. This method has no environmental pollution and toxic residues, and the obtained product has high purity. 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...

Claims

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Application Information

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IPC IPC(8): C01F7/42
Inventor 辛秀兰徐培力徐培全褚洪波徐宝财
Owner BEIJING TECHNOLOGY AND BUSINESS UNIVERSITY
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