Method of producing a highly-pure aluminum hydroxide

Patent metadata

Field	Value
Publication number	US-10526211-B2
Application number	US-201715656079-A
Country	US
Kind code	B2
Filing date	Jul 21, 2017
Priority date	Jul 21, 2016
Publication date	Jan 7, 2020
Grant date	Jan 7, 2020

Abstract

A method of producing a highly-pure aluminum hydroxide, comprising the following steps: (1) reacting alcohol with metal aluminum to produce aluminum alkoxide, then hydrolyzing the aluminum alkoxide with water to produce an aluminum hydroxide slurry and an alcohol, filtering the aluminum hydroxide slurry, washing a resulting filter cake with water to remove the alcohol trapped therein, and drying the filter cake after the water washing to produce an aluminum hydroxide powder, (2) sending the alcohol-containing water produced in step (1) to an alcohol extraction unit for separating water and alcohol through extraction, and sending the separated water back to step (1) for recycling, (3) dehydrating the hydrous alcohol produced by hydrolyzing the aluminum alkoxide in step (1) before using it as the raw materials for reacting metal aluminum with alcohol to produce aluminum alkoxide in step (1). The method can improve the recovery of alcohol, reduce the production cost of a highly-pure aluminum hydroxide, improve the purity of aluminum oxide and achieve a zero discharge of sewage by recycling water.

First claim

The invention claimed is:

1. A method of producing aluminum hydroxide, comprising:
(1) reacting alcohol with metal aluminum to produce aluminum alkoxide, then hydrolyzing the aluminum alkoxide with water to produce an aluminum hydroxide slurry and a hydrous alcohol, separating the hydrous alcohol from the aluminum hydroxide slurry, wherein a content of water in the hydrous alcohol is less than 50 wt %, filtering the aluminum hydroxide slurry to obtain a filter cake and a filtrate, washing the filter cake with water to remove the alcohol trapped therein into a wash solution, and drying the washed filter cake to produce an aluminum hydroxide powder, combining the filtrate and the wash solution to obtain an alcohol-containing water, wherein the alcohol-containing water has an alcohol content of less than 50 wt %;
(2) sending the alcohol-containing water to an alcohol extraction unit for separating water and alcohol through extraction, using water separated from the alcohol extraction unit to wash the filter cake, to hydrolyze aluminum alkoxide, or both; and
(3) dehydrating the hydrous alcohol produced by hydrolyzing the aluminum alkoxide in step (1), and reacting the resulting anhydrous alcohol with metal aluminum to produce aluminum alkoxide.

2. The method according to claim 1 , characterized in that gas is used for drying during the process of drying the filter cake in step (1) and the resulting dry off-gas is further washed with water to remove the alcohol therein.

3. The method according to claim 2 , characterized in that the water used for washing the off-gas produced during the process of drying the filter cake is the water produced by the extraction separation in step (2).

4. The method according to claim 3 , characterized in that the water obtained after water washing the off-gas from the process of drying the filter cake is used for washing the filter cake and hydrolyzing the aluminum alkoxide.

5. The method according to claim 1 , characterized in that the alcohol in step (1) is C 1 -C 20 alkanol.

6. The method according to claim 1 , characterized in that temperature for reacting alcohol with metal aluminum in step (1) is from 60° C. to 200° C., and molar ratio of alcohol to metal aluminum is from 2 to 5:1.

7. The method according to claim 1 , characterized in that a temperature for hydrolyzing the aluminum alkoxide with water in step (1) is from 30° C. to 90° C., and a weight ratio of water to aluminum alkoxide is from 0.5 to 5:1.

8. The method according to claim 1 , characterized in that the solid content of the aluminum hydroxide slurry produced by hydrolyzing the aluminum alkoxide in step (1) is from 7 to 12 wt. %, calculated as aluminum oxide.

9. The method according to claim 1 , characterized in that the alcohol content of the aluminum hydroxide slurry produced by hydrolyzing the aluminum alkoxide in step (1) is from 1 to 30 wt. %.

10. The method according to claim 1 , characterized in that a diameter of the aluminum hydroxide particles is from 0.5 μm to 1000 μm in the aluminum hydroxide slurry obtained by hydrolyzing the aluminum alkoxide in step (1).

11. The method according to claim 1 , characterized in that a temperature for washing the filter cake with water in step (1) is from 40° C. to 90° C.

12. The method according to claim 1 , characterized in that a number of times for washing the filter cake with water in step (1) is from 1 to 3.

13. The method according to claim 1 , characterized in that an amount of washing water in the process of washing the filter cake with water in step (1) is from 1 to 10 times the weight of the filter cake.

14. The method according to claim 1 , characterized in that an extraction agent used for separating water and alcohol through extraction in step (2) is C 6 -C 9 arene or C 6 -C 9 alkane.

15. The method according to claim 1 , characterized in that the temperature for the extraction separation of water and alcohol in step (2) is from 50° C. to 90° C.

16. The method according to claim 1 , further comprising: after the extraction separation in step (2), rectifying a resulting extraction phase to separate the extraction agent from alcohol, and reacting the alcohol with metal aluminum to produce aluminum alkoxide.

17. The method according to claim 14 , characterized in that the temperature for the extraction separation of water and alcohol in step (2) is from 50° C. to 90° C.

18. The method according to claim 14 , further comprising: after the extraction separation in step (2), rectifying a resulting extraction phase to separate the extraction agent from alcohol, and reacting the alcohol with metal aluminum to produce aluminum alkoxide.

Assignees

• China Petroleum & Chem Corp
• Sinopec Res Inst Petroleum

Inventors

• Yang Yanpeng
• Ma Aizeng

Classifications

• C01F7/42 Primary

  Preparation of aluminium oxide or hydroxide from metallic aluminium, e.g. by oxidation · CPC title

• C01P2004/61

  Micrometer sized, i.e. from 1-100 micrometer · CPC title

• C01F7/36 Primary

  from organic aluminium salts · CPC title

• C01F7/30 Primary

  Preparation of aluminium oxide or hydroxide by thermal decomposition or by hydrolysis or oxidation of aluminium compounds · CPC title

• C01P2006/80

  Compositional purity · CPC title