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Preparation method for anhydrous aluminum fluoride

A technology of aluminum fluoride and aluminum fluoride, which is applied in the field of preparation of anhydrous aluminum fluoride, can solve the problems of high cost, long preparation period, low output and the like

Inactive Publication Date: 2012-03-28
GUIZHOU BRANCH CHINA ALUMINUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Some people also use the method of vacuum volatilization and recrystallization to prepare anhydrous aluminum fluoride. This method can obtain aluminum fluoride with a purity higher than 99.5%, but the cost is high, and the preparation cycle is long and the output is low.

Method used

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preparation example Construction

[0018] A method for preparing anhydrous aluminum fluoride. In the preparation process, the aluminum fluoride trihydrate reagent is first put into a tray, and dried in a blast drying oven at 110-260°C for 8-16 hours. At this time, the fluoride trihydrate Aluminum desorbs most of the water of crystallization, forming a compound containing about 1 water of crystallization (AlF 3· ·H 2 o). Since the drying temperature is lower than the hydrolysis temperature of aluminum fluoride, alumina will not be hydrolyzed in the process, which ensures that no impurities are generated in the process. At this stage, the weight loss rate of aluminum fluoride trihydrate is 20%~26%.

[0019] After the above dried aluminum fluoride is cooled to room temperature, add ammonium bifluoride and mix well. The mass ratio of the added ammonium bifluoride to the initial aluminum fluoride trihydrate is 1:20-1:12. If ammonium fluoride is added, the The mass ratio of ammonium chloride to the initial aluminu...

Embodiment 1

[0023] Take 1500g of aluminum fluoride trihydrate, put it in a stainless steel tray, put it in a blast drying oven at 130°C and dry it for 16 hours, take it out, cool it to room temperature, add 120g of ammonium bifluoride and mix evenly, and place the mixed material in a graphite crucible Then put it into the high temperature furnace and wait for roasting. The gas generated during the roasting process is absorbed with hydrochloric acid solution and sodium hydroxide solution sequentially. The temperature curve of calcination is as follows: from room temperature to 300°C, heat up for 90 minutes; at 300~500°C, heat up for 120 minutes; at 500~650°C, heat up for 120 minutes.

Embodiment 2

[0025] Take 1500g of aluminum fluoride trihydrate, place it in a stainless steel tray, put it in a blast drying oven at 170°C and dry it for 12 hours, take it out, cool it to room temperature, add 100g of ammonium bifluoride and mix evenly, and place the mixed material in a graphite crucible Then put it into the high temperature furnace and wait for roasting. The gas generated during the roasting process is absorbed with hydrochloric acid solution and sodium hydroxide solution sequentially. The roasting temperature curve is as follows: from room temperature to 300°C, heat up for 70 minutes; at 300~500°C, heat up for 150 minutes; at 500~650°C, heat up for 90 minutes.

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Abstract

The invention relates to a preparation method for anhydrous aluminum fluoride. The method is characterized in that: analytically pure aluminum fluoride trihydrate and ammonium hydrogen fluoride are used as raw materials in a preparation process of the method; and the preparation process comprises the following steps of: (1) drying the aluminum fluoride trihydrate to obtain AlF3.H2O; (2) cooling the dried AlF3.H2O to room temperature and then adding the ammonium hydrogen fluoride to uniformly mix; and (3) roasting the mixture obtained in the step (2) to prepare aluminum fluoride. By using the method, the cost is low, and the anhydrous aluminum fluoride with purity of more than 99.7 percent and aluminum oxide content of less than 0.05 percent can be prepared.

Description

technical field [0001] The invention relates to a preparation method of anhydrous aluminum fluoride. Background technique [0002] Aluminum fluoride is used industrially in the aluminum electrolysis industry to adjust the molecular ratio of the electrolyte. The alumina content in industrial aluminum fluoride is as high as 4-15%, but since the alumina is also the raw material for aluminum electrolysis, it will not affect the electrolysis process. However, in laboratory research, aluminum fluoride with high purity (purity greater than 99.5%) is required for basic research on the physical, chemical and electrochemical properties of electrolytes, and industrial aluminum fluoride can no longer meet the requirements. However, among commercially available reagents, the purity of analytically pure anhydrous aluminum fluoride is only 85%-96%, which cannot meet the requirements of basic experimental research. High-purity anhydrous aluminum fluoride reagents are expensive, and the pr...

Claims

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Application Information

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IPC IPC(8): C01F7/50
Inventor 颜恒维杨建红
Owner GUIZHOU BRANCH CHINA ALUMINUM IND
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