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Preparation method of high-purity diantimony trioxide

A technology for purifying antimony trioxide and antimony trichloride, which is applied in the fields of chemical instruments and methods, inorganic chemistry, antimony compounds, etc., and can solve the problem of low purity of antimony trioxide, impurity High content and other problems, to achieve the effect of low cost, high production efficiency, low impurity content

Inactive Publication Date: 2011-04-20
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] High-purity antimony trioxide is widely used in the doping and diffusion process of semiconductor production. The current preparation method is to dissolve antimony trichloride in a mixture of hydrochloric acid and distilled water, and then dissolve sodium carbonate in distilled water and boil. Then slowly pour the antimony trichloride solution into the boiling solution of sodium carbonate, continue to boil, cool, pour out the clear liquid, drain it with a Buchner funnel, put it in an oven at 150°C, and dry it to obtain antimony trioxide. The antimony trioxide prepared by this method has low purity and high impurity content, and can only be used in flame retardants such as resins and synthetic rubbers, catalysts for petrochemicals and synthetic fibers, etc., and cannot meet the needs of high-end products in the electronics industry and semiconductors.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 1. Distillation and purification of antimony trichloride:

[0015] 500g antimony trichloride rectification purification;

[0016] 2. Hydrolysis and ammonia solution:

[0017] Put the antimony trichloride purified by rectification into a glass beaker, add 5000mL of distilled water, heat at 80°C, dissolve, continue to heat at 150°C until boiling, and keep stirring, when white antimony oxychloride and antimony trioxide appear When the mixture precipitated, add 28% high-purity ammonia water, adjust the pH value to 8, and let stand overnight to obtain A;

[0018] 3. Washing to obtain antimony trioxide:

[0019] Suck out the supernatant in A after standing overnight, put the precipitate in a glass beaker, add 3000mL distilled water, heat to boiling, the temperature is 160°C, adjust the pH value to 8 with ammonia water, wash 5 times repeatedly, and pump the precipitate with a Buchner funnel Dry it, put it in an oven, and bake it at 120°C for 4 hours to obtain high-purity an...

Embodiment 2

[0021] 1. Distillation and purification of antimony trichloride:

[0022] 400g antimony trichloride rectification purification;

[0023] 2. Hydrolysis and ammonia solution:

[0024] Put the antimony trichloride purified by rectification into a glass beaker, add 4000mL of distilled water, heat to 85°C, dissolve, continue to heat to 160°C, until boiling, keep stirring, when white antimony oxychloride and antimony trioxide appear When the mixture precipitated, add 26% high-purity ammonia water, adjust the pH value to 9, and let stand overnight to obtain A;

[0025] 3. Washing to obtain antimony trioxide:

[0026] Suck out the supernatant in A after standing overnight, put the precipitate in a glass beaker, add 3500mL distilled water, heat to boiling, the temperature is 165°C, adjust the pH value to 9 with ammonia water, wash 4 times repeatedly, and pump the precipitate with a Buchner funnel Dry it, put it in an oven, and bake it at 120°C for 3.5 hours to obtain high-purity ant...

Embodiment 3

[0028] 1. Distillation and purification of antimony trichloride:

[0029] 450g antimony trichloride rectification purification;

[0030] 2. Hydrolysis and ammonia solution:

[0031] Put the antimony trichloride purified by rectification into a glass beaker, add 4500mL of distilled water, heat to 85°C, dissolve, continue to heat to 155°C, until boiling, keep stirring, when white antimony oxychloride and antimony trioxide appear When the mixture precipitated, add 28% high-purity ammonia water, adjust the pH value to 8, and let stand overnight to obtain A;

[0032] 3. Washing to obtain antimony trioxide:

[0033] Suck out the supernatant in A after standing overnight, put the precipitate in a glass beaker, add 4000mL distilled water, heat to boiling, the temperature is 165°C, adjust the pH value to 8.5 with ammonia water, wash 5 times repeatedly, and pump the precipitate with a Buchner funnel Dry it, put it in an oven, and bake it at 120°C for 4 hours to obtain high-purity ant...

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Abstract

The invention relates to the field of a preparation method of an inorganic compound, in particular to a preparation method of high-purity diantimony trioxide, which is characterized by comprising the following steps of: rectifying antimony trichloride, hydrolyzing, ammonolyzing, washing, and the like to prepare the high-purity diantimony trioxide. The invention has simple processing steps, higher production efficiency and low cost. The obtained diantimony trioxide has high purity and low impurity content and can satisfy urgent needs of the current markets.

Description

technical field [0001] The invention relates to the field of preparation methods of inorganic compounds, in particular to a preparation method of high-purity antimony trioxide. Background technique [0002] High-purity antimony trioxide is widely used in the doping and diffusion process of semiconductor production. The current preparation method is to dissolve antimony trichloride in a mixture of hydrochloric acid and distilled water, and then dissolve sodium carbonate in distilled water and boil. Then slowly pour the antimony trichloride solution into the boiling solution of sodium carbonate, continue to boil, cool, pour out the clear liquid, drain it with a Buchner funnel, put it in an oven at 150°C, and dry it to obtain antimony trioxide. The antimony trioxide prepared by this method has low purity and high impurity content, and can only be used in flame retardants such as resins and synthetic rubbers, catalysts for petrochemicals and synthetic fibers, etc., and cannot me...

Claims

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Application Information

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IPC IPC(8): C01G30/00
Inventor 胡建华
Owner TIANJIN CHEM REAGENT RES INST
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