A kind of preparation method of silver hexafluoroantimonate

A technology of silver hexafluoroantimonate and hexafluoroantimonate, applied in antimonate/antimonite and other directions, can solve the problems of low product purity, complicated impurity removal process and high cost of raw materials, and achieve high purity and purification method. Simple, high removal rate of impurities

Active Publication Date: 2020-07-24
CHENZHOU CITY JINGUI SILVER IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The cost of raw materials in this application is high, and the impurity removal process in the later stage is complicated, requiring 6-12 recrystallizations, and the purity of the product is low

Method used

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  • A kind of preparation method of silver hexafluoroantimonate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] 1) Preparation of hexafluoroantimonic acid: at 60°C, mix antimony trioxide with 40% hydrogen fluoride in acetic acid solution, and then dropwise add mass percent at a rate of 1 mL / min under stirring at 60 r / min. The concentration is 30% hydrogen peroxide, and hexafluoroantimonic acid solution is obtained after reacting for 1 hour; wherein, the mass volume ratio of antimony trioxide to the acetic acid solution of hydrogen fluoride is 1:1g / ml, and the mass volume ratio of antimony trioxide to hydrogen peroxide is 1:1g / ml;

[0050] 2) Preparation of silver hexafluoroantimonate mother liquor: react silver hexafluoroantimonate mother liquor in silver hexafluoroantimonate solution for 0.5h at 60°C to obtain silver hexafluoroantimonate mother liquor; the amount of silver carbonate and antimony trioxide equal amounts of substances;

[0051] 3) Silver hexafluoroantimonate mother liquor concentration and cooling crystallization: the silver hexafluoroantimonate mother liquor was ...

Embodiment 2

[0055] 1) Preparation of hexafluoroantimonic acid: at 100°C, mix antimony trioxide with 40% hydrogen fluoride in acetic acid solution, and then dropwise add 100% by mass at a rate of 30mL / min under stirring at 80r / min. The concentration is 30% hydrogen peroxide, and hexafluoroantimonic acid solution is obtained after reacting for 2 hours; wherein, the mass volume ratio of antimony trioxide to acetic acid solution of hydrogen fluoride is 1:1.5g / ml, and the mass volume ratio of antimony trioxide to hydrogen peroxide 1:1g / ml;

[0056] 2) Preparation of silver hexafluoroantimonate mother liquor: Silver carbonate in hexafluoroantimonic acid solution was reacted for 1 hour at 100°C to obtain silver hexafluoroantimonate mother liquor; wherein the amount of silver carbonate was the same as that of antimony trioxide equal amounts of substances;

[0057] 3) Silver hexafluoroantimonate mother liquor concentration and cooling crystallization: the silver hexafluoroantimonate mother liquor...

Embodiment 3

[0060] 1) Preparation of hexafluoroantimonic acid: at 120°C, mix antimony trioxide with 40% hydrogen fluoride in acetic acid solution, and then dropwise add 100% by mass at a rate of 5mL / min under stirring at 100r / min. The concentration is 30% hydrogen peroxide, and hexafluoroantimonic acid solution is obtained after reacting for 4 hours; wherein, the mass volume ratio of antimony trioxide to the acetic acid solution of hydrogen fluoride is 1:2g / ml, and the mass volume ratio of antimony trioxide to hydrogen peroxide is 1:1g / ml;

[0061] 2) Preparation of silver hexafluoroantimonate mother liquor: silver carbonate in hexafluoroantimonic acid solution, after reacting for 1 hour at 120° C., to obtain silver hexafluoroantimonate mother liquor; wherein the amount of silver carbonate is the same as that of antimony trioxide equal amounts of substances;

[0062] 3) Silver hexafluoroantimonate mother liquor is concentrated and cooled to crystallize: the silver hexafluoroantimonate mo...

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Abstract

The invention discloses a preparation method of silver hexafluoroantimonate. The preparation method comprises the following steps: mixing antimony trioxide and an acetic acid solution containing hydrogen fluoride, dropwise adding hydrogen peroxide at a speed of 1 to 30 mL / min to obtain a hexafluoroantimonate solution, adding silver carbonate to obtain a silver hexafluoroantimonate mother solution, concentrating, cooling, crystallizing to otain silver hexafluoroantimonate crude crystals, recrystallizing and purifying to obtain a silver hexafluoroantimonate product. By selecting the raw materials provided by the invention and controlling the reaction sequence of various steps, the reaction temperature, the reaction time as well as the dropwise addition speed of hydrogen peroxide, the entireoperation process of the preparation method provided by the invention is convenient, the reaction condition is mild, the raw material price is low, the environmental pollution is slight, the removalrate of impurities is high, and the purity of a final product is high and can reach 99 percent or more.

Description

technical field [0001] The invention belongs to the technical field of preparation of fine chemicals, and in particular relates to a preparation method of silver hexafluoroantimonate. Background technique [0002] Silver hexafluoroantimonate is a high value-added chemical product, which is currently mainly used in the field of organic synthesis and photochemistry. Compared with general catalysts, it has higher selectivity, better stability and longer service life, so its market The demand is gradually expanding. At present, there is no domestic enterprise producing silver hexafluoroantimonate, and foreign companies mainly produce it in the United States and Europe. Their products are exported to my country, but the price is very expensive. The main reason is that there is too little research on silver hexafluoroantimonate in my country, and the production The conditions are harsh and industrialization is difficult. The preparation method of silver hexafluoroantimonate mainl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G30/02
CPCC01G30/02C01P2006/80
Inventor 代林涛谢兆凤陈兰黄前军蒋朝金
Owner CHENZHOU CITY JINGUI SILVER IND CO LTD
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