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A kind of preparation method of high-purity antimony trioxide

A high-purity technology of antimony trioxide, applied in chemical instruments and methods, antimony oxide/antimony hydroxide/antimony oxyacid, inorganic chemistry, etc., can solve the problem that the product particle size cannot meet the requirements of fine fields, trioxide The problem of large particle size of antimony and general product purity can achieve the effect of short time, high purity and simple reagents.

Active Publication Date: 2022-05-20
HUNAN LOUDI HUAXING ANTIMONY IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The amount of leaching agent used in this method is too much, and if the chemical reagents are not recovered properly, it is easy to cause environmental pollution, which is uneconomical and the cost is too high
[0004] Chinese invention patent CN201711117564.3 discloses a method for purifying antimony trioxide. The method involves hydrolyzing industrial-grade antimony trioxide and acetic acid aqueous solution to remove arsenic impurities. This method reduces the amount of waste water and the arsenic impurities. content, but this method does not remove other impurities (such as lead, iron, cadmium, etc.) in industrial antimony trioxide.
Chinese invention patent CN201410328080.3 discloses a method for removing lead, cadmium and iron in crude antimony refining. The method uses a compound lead removing agent with a phosphoric acid content of 92-95wt% and a sodium chloride content of 0.3-0.5wt%. At a furnace temperature of 700-800°C, the impurity metals in the crude antimony solution are removed. This method adopts a lower temperature, and the impurity removal effect is good without rebound, but the compound lead removal dose used in the impurity removal process of this method is relatively low More, the amount added is 120-150 kg / m 3 Antimony liquid, the cost is relatively high, and the particle size of antimony trioxide is relatively large

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A preparation method of high-purity antimony trioxide, specifically comprising the following steps:

[0037] (1) Add 1kg of crude antimony ore (1.0%≤Pb≤2.0%) into 3L of 1mol / L hydrochloric acid for impregnation, then pass chlorine gas into the solution, the flow rate of chlorine gas is 300L / h, and react at 70-90°C After 2-4 hours, filter and wash to obtain a mixture of antimony chloride.

[0038] (2) Add 40g of iron powder (reducing agent) to the antimony chloride mixed solution, react at 70-90°C for 2-3 hours, filter and wash to obtain antimony chloride solution.

[0039] (3) Slowly add 4mol / L sodium hydroxide solution to the above antimony chloride solution until the precipitate in the solution no longer increases or the precipitate begins to decrease, that is, stop adding the sodium hydroxide solution and adjust the pH value to 8~ 9. Stir again for 1-3 hours, filter, wash, dry, and then roast in air atmosphere at 600-800°C for 3-5 hours to obtain antimony trioxide. ...

Embodiment 2

[0046] A preparation method of high-purity antimony trioxide, specifically comprising the following steps:

[0047] (1) Add 1kg of crude antimony ore (0.8%≤Pb<1.0%) into 3L of 5mol / L hydrochloric acid for impregnation, then pass chlorine gas into the solution, the flow rate of chlorine gas is 360L / h, and react at 70-90°C After 2-4 hours, filter and wash to obtain a mixture of antimony chloride.

[0048] (2) Add 45g of iron powder (reducing agent) to the antimony chloride mixed solution, react at 70-90°C for 2-3 hours, filter and wash to obtain antimony chloride solution.

[0049] (3) Slowly add 4mol / L sodium hydroxide solution to the above antimony chloride solution until the precipitate in the solution no longer increases or the precipitate begins to decrease, that is, stop adding the sodium hydroxide solution and adjust the pH value to 8~ 9. Stir again for 1-3 hours, filter, wash, dry, and then roast in air atmosphere at 600-800°C for 3-5 hours to obtain antimony trioxide. ...

Embodiment 3

[0056] A preparation method of high-purity antimony trioxide, specifically comprising the following steps:

[0057] (1) Add 1kg of crude antimony ore (0.6%≤Pb<0.8%) into 4L of 5mol / L hydrochloric acid for impregnation, then pass chlorine gas into the solution, the flow rate of chlorine gas is 280L / h, and react at 70-90°C After 2-4 hours, filter and wash to obtain a mixture of antimony chloride.

[0058] (2) Add 51g of iron powder (reducing agent) to the antimony chloride mixed solution, react at 70-90°C for 2-3 hours, filter and wash to obtain antimony chloride solution.

[0059] (3) Slowly add 4mol / L sodium hydroxide solution to the above antimony chloride solution until the precipitate in the solution no longer increases or the precipitate begins to decrease, that is, stop adding the sodium hydroxide solution and adjust the pH value to 8~ 9. Stir again for 1-3 hours, filter, wash, dry, and then roast in air atmosphere at 600-800°C for 3-5 hours to obtain antimony trioxide. ...

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PUM

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Abstract

The invention discloses a method for preparing high-purity antimony trioxide, and relates to the technical field of antimony trioxide preparation. The preparation method of a high-purity antimony trioxide disclosed by the present invention is as follows: adding crude antimony ore to hydrochloric acid for immersion, feeding chlorine gas, adding iron powder to the obtained antimony chloride mixed solution, and reacting to obtain an antimony chloride solution; Then add an appropriate amount of 4mol / L sodium hydroxide solution, the pH value is 8-9, stir and filter, wash, dry, and roast in the air atmosphere to obtain antimony trioxide; Air and composite lead remover, the obtained antimony trioxide powder is vaporized and then quenched to obtain high-purity antimony trioxide. The method provided by the invention is simple to prepare, uses less composite lead remover, lower cost, can be recycled and used without burdening the environment, and the purity of the prepared antimony trioxide can reach up to 99.5%, and the particle size can reach Nanoscale, uniform particle size distribution.

Description

technical field [0001] The invention belongs to the technical field of antimony trioxide preparation, and in particular relates to a preparation method of high-purity antimony trioxide. Background technique [0002] Antimony trioxide (Sb 2 o 3 ), white crystal powder, yellow when heated, and turn white or gray again after cooling, with a relative density of 5.22 to 5.67. It is an important raw material in chemical production. The application of pure antimony products in high-tech fields such as chemical raw materials is becoming more and more extensive, and with the application requirements in the fine field, the requirements for its purity and particle size are correspondingly higher and higher. [0003] The traditional production methods of antimony trioxide are divided into traditional fire method and wet method. The production of antimony trioxide by fire method is divided into direct method and indirect method. The direct method is to directly produce antimony triox...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G30/00B82Y40/00
CPCC01G30/005B82Y40/00C01P2006/80C01P2006/60Y02P10/20
Inventor 龚文
Owner HUNAN LOUDI HUAXING ANTIMONY IND
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