Preparation method of high-purity antimony trioxide

An antimony trioxide, high-purity technology, applied in chemical instruments and methods, antimony oxide/antimony hydroxide/antimony oxyacid, inorganic chemistry, etc. The large particle size of antimony and the large amount of leaching agent can achieve the effects of short time, improved purity and simple reagents.

Active Publication Date: 2021-08-20
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 is to hydrolyze 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.)
Chinese invention patent CN201410328080.3 discloses a method for removing lead, cadmium and iron in the refining of crude antimony. 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 is relatively low. More, the amount added is 120~150kg / 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 solution for impregnation, then pass chlorine gas into the solution, the flow rate of chlorine gas is 300L / h, at 70~90℃ React for 2 to 4 hours, filter and wash to obtain a mixed solution 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-mentioned 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 obta...

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 solution for impregnation, then pass chlorine gas into the solution, the flow rate of chlorine gas is 360L / h, and the React for 2 to 4 hours, filter and wash to obtain a mixed solution 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-mentioned 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...

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 solution for impregnation, then pass chlorine gas into the solution, the flow rate of chlorine gas is 280L / h, at 70-90°C React for 2 to 4 hours, filter and wash to obtain a mixed solution 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-mentioned 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 obt...

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Abstract

The invention discloses a preparation method of high-purity antimony trioxide, and belongs to the technical field of antimony trioxide preparation. The preparation method comprises the following steps of: adding crude antimony ore into a hydrochloric acid solution for dipping, introducing chlorine, adding iron powder into an obtained antimony chloride mixed solution, and performing a reaction to obtain an antimony chloride solution; then adding a proper amount of 4 mol / L sodium hydroxide solution with the pH value of 8-9, performing stirring, filtering, washing and drying, and performing roasting in an air atmosphere to obtain antimony trioxide; gasifying the antimony trioxide into liquid, introducing compressed air and a composite lead removal agent, gasifying and quenching prepared antimony trioxide powder, thereby obtaining the high-purity antimony trioxide. According to the method provided by the invention, simplicity in preparation is realized, the usage amount of the composite lead removal agent is small, the cost is relatively low, the composite lead removal agent can be recycled, and no burden is caused to the environment; the purity of the prepared antimony trioxide can reach 99.5% at most, the particle size can reach the nanoscale, and the particle size distribution is uniform.

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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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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