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Production method of selenium sulfide powder

A production method, the technology of selenium disulfide, applied in the direction of binary selenium/tellurium compounds, etc., can solve the problems of high equipment requirements, low single-batch production capacity, and many quartz wastes, and achieve simple equipment and operation, convenient absorption and treatment, and synthesis The effect of low temperature

Inactive Publication Date: 2020-12-08
广东先导稀贵金属材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Its shortcoming is: the selenium disulfide purity that this method prepares is on the low side
Its disadvantages are: vacuum seal the tube, it is necessary to vacuum the inside of the quartz tube to 10 -5 Calcination and sealing after Pa below, higher requirements for equipment
The amount of quartz tube is less, and the production capacity of a single batch is low; the quartz tube is a consumable product, which produces a lot of quartz waste, and the overall production cost is high

Method used

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  • Production method of selenium sulfide powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Get 3N selenium powder and 3N sulfur powder, batch 2000g by mass ratio 53.0:47.0, put into ball mill and ball mill and mix for 20min to obtain the mixture, put the mixture in a quartz crucible, then place the quartz crucible in a melting furnace, The temperature of the melting furnace was raised to 130°C within 10 minutes, and the temperature was kept and stirred for 12 hours to obtain the melt. Pour the molten material into pure water to cool, then put it into an oven, dry it at 40°C, cool it, pulverize it and sieve it to obtain 1982g of selenium disulfide powder.

[0031] The selenium disulfide powder prepared in this embodiment is orange yellow, detected by X-ray diffraction, the product phase is pure selenium disulfide, the selenium content is 52.53%, soluble selenium <1.0ppm, and the ignition residue is 0.087%. The total amount of impurities is less than 1000ppm, and the product yield is 99.1%.

Embodiment 2

[0033] Get 3N selenium powder and 3N sulfur powder, batch 2000g by mass ratio 53.5:46.5, put into ball mill and ball mill and mix for 15min to obtain the mixture, the mixture is placed in a quartz crucible, then the quartz crucible is placed in a melting furnace, The temperature of the melting furnace was raised to 140°C within 14 minutes, and the temperature was kept and stirred for 10 hours to obtain the melt. Pour the molten material into pure water to cool, then put it into an oven, dry it at 30°C, and then cool it, pulverize it and sieve it to obtain 1974g of selenium disulfide powder.

[0034] The selenium disulfide powder prepared in this embodiment is orange yellow, and detected by X-ray diffraction, the product phase is pure selenium disulfide, the selenium content is 52.78%, the soluble selenium is 3.5ppm, the ignition residue is 0.110%, and the impurity The total amount is less than 1000ppm, and the product yield is 98.7%.

Embodiment 3

[0036] Get 3N selenium powder and 3N sulfur powder, batch 2000g by mass ratio 54.5:45.5, put into ball mill and ball mill and mix for 25min to obtain the mixture, the mixture is placed in a quartz crucible, then the quartz crucible is placed in a melting furnace, The temperature of the melting furnace was raised to 160°C within 12 minutes, and the temperature was kept and stirred for 6 hours to obtain the melt. Pour the molten material into pure water to cool, then put it into an oven, dry it at 100°C, and then cool it, pulverize it and sieve it to obtain 1964g of selenium disulfide powder.

[0037] The selenium disulfide powder prepared in this embodiment is orange-yellow, and detected by X-ray diffraction, the product phase is pure selenium disulfide, the selenium content is 53.57%, soluble selenium<1.0ppm, and the ignition residue is 0.070%. The total amount of impurities is less than 1000ppm, and the product yield is 98.2%.

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Abstract

The invention relates to a production method of selenium sulfide powder. The method comprises the following steps: S1, performing proportioning: proportioning selenium powder and sulfur powder in a mass ratio of (53.0-55.0): (45.0-47.0), putting the mixed material into a ball-milling tank, performing ball-milling and uniform mixing or putting the mixed mateiral into a homogenizer, and uniformly performing mixing to form a mixture; S2, performing charging: putting the mixture into a crucible, and then putting the crucible into a melting furnace; and S3, performing heating reaction: heating themelting furnace to a target temperature of 130-200 DEG C at a certain heating rate, and carrying out a heat preservation stirring reaction for 4-12 h to obtain a melt; and cooling the melt , drying the cooled melt, crushing the dried melt and sieving the crushed melt to obtain selenium sulfide powder. According to the production method of the selenium sulfide, the selenium powder with the purity of 3N or above and the sulfur powder are selected as raw materials, and the selenium sulfide powder with the corresponding purity can be obtained; vacuumizing is not needed in the production process, equipment and operation are simple, and the production yield is over 98%; because the synthesis temperature is low, less smoke is generated by volatilization, the absorption treatment is convenient, and the method is environment-friendly.

Description

technical field [0001] The invention relates to the field of preparation of selenium compounds, in particular to a production method of selenium disulfide powder. Background technique [0002] Selenium Sulfide is an orange-yellow to reddish-brown powder with a faint smell of hydrogen sulfide; it is insoluble in water, slightly soluble in chloroform, easily soluble in aqua regia, and will decompose slowly in nitric acid. Selenium disulfide has anti-seborrhea and anti-fungal effects, and has good curative effects on seborrheic dermatitis, tinea versicolor and other diseases; its 25% suspoemulsion can be used as shampoo, and has good effects on dandruff patients . [0003] At present, there are two main methods for the preparation of selenium disulfide. [0004] One is wet synthesis: under acidic conditions, sodium sulfide (or ammonium sulfide, ammonium bisulfide) solution and glacial acetic acid solution are added to selenous acid solution (selenium dioxide dissolved in wate...

Claims

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Application Information

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IPC IPC(8): C01B19/04
CPCC01B19/04C01P2006/80
Inventor 付勇王波朱刘
Owner 广东先导稀贵金属材料有限公司