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Preparation method of high-purity antimony sulfide

A high-purity technology of antimony sulfide, applied in antimony sulfide, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of large environmental pollution, low purity of antimony sulfide, difficulty in large-scale production, etc., to expand the scope of use, remove impurities, etc. The effect of high removal rate and high production efficiency

Active Publication Date: 2020-05-08
KUNMING DIBOO TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In view of the above-mentioned deficiencies in the prior art, the purpose of the present invention is to provide a preparation method of high-purity antimony sulfide, aiming to solve the problem of complex production process of existing antimony sulfide, The problem of high environmental pollution, difficulty in large-scale production and low purity of prepared antimony sulfide

Method used

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  • Preparation method of high-purity antimony sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] 1. Mix 210Kg granular antimony alloy (containing Sb~99.9%, Pb~0.05%, Bi~0.053%, As~0.02%) and 85Kg sulfur powder with a stirrer, then add it into a closed container and heat to Insulate at 400°C and react for 2 hours to obtain 291.40Kg of low-purity antimony sulfide;

[0036] 2. Put the low-purity antimony sulfide in a vacuum furnace, the condensing area is 35cm away from the heating area, vacuumize to 5-50Pa, slowly raise the temperature to 950°C, keep it warm for 8h under this condition, control the temperature of the condensing area to 150°C, and distill Collect the mixture 285.4Kg of low-boiling impurity and antimony sulfide in volatile matter after completion;

[0037] 3. Put the mixture of low-boiling point impurities and antimony sulfide in a vacuum furnace that does not adhere to impurities, add 1% sulfur, and homogenize and synthesize the collected antimony sulfide at 560°C under normal pressure; Then evacuate to 5-50Pa, slowly raise the temperature to 630°C, ...

Embodiment 2

[0039] 1. Mix 210Kg of granular antimony alloy (containing Sb~97.42%, Pb~0.83%, Bi~0.53%, Cu~0.37%, Fe~0.29%, As~0.02%) with 85Kg of sulfur powder and 85Kg of sulfur powder After fully mixed with the container, add it into a closed container, heat it to 400°C and keep it warm, and the reaction time is 1.5h to obtain 293.35Kg of low-purity antimony sulfide;

[0040] 2. Put the low-purity antimony sulfide in a vacuum furnace, the condensing area is 80cm away from the heating area, vacuumize to 5-50Pa, slowly raise the temperature to 1200°C, keep it warm for 5h under this condition, control the temperature of the condensing area to 200°C, and distill Collect the mixture 285.43Kg of low-boiling impurity and antimony sulfide in volatile matter after completion;

[0041] 3. Put the mixture of low-boiling point impurities and antimony sulfide in a vacuum furnace that does not adhere to impurities, add 2% sulfur, and homogenize and synthesize the collected antimony sulfide at 580°C un...

Embodiment 3

[0043] 1. Put 300Kg of Sb-40% antimony sulfide concentrate in a vacuum furnace, the condensation area is 50cm away from the heating area, vacuumize to 5-50Pa, slowly raise the temperature to 1100°C, keep the temperature for 7 hours under this condition, and control the temperature of the condensation area At 200°C, 228.4Kg of a mixture of low-boiling impurities and antimony sulfide was collected in the volatile matter after the distillation;

[0044] 2. Put the mixture of low-boiling-point impurities and antimony sulfide in a vacuum furnace that does not adhere to impurities, add 2% sulfur, and homogenize and synthesize the collected antimony sulfide at 600°C under normal pressure; Then evacuate to 5-50Pa, slowly raise the temperature to 680°C, and keep it warm for 3 hours under this condition. After the distillation is completed, 158.6Kg of residue is collected. After testing, the obtained residue is Sb 2 S 3 , and its purity is 99.92%.

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Abstract

The invention discloses a preparation method of high-purity antimony sulfide. The method comprises the following steps: putting low-purity antimony sulfide or antimony sulfide concentrate into a vacuum furnace, carrying out first distillation under a first preset temperature condition to volatilize impurities with boiling points lower than that of antimony sulfide and antimony sulfide at the sametime, and collecting antimony sulfide only containing low-boiling-point impurities by controlling vacuum distillation and condensation conditions; placing the antimony sulfide containing the low-boiling-point impurities into another vacuum furnace; and homogenizing and re-synthesizing the collected antimony sulfide under the normal pressure and the second preset temperature condition, then carrying out secondary distillation under the vacuum condition for impurity removal, so that impurities with the boiling point lower than that of antimony sulfide volatilize wherein antimony sulfide remains,thereby preparing high-purity antimony sulfide, the second preset temperature being lower than the first preset temperature. According to the method, chemical agents such as acid and alkali are not used, three-waste emission is avoided, the technological process is simple and easy to operate, and the production efficiency is high; the purity of antimony sulfide prepared by the method is up to 99.9% or above.

Description

technical field [0001] The invention relates to the field of nonferrous metal metallurgy, in particular to a method for preparing high-purity antimony sulfide. Background technique [0002] Antimony sulfide is a black solid powder with a melting point of 548°C. The antimony oxide produced by its pyrolysis and the metal antimony produced in the presence of a reducing agent can prevent the oxidative combustion of materials at high temperatures, maintain the frictional stability of materials, and improve The anti-combustion performance of the material can also reduce the decomposition rate of the organic binder at high temperature, improve the service life of the material, and play the role of a high-temperature inorganic binder and a lubricating friction modifier. In addition, the hardness of antimony sulfide is relatively low in high temperature reaction, which can reduce the noise and vibration generated by the friction material during braking. Antimony sulfide's outstandin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G30/00
CPCC01G30/008C01P2006/80
Inventor 戴卫平陈巍郑春阳韩龙李建国宋春丽陈浩马祥亚
Owner KUNMING DIBOO TECH
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