Process for synthesizing high-purity cobalt disulfide powder at normal pressure

A cobalt disulfide, high-purity technology, applied in chemical instruments and methods, inorganic chemistry, cobalt compounds, etc., can solve the problems of poor product crystallinity, hydrogen sulfide gas is easy to pollute the environment, etc., achieve low synthesis temperature, reduce synthesis cost, good safety effect

Inactive Publication Date: 2005-03-16
BEIJING GENERAL RES INST OF MINING & METALLURGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The product synthesized by this method has poor crystallinity, and hydrogen sulfide gas is easy to pollute the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] In a nitrogen protective atmosphere, 3.3 grams of high-purity cobalt powder (≥99.5%) and 7.2 grams of spectroscopically pure sulfur powder (making the excess weight of sulfur powder 2 times) were mixed in proportion, packed into a quartz glass tube, and the system was pumped After vacuuming to 0.1Pa for degassing, put the quartz glass tube into the muffle furnace, pass through argon protection, start heating up to 100°C, keep the temperature for 3 days, then raise the temperature to 200°C, keep the temperature for 6 days, and finally rise to 420°C ℃ for 2 hours, cooled to room temperature. Take out the material and grind it, sieve it to 0.074mm (200 mesh), take the material under the sieve and put it into another quartz glass tube, add sulfur according to the ratio of 2 times the theoretical weight excess, put it into the muffle furnace again, and pass it into the argon Protected by gas, the temperature was first raised to 200°C, kept at a constant temperature for 2 day...

Embodiment 2

[0015] According to the same materials and steps as in Example 1, 100 grams of cobalt powder and 162.7 grams of sulfur powder (1.5 times in excess) were added, the system was evacuated to 0.1 Pa for degassing, and the quartz glass tube was put into a muffle furnace. Introduce argon protection, start heating up to 100°C, keep the temperature for 3 days, then raise the temperature to 200°C, keep the temperature for 5 days, then raise the temperature to 440°C and keep the temperature for 2 hours, finally raise the temperature to 700°C and keep the temperature for 1 hour, then cool to room temperature. After cooling, grinding, and sieving, add sulfur at a ratio of 1.5 times the theoretical excess, and refill the quartz tube. Under the same conditions, start to heat up to 200°C, keep the temperature for 2 days, and then raise the temperature to 380°C. Keep the temperature constant for 7 days, finally rise to 440°C and keep the temperature constant for 2 hours, then cool to room temp...

Embodiment 3

[0017] According to the same materials and steps as in Example 1, 300 grams of cobalt powder and 650.8 grams of sulfur powder (2 times in excess) were added, and after the system was evacuated to 0.01 Pa for degassing, the quartz glass tube was put into a muffle furnace and passed through Protected by argon, the temperature was first raised to 150°C, kept at a constant temperature for 3 days, then raised to 200°C, kept at a constant temperature for 6 days, finally raised to 440°C, kept at a constant temperature for 2 hours, and cooled to room temperature. After cooling, grinding, and sieving, add sulfur according to the ratio of 1.5 times the theoretical excess, and repack it into the quartz tube. After 7 days, the temperature was raised to 420°C for 2 hours and cooled to room temperature. Obtained 625.1 g of cobalt disulfide powder with a purity greater than 99%.

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Abstract

The invention relates to a process for preparing high purity fine granule cobalt disulfide powder by using single mass powder as raw material through twice high temperature synthesis under ordinary pressure system, the method is conducted in vacuum or inert atmosphere protection such as in argon or in nitrogen.

Description

technical field [0001] The invention belongs to the technical field of inorganic synthesis, and particularly relates to a method for obtaining high-purity, fine-grained cobalt disulfide powder by secondary high-temperature synthesis using simple powder as a raw material under normal pressure system. The high-purity cobalt disulfide powder It can be used as the positive stage material of high temperature thermal battery. Background technique [0002] High-purity cobalt disulfide powder can be used as an electrode material for lithium / disulfide thermal batteries to increase the high-temperature stability of the electrode and improve its electrochemical performance, which has attracted widespread attention in recent years. The synthesis method reported in "Inorganic Compound Synthesis Handbook" (published in October, 1983) mainly contains: (1) using cobalt powder and sulfur powder in a molar ratio of 1:1 as raw materials, mixing and vacuum sealing in a q...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/00
Inventor 李强唐威
Owner BEIJING GENERAL RES INST OF MINING & METALLURGY
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