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Method for synthesizing high-purity nickel disulfide

A technology of nickel disulfide and synthesis method, applied in the direction of nickel sulfide, etc., to achieve the effects of simple process technology, mild preparation conditions, and cheap raw materials

Active Publication Date: 2015-01-07
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the above-mentioned technical problems existing in the preparation of existing high-purity nickel disulfide, the present invention provides a synthesis method of high-purity nickel disulfide with simple process and low cost. The present invention has the advantages of mild reaction conditions, low cost, simple operation and high yield Advantages of high purity

Method used

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  • Method for synthesizing high-purity nickel disulfide

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Embodiment 1

[0019] Dissolve 6mmol of nickel nitrate in 250mL of deionized water, add nitric acid to adjust the pH value of the solution to 0.7, then add 35mmol of thiourea, fully dissolve, move to a 300mL closed hydrothermal reaction kettle, heat up to 200°C, react for 24 hours, and the reaction is over Finally, the solution was taken out, filtered, washed with water, washed with alcohol, and vacuum dried to obtain 0.70 g of nickel disulfide with a purity greater than 99%. Calculated based on the reacted metallic nickel, the yield of nickel disulfide was 94.9%.

Embodiment 2

[0021] Dissolve 6mmol of nickel sulfate in 250mL of deionized water, add sulfuric acid to adjust the pH value of the solution to 0.6, then add 35mmol of sodium sulfide, after fully dissolved, move to a 300mL closed hydrothermal reaction kettle, heat up to 220°C, react for 12 hours, and the reaction ends Finally, the solution was taken out, filtered, washed with water, washed with alcohol, and vacuum dried to obtain 0.63 g of nickel disulfide with a purity greater than 99%. Calculated based on the reacted metallic nickel, the yield of nickel disulfide was 86.2%.

Embodiment 3

[0023] Dissolve 6mmol of nickel acetate in 250mL of deionized water, add acetic acid to adjust the pH value of the solution to 0.5, then add 35mmol of thioacetamide, fully dissolve, move to a 300mL closed hydrothermal reaction kettle, heat up to 200°C, and react for 36 hours. After the reaction, the solution was taken out, filtered, washed with water, washed with alcohol, and vacuum-dried to obtain 0.66 g of nickel disulfide with a purity greater than 99%. Calculated based on the reacted metallic nickel, the yield of nickel disulfide was 89.4%.

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Abstract

The invention discloses a method for synthesizing high-purity nickel disulfide. The method comprises the following steps: dissolving soluble nickel salt into deionized water, dropwise adding acid to adjust the pH value of the solution to be 0-3, further adding a water-soluble sulfur-containing compound with the molar ratio of molar ratio to nickel to be 4-12, stirring to completely dissolve, pouring the mixture into a sealed hydrothermal reaction kettle, reacting for 6-72 hours at 180-300 DEG C, washing with water and alcohol, and performing vacuum drying, thereby obtaining the high-purity nickel disulfide. The method adopts a one-step hydrothermal method to prepare the high-purity nickel disulfide, is cheap in raw material, simple in process, gentle in preparation condition, free of protecting gas, high in product purity, is a high-efficiency and environment-friendly synthesis method, and can be used for synthesizing high-purity cobalt disulfide, iron disulfide and the like.

Description

technical field [0001] The invention relates to a method for synthesizing high-purity nickel disulfide. Background technique [0002] Nickel sulfide is an electronic, energy and chemical material that has attracted more and more attention in recent years. It has a unique electronic structure, molecular structure and excellent optical, electrical and magnetic properties. Battery storage devices, infrared detectors, hydrodenitrogenation reactions, hydrodesulfurization reactions, etc. have broad industrial application prospects. Nickel sulfide is a very complex system, and there are many phase compositions with different proportions, such as Ni 3 S 2 、Ni 6 S 5 、Ni 7 S 6 、Ni 9 S 8 , NiS, Ni 3 S 4 and NiS 2 Wait. Therefore, it is very difficult to control the reaction process to prepare single-phase nickel sulfide powder. [0003] Currently preparing NiS 2 There are many ways. Chinese patent CN 1240765A discloses a method for preparing high-purity NiS 2 The method...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/11
Inventor 杨运泉王威燕李路张锟仵奎
Owner XIANGTAN UNIV
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