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Method for preparing sodium-ion battery negative electrode material antimony sulfide from high-arsenic-antimony soot

A sodium-ion battery, high-arsenic antimony soot technology, applied in the direction of antimony sulfide, chemical instruments and methods, antimony compounds, etc., can solve the problem of losing valuable metals, and achieve the effect of avoiding the recovery process

Inactive Publication Date: 2021-06-04
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in order to ensure the purity of the product, the above method inevitably loses some valuable metals in the lengthy recovery process.

Method used

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  • Method for preparing sodium-ion battery negative electrode material antimony sulfide from high-arsenic-antimony soot
  • Method for preparing sodium-ion battery negative electrode material antimony sulfide from high-arsenic-antimony soot

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 5g of high-arsenic and antimony soot into an autoclave equipped with 50mL of 4mol / L NaOH solution, adjust the oxygen pressure by blowing oxygen, and filter to obtain the filter residue after the reaction is complete; after washing with water several times, use 2mol / L H 2 SO 4 solution to dissolve it, and detect the specific ion concentration (removal rate of As and Sb 3+ concentration in the solution); according to the molar ratio of Sb:S=1:2, add thiourea to the solution, stir evenly and then transfer to the autoclave; the hydrothermal temperature is controlled at 180°C, and the hydrothermal time is controlled at 80min , After the reaction is over, wash the product with alcohol several times and dry it at 80°C.

[0024] Weigh 0.07g of the above-prepared product, 0.02g of acetylene black (conductive agent), 0.01g of PVDF (HSV900, binder), and add an appropriate amount of NMP solution after fully grinding. , after vacuum drying at 120°C, cut into discs with a diame...

Embodiment 2

[0028] Add 5g of high arsenic and antimony soot into an autoclave equipped with 50mL of 5mol / L NaOH solution, adjust the oxygen pressure by blowing oxygen, and filter to obtain the filter residue after the reaction is complete; after washing with water for many times, use 3mol / L H 2 SO 4 solution to dissolve it, and detect the specific ion concentration (removal rate of As and Sb 3+ concentration in the solution); according to the molar ratio of Sb:S=1:2.5, add thiourea to the solution, stir evenly and then transfer to the autoclave; the hydrothermal temperature is controlled at 160°C, and the hydrothermal time is controlled at 100min , After the reaction is over, wash the product with alcohol several times and dry it at 80°C.

[0029] Weigh 0.07g of the above-prepared product, 0.02g of acetylene black (conductive agent), 0.01g of PVDF (HSV900, binder), and add an appropriate amount of NMP solution after fully grinding. , after vacuum drying at 120°C, cut into discs with a d...

Embodiment 3

[0031] Add 5g of high-arsenic and antimony soot into an autoclave equipped with 50mL of 6mol / L NaOH solution, adjust the oxygen pressure by blowing oxygen, and filter to obtain the filter residue after the reaction is complete; 2 SO 4 solution to dissolve it, and detect the specific ion concentration (removal rate of As and Sb 3+ Concentration in the solution); according to the molar ratio of Sb:S=1:3, add thiourea to the solution, stir evenly and transfer to the autoclave; the hydrothermal temperature is controlled at 140°C, and the hydrothermal time is controlled at 120min , After the reaction is over, wash the product with alcohol several times and dry it at 80°C.

[0032] Weigh 0.07g of the above-prepared product, 0.02g of acetylene black (conductive agent), 0.01g of PVDF (HSV900, binder), and add an appropriate amount of NMP solution after fully grinding. , after vacuum drying at 120°C, cut into discs with a diameter of 12 mm, and assemble them in a glove box with an ar...

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Abstract

The invention discloses a method for preparing a sodium-ion battery negative electrode material antimony sulfide from high-arsenic-antimony soot. The method comprises the following steps: by taking high-arsenic-antimony soot (comprising specific components of As2O3, As4O6, Sb2O3 and the like) as a raw material, forming soluble arsenate from arsenic by adopting a pressurized oxidation-alkaline leaching method, and filtering to remove the soluble arsenate; then dissolving antimony (Sb2O3) existing in a solid phase by using diluted hydrochloric acid to obtain a relatively pure antimony trichloride solution; under a stirring condition, adding a proper amount of a water-soluble sulfur source into the obtained solution, and uniformly mixing; transferring the obtained mixed solution into a reaction kettle and carrying out hydrothermal reaction at a certain temperature; after the hydrothermal reaction is finished, washing with alcohol for multiple times, and drying to obtain a product. According to the patent, a tedious metal extraction preparation process is avoided, antimony is directly converted into the sodium ion battery negative electrode material with higher practical value, and the recovery rate of antimony can reach 85% or above.

Description

technical field [0001] The invention belongs to the field of reclaiming high-arsenic and antimony soot to prepare sodium-ion battery negative electrode materials, and in particular relates to a sodium-ion battery negative electrode material Sb 2 S 3 and its preparation method. Background technique [0002] Thanks to the progress and development of modern technology, the recovery technology of various valuable metals has become more and more mature, which can effectively deal with the problems of complex ore composition and low grade. In the common copper and lead smelting process, harmful impurity metal elements such as arsenic, antimony, bismuth, which are common in complex ores, will be continuously enriched and accumulated in the process of smelting, refining, electrolysis, etc., making the smelting process of the target metal product become difficulty. Effective control of some impurity metal elements in the recovery and smelting process can not only ensure the normal...

Claims

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Application Information

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IPC IPC(8): C01G30/00C22B7/02C22B30/02
CPCC01G30/008C01P2002/72C01P2004/03C22B7/008C22B7/02C22B30/02Y02P10/20
Inventor 欧星叶隆苏石临张宝张佳峰
Owner CENT SOUTH UNIV
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