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Preparation method of Li/Na ion battery anode material Fe<1-x>S/C

A technology for sodium ion batteries and negative electrode materials, which is applied to battery electrodes, circuits, electrical components, etc., can solve the problems of high pollution degree and difficult wastewater treatment, and achieve the effects of high synthesis efficiency, effective reuse and simple preparation method.

Active Publication Date: 2018-09-28
苏州茂开电子材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Sulfur-containing petroleum sewage is purple-red and accompanied by a strong stench. Its main components are sulfide, ammonia, oil, volatile phenol and other substances. Its pollution level is high and wastewater treatment is difficult.

Method used

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  • Preparation method of Li/Na ion battery anode material Fe&lt;1-x&gt;S/C

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Experimental program
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Effect test

Embodiment 1

[0045] A kind of lithium / sodium ion battery anode material Fe 1-x The preparation method of S / C comprises steps as follows:

[0046] Take 10mL of sulfur-containing petroleum sewage into a three-necked flask, add 1.5ml of 15wt℅ hydrogen peroxide aqueous solution, and stir at 50°C for 30min to obtain pretreated sulfur-containing petroleum sewage; then add 30mL of 0.1mol L -1 The ferric chloride aqueous solution is slowly added dropwise to the above-mentioned pretreated sulfur-containing petroleum sewage, continuously stirred and added 2ml 2wt℅ethylenediammonium tetraacetic acid aqueous solution to make the pH value to 4, and stirred at room temperature for 2h to obtain a uniform mixed solution; The mixed solution was put into a reaction kettle, hydrothermally treated at 180°C for 24 hours, then naturally cooled to room temperature, and the precipitate obtained by centrifugation was dried at 60°C to obtain a black powder; the black powder was washed twice with water and then wash...

Embodiment 2

[0053] A kind of lithium / sodium ion battery anode material Fe 1-x The preparation method of S / C comprises steps as follows:

[0054] Take 10mL of sulfur-containing petroleum sewage into a three-necked flask, add 0.5ml of 15wt℅ peracetic acid aqueous solution, and stir at 40°C for 40min to obtain pretreated sulfur-containing petroleum sewage; then add 40mL of 0.1mol L -1 The ferric nitrate aqueous solution is slowly added dropwise to the above-mentioned pretreated sulfur-containing petroleum sewage, continuously stirred and added 2ml 2wt℅ citric acid aqueous solution to make the pH value to 2, and stirred at room temperature for 2 hours to obtain a uniform mixed solution; Put it into the reaction kettle, hydrothermally treat it at 150°C for 48 hours, then cool it naturally to room temperature, and dry the precipitate obtained by centrifugation at 60°C to obtain a black powder; wash the black powder twice with water and once with ethanol, and dry at 100°C Dry for 2 hours, and t...

Embodiment 3

[0057] A kind of lithium / sodium ion battery anode material Fe 1-x The preparation method of S / C comprises steps as follows:

[0058] Take 10mL of sulfur-containing petroleum sewage into a three-necked flask, add 2ml of 15wt℅ ammonium persulfate aqueous solution, and stir at 60°C for 20min to obtain pretreated sulfur-containing petroleum sewage; then add 25mL of 0.1mol L -1 The ferric chloride aqueous solution is slowly added dropwise to the above-mentioned pretreated sulfur-containing petroleum sewage, stirring continuously and adding 2ml 2wt℅ glycine acid aqueous solution to make the pH value to 5, stirring at room temperature for 2 hours to obtain a uniform mixed solution; the mixed solution Put it into a reaction kettle, heat it at 220°C for 10 hours, cool it down to room temperature naturally, and dry the precipitate at 60°C after centrifugation to obtain a black powder; wash the black powder twice with water and once with ethanol, and then dry it at 100°C Dry for 2 hours...

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Abstract

The invention provides a preparation method of a Li / Na ion battery anode material Fe<1-x>S / C. The preparation method includes the steps of: 1) performing oxidizing reaction to sulfur-bearing petroleumwastewater with an oxidant to obtain pretreated sulfur-bearing petroleum wastewater; 2) adding a ferric salt water solution and an additive to the pretreated sulfur-bearing petroleum wastewater untilpH value is 2-5, and uniformly mixing the components; 3) performing hydrothermal treatment at 150-220 DEG C for 10-48 h, and separating, washing, drying and grinding the product to obtain a precursor; 4) under protection of inert gas, performing heat preservation to the precursor for 1-3 h at 300-400 DEG C and calcining the precursor for 5-12 h at 600-800 DEG C. The preparation method employs theindustrial waste, sulfur-bearing petroleum wastewater, as a main raw material, is simple and low-cost and achieves effective reutilization of wastes. The anode material has excellent electrochemicalperformance and is high in specific discharge capacity.

Description

technical field [0001] The invention relates to a lithium / sodium ion battery negative electrode material Fe 1-x The preparation method of S / C belongs to the technical field of lithium / sodium ion battery negative electrode materials. Background technique [0002] The high capacity and environmental friendliness of iron-based materials make them suitable for Li-ion or Na-ion batteries. However, the practical application of iron-based materials is still limited by the rapid capacity fading, because the severe volume expansion during ion intercalation / extraction leads to the structural collapse of iron-based materials, thereby shortening their cycle life. In order to solve this problem and improve its electrochemical performance, iron-based materials and carbon are combined to form nanoscale carbon composites, such as: graphene / Fe 3 o 4 , Fe 1-x S / C, FeS / C and Fe 3 o 4 / C etc. These carbons can regulate the Li + / Na + The volume expansion induced during intercalation / ex...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62
CPCH01M4/364H01M4/5815H01M4/625Y02E60/10
Inventor 何文闫珍珍张旭东
Owner 苏州茂开电子材料有限公司
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