Method for preparing thin-layer graphene negative electrode active material by utilizing antibiotic bacterium dregs

A technology of negative electrode active material and antibiotic slag, which is applied in the field of preparing thin-layer graphene negative electrode active material from antibiotic slag, can solve the problems of complex process, low economic value, and difficulty in treating harmful solid waste of bacterial slag.

Active Publication Date: 2021-01-15
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problems of complex process, long production cycle, low yield, high cost, difficulty in the treatment of harmful solid waste of existing fungus slag, and low economic value of treatment in the existing grap...

Method used

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  • Method for preparing thin-layer graphene negative electrode active material by utilizing antibiotic bacterium dregs
  • Method for preparing thin-layer graphene negative electrode active material by utilizing antibiotic bacterium dregs
  • Method for preparing thin-layer graphene negative electrode active material by utilizing antibiotic bacterium dregs

Examples

Experimental program
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Effect test

Embodiment 1

[0078] Take 20g of dry oxytetracycline slag raw material, first disperse it in 80mL of 20wt.% HF acid solution, stir for 4h, after pumping and filtering, then add it into 80mL of 18wt.%HCl acid solution, stir for 4h, then pass solid Liquid separation, washing to neutrality, suction filtration and drying to obtain dried bacteria residue powder (acid-treated bacteria residue).

[0079] Take 2g of dried bacteria residue powder (acid-treated bacteria residue), add it to 20mL of water, stir for 5min, and add 3g of NaOH, and heat it at 200°C for 12h. After cooling, filter to obtain the liquid part; add 2g Fe(NO 3) 3 .9H 2 O, after stirring for 10 minutes, stir and evaporate to dryness at 100°C, place in a tube furnace filled with nitrogen, first heat at 500°C for 2 hours, continue to heat up to 800°C for 2 hours (heating rate is 5°C / min), cool to room temperature and take out. Pickling, water washing to neutrality and then vacuum drying to obtain a thin-layer graphene negative ...

Embodiment 2

[0082] Compared with Example 1, the difference mainly lies in changing the temperature of the liquefaction process, specifically:

[0083] Take 20g of dry oxytetracycline slag raw material, first disperse it in 80mL of 20wt.% HF acid solution, stir for 4h, after pumping and filtering, then add it into 80mL of 18wt.%HCl acid solution, stir for 4h, then pass solid Liquid separation, washing to neutrality, suction filtration and drying to obtain dried bacteria residue powder (acid-treated bacteria residue).

[0084] Take 2g of dried bacteria residue powder (acid-treated bacteria residue), add it to 20mL of water, stir for 5min, and add 3g of NaOH, and heat it at 120°C for 12h. After cooling, filter to obtain the liquid part; add 2g Fe(NO 3 ) 3 .9H 2 O, after stirring for 10 minutes, stir and evaporate to dryness at 100°C, place in a tube furnace filled with nitrogen, first heat at 500°C for 2 hours, continue to heat up to 500°C for 2 hours (heating rate is 5°C / min), cool to ...

Embodiment 3

[0087] Compared with Example 1, the difference mainly lies in changing the temperature of the liquefaction process, specifically:

[0088] Take 20g of dry oxytetracycline slag raw material, first disperse it in 80mL of 20wt.% HF acid solution, stir for 4h, after pumping and filtering, then add it into 80mL of 18wt.%HCl acid solution, stir for 4h, then pass solid Liquid separation, washing to neutrality, suction filtration and drying to obtain dried bacteria residue powder (acid-treated bacteria residue).

[0089] Take 2g of dried fungal residue powder (acid-treated fungal residue), add it to 20mL of water, stir for 5min, add 3g of NaOH, and heat at 210°C for 10h. After cooling, filter to obtain the liquid part; add 2g Fe(NO 3 ) 3 .9H 2 O, after stirring for 10 minutes, stir and evaporate to dryness at 100°C, place in a tube furnace filled with nitrogen, first heat at 500°C for 2 hours, continue to heat up to 800°C for 2 hours (heating rate is 5°C / min), cool to room temper...

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Abstract

The invention belongs to the technical field of waste utilization and lithium ion battery material preparation, and particularly discloses a method for preparing a thin-layer graphene negative electrode active material from antibiotic bacterium dregs, which comprises the following steps of: carrying out hydrothermal liquefaction on an aqueous solution containing antibiotic bacterium dregs and alkali, and carrying out solid-liquid separation to obtain a bacterium dreg solution; adding a transition metal source into the bacterium dreg solution, carrying out dehydration treatment after liquid phase mixing, and then carrying out heat treatment, the heat treatment comprising first-stage heat treatment and second-stage heat treatment which are carried out in sequence, the temperature of the first-stage heat treatment being 400-600 DEG C, the temperature of the second-stage heat treatment being 700-900 DEG C, and the heating rate in the heat treatment process being 2-10 DEG C/min; and washingand drying a product obtained by heat treatment to obtain the thin-wall graphene. According to the invention, efficient utilization of the waste material is realized, and the graphene negative electrode material with high thin wall and high electrochemical performance is co-produced.

Description

technical field [0001] The invention belongs to the technical field of graphene materials, and in particular relates to a method for preparing thin-layer graphene negative electrode active materials from antibiotic bacteria residues. Background technique [0002] Graphene is a two-dimensional crystal material with a hexagonal honeycomb lattice formed by a single layer of carbon atoms closely arranged. The special structure endows it with excellent physical and chemical properties, so it is widely used in catalysis, storage Energy, medicine and other fields. At present, the preparation methods of graphene mainly include micromechanical exfoliation method, graphite oxide reduction method, crystal film growth epitaxial method, silicon carbide surface epitaxial growth method and chemical vapor deposition method, etc., but these methods have different defects. The micro-mechanical exfoliation method has low production efficiency and poor controllability; the graphene prepared by...

Claims

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Application Information

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IPC IPC(8): C01B32/184C01B32/194H01M4/587H01M10/0525
CPCC01B32/184C01B32/194H01M4/587H01M10/0525C01B2204/22C01B2204/32C01B2204/30Y02E60/10
Inventor 唐晶晶丁静杨娟周向阳郭龙龙王炯
Owner CENT SOUTH UNIV
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