Method for preparing thin-layer graphene negative electrode active material by using antibiotic bacteria residue

A technology of negative electrode active material and antibiotic slag, which is applied in the field of preparation of thin-layer graphene negative electrode active material from antibiotic slag, can solve the problems of low economic value, long production cycle, and difficult disposal of harmful solid waste of bacteria slag, and achieves Catalytic graphitization and the effect of changing the structure of carbon materials, improving the order of atomic arrangement, and excellent electrochemical performance

Active Publication Date: 2022-03-22
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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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 graphene preparation method. The first purpose is to provide a method for preparing thin-layer graphene negative electrode active material by using antibiotic slag, aiming at realizing the treatment of harmful solid waste of bacterium slag and co-producing thin-layer graphene

Method used

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  • Method for preparing thin-layer graphene negative electrode active material by using antibiotic bacteria residue
  • Method for preparing thin-layer graphene negative electrode active material by using antibiotic bacteria residue
  • Method for preparing thin-layer graphene negative electrode active material by using antibiotic bacteria residue

Examples

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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 el...

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 ro...

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 temperat...

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Abstract

The invention belongs to the technical field of waste material utilization and lithium ion battery material preparation, and specifically discloses a method for preparing a thin-layer graphene negative electrode active material by using antibiotic slag. The aqueous solution containing antibiotic slag and alkali is hydrothermally liquefied, and then solidified. liquid separation to obtain a bacterial residue solution; adding a transition metal source to the bacterial residue solution, mixing the liquid phases, performing dehydration treatment, and then performing heat treatment; the heat treatment includes the first stage of pretreatment and the second stage of heat treatment in sequence; The temperature of the first stage of heat treatment is 400-600°C; the temperature of the second stage of heat treatment is 700-900°C; and the heating rate of the heat treatment process is 2-10°C / min; the product obtained by heat treatment is washed and dried, That is, the thin-walled graphene is obtained. The invention realizes the high-efficiency utilization of the waste materials, and co-produces the graphene negative electrode material with high thin wall and high electrochemical performance.

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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Patent Type & Authority Patents(China)
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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