Method for preparing thin-layer graphene/transition metal fluoride composite positive electrode active material by using antibiotic bacteria residue

A technology of antibiotic slag and thin-layer graphene, which is applied in the direction of active material electrodes, negative electrodes, battery electrodes, etc., can solve the problems of low conductivity and poor cycle stability of transition metal fluorides, and achieve rapid charge transmission , Improve electrical conductivity, realize the effect of energy utilization and high-value utilization

Active Publication Date: 2022-03-29
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to solve the problems of low electrical conductivity and poor cycle stability of transition metal fluorides, using antibiotic slag as raw material to realize low-cost, harmless and high-value utilization, and to provide a thin film prepared from antibiotic slag. Method for layer graphene / transition metal fluoride positive electrode active material (the present invention is also referred to as thin layer graphene / transition metal fluoride composite positive electrode or abbreviated as positive electrode material)

Method used

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  • Method for preparing thin-layer graphene/transition metal fluoride composite positive electrode active material by using antibiotic bacteria residue
  • Method for preparing thin-layer graphene/transition metal fluoride composite positive electrode active material by using antibiotic bacteria residue
  • Method for preparing thin-layer graphene/transition metal fluoride composite positive electrode active material by using antibiotic bacteria residue

Examples

Experimental program
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Effect test

Embodiment 1

[0080] Using oxytetracycline slag as the carbon precursor, take 30g of dry antibiotic slag raw material, first disperse it into 120mL of 20wt.% HF acid solution, stir for 4h, and then add it to 120mL of 18wt.% HCl acid solution after suction filtration solution, stirred for 4h, suction filtered and washed (referring to water washing, the washing of the acid treatment process in the following cases all refers to water washing) and then dried after neutralization to obtain dry bacterial residue (pretreated bacterial residue).

[0081] Take 2g of dried fungal residue powder (pretreated fungal residue), add it to 20mL water, stir for 5min, add 3g of NaOH, and heat it at 200°C for 12h. Carry out solid-liquid separation to the hydrothermal system, obtain the solution part (bacteria residue liquid), add 2gFe(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 argon, first calcinate at 500°C for 2h, continue to...

Embodiment 2

[0085] Compared with Example 1, the difference mainly lies in the amount of iron salt in the alkali of the control liquefaction process and the heat treatment process, specifically:

[0086] Using oxytetracycline slag as the carbon precursor, take 30g of dry antibiotic slag raw material, first disperse it into 120mL of 20wt.% HF acid solution, stir for 4h, and then add it to 120mL of 18wt.% HCl acid solution after suction filtration solution, stirred for 4 hours, filtered with suction, washed neutral and then dried to obtain dry scum (pretreated scum).

[0087] Take 2g of dried fungus residue powder (pretreated fungus residue), add it to 20mL water, stir for 5min, add 1g of NaOH, and heat it at 200°C for 12h. Add 1gFe(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 argon, first calcinate at 500°C for 2h, continue to heat up to 800°C for 2h (heating rate is 5°C / min), cool to room temperature and tak...

Embodiment 3

[0090] Compared with Example 1, the difference mainly lies in the amount of iron salt in the alkali of the control liquefaction process and the heat treatment process, specifically:

[0091] Using oxytetracycline slag as the carbon precursor, take 30g of dry antibiotic slag raw material, first disperse it into 120mL of 20wt.% HF acid solution, stir for 4h, and then add it to 120mL of 18wt.% HCl acid solution after suction filtration In the solution, stir for 4 hours, filter with suction and wash neutral, then dry with suction to obtain dry bacteria residue (pretreated bacteria residue). Take 2g of dried fungus residue powder (pretreated fungus residue), add it to 20mL water, stir for 5min, add 4g of NaOH, and heat at 200°C for 12h. Add 6gFe(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 argon, first calcinate at 500°C for 2h, continue to heat up to 800°C for 2h (heating rate is 5°C / min), cool to r...

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Abstract

The invention belongs to the technical field of bacterial residue solid waste treatment and battery materials, and specifically relates to a method for preparing a thin-layer graphene / transition metal fluoride composite positive electrode active material by using antibiotic bacterial residue. Performing hydrothermal liquefaction with an aqueous alkali solution, followed by solid-liquid separation to obtain a bacterial residue solution; adding a transition metal M source to the bacterial residue solution, mixing the liquid phases, performing dehydration treatment, and then performing heat treatment; the heat treatment includes sequentially performing The first stage of pretreatment and the second stage of heat treatment; the product obtained by the heat treatment and the fluorine source are subjected to fluorination and annealing treatment to obtain the thin-layer graphene / M metal fluoride composite positive electrode active material. The invention also provides the material prepared by the preparation method and its application in lithium batteries. The technical scheme described in the present invention can realize the double synergy of chemical and physical structures, which helps to significantly improve the electrochemical performance of materials.

Description

technical field [0001] The invention belongs to the technical field of lithium-ion battery electrode materials, and in particular relates to a method for preparing thin-sheet graphene / transition metal fluoride composite positive electrodes from antibiotic bacteria residues. Background technique [0002] Lithium-ion batteries are widely used in portable electronic devices, new energy vehicles, energy storage power systems and other fields due to their high operating voltage, no memory effect, high energy density, and low self-discharge rate. With the development of new energy technologies such as electric vehicles, traditional lithium-ion battery cathode materials, such as lithium cobalt oxide, lithium iron phosphate, ternary materials, etc., are subject to lithium deintercalation mechanisms, and their specific capacity is difficult to meet the needs of the next generation of high energy density lithium batteries. ion battery needs. Therefore, the development of alternative ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/62H01M4/58H01M10/0525
CPCH01M4/625H01M4/628H01M4/582H01M4/624H01M10/0525H01M2004/027Y02E60/10
Inventor 杨娟丁静唐晶晶周向阳刘晓剑王炯
Owner CENT SOUTH UNIV
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