CN103647081B - The preparation method of ascorbic acid modified graphite - Google Patents

The preparation method of ascorbic acid modified graphite Download PDF

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Publication number
CN103647081B
CN103647081B CN201310568784.3A CN201310568784A CN103647081B CN 103647081 B CN103647081 B CN 103647081B CN 201310568784 A CN201310568784 A CN 201310568784A CN 103647081 B CN103647081 B CN 103647081B
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China
Prior art keywords
graphite
ascorbic acid
acid modified
mixture
modified graphite
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Expired - Fee Related
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CN201310568784.3A
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Chinese (zh)
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CN103647081A (en
Inventor
王维利
范未峰
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CHENGDU XINGNENG NEW MATERIALS CO LTD
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CHENGDU XINGNENG NEW MATERIALS CO LTD
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/62Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention provides a kind of preparation method of ascorbic acid modified graphite, belong to chemical cell preparation field.The present invention by after potassium permanganate and native graphite are carried out oxidation processes, then carries out ultrasonic, sintering with ascorbic acid, obtains a kind of negative material of ascorbic acid modified graphite.The modified graphite that method provided by the invention is prepared is the complex carbon material with nucleocapsid structure, improve the chemical property of graphite material, not only can improve the compatibility of electrode and electrolyte, in cyclic process subsequently, stop the insertion of solvent, reduce irreversible loss; And its external sheath thing secures graphite flake, at Li +when deintercalation changes graphite volume repeatedly, stop coming off of graphite linings.

Description

The preparation method of ascorbic acid modified graphite
Technical field
The invention belongs to chemical cell preparation field, particularly relate to a kind of preparation method of ascorbic acid modified graphite.
Background technology
Native graphite is widely used as the negative material of lithium ion battery, but the compatibility of native graphite and electrolyte is poor, in embedding/de-lithium process, easily there is the stripping of graphite linings and cause cycle performance to decline, thus limiting the application of pure natural graphite in lithium ion battery.
Along with the extensively universal of various small-sized portable electronic product and electric bicycle and development, the commercial development of New Generation of Electric Vehicle (EV), hybrid vehicle (HEV), has higher requirement to the energy density of lithium ion battery and performance.Traditional carbon-based negative electrode material all can not meet the needs of Novel cathode material for lithium ion battery of future generation in specific capacity, specific energy, and therefore the carbon-based negative electrode material of development of new has very important meaning.
Summary of the invention
A preparation method for ascorbic acid modified graphite, is characterized in that comprising the following steps:
(1) with potassium permanganate, native graphite is carried out oxidation processes, obtain mixture A;
(2) mixture A and ascorbic acid are mixed in proportion, and carry out ultrasonic disperse in deionized water, obtain mixture B;
(3) mixture B is carried out drying, then carburizing sintering 2 ~ 4 hours under the inert gas shielding of 700 DEG C ~ 900 DEG C, obtains described ascorbic acid modified graphite.
Preferably, the mass ratio of the native graphite described in step (1) and potassium permanganate is 1:(0.05 ~ 0.2).
Preferably, the oxidation processes described in step (1) comprises the following steps: oxidizing temperature is 800 DEG C ~ 1000 DEG C, and oxidization time is 10 ~ 40 seconds.
Preferably, the mass ratio of the mixture A described in step (2) and ascorbic acid is 2:(0.5 ~ 1).
Beneficial effect of the present invention is as follows:
1. the present invention adopts ascorbic acid modified graphite, and ascorbic acid has advantages such as being extensively easy to get, cheap, can reduce the cost of modified graphite, reduces it produces battery cost as negative material further.
2. with the modified graphite that method provided by the invention is prepared from, at high-graphitized carbon material surface coated one deck ascorbic acid amorphous carbon material, prepare the complex carbon material with nucleocapsid structure, improve the chemical property of graphite material, not only can improve the compatibility of electrode and electrolyte, in cyclic process subsequently, stop the insertion of solvent, reduce irreversible loss; And its external sheath thing secures graphite flake, at Li +when deintercalation changes graphite volume repeatedly, stop coming off of graphite linings.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
embodiment 1
A preparation method for ascorbic acid modified graphite, is characterized in that comprising the following steps:
(1) be 1:0.05 mixing by the mass ratio of native graphite and potassium permanganate, at temperature is 800 DEG C, oxidation processes 40 seconds, obtains mixture A;
(2) by mixture A and ascorbic acid be the ratio mixing of 2:1 in mass ratio, and carry out ultrasonic disperse in deionized water, obtain mixture B;
(3) mixture B is carried out drying, then carburizing sintering 3 ~ 4 hours under the inert gas shielding of 700 DEG C ~ 800 DEG C, obtains described ascorbic acid modified graphite.
embodiment 2
A preparation method for ascorbic acid modified graphite, is characterized in that comprising the following steps:
(1) be 1:0.2 mixing by the mass ratio of native graphite and potassium permanganate, at temperature is 1000 DEG C, oxidation processes 10 seconds, obtains mixture A;
(2) by mixture A and ascorbic acid be the ratio mixing of 2:0.8 in mass ratio, and carry out ultrasonic disperse in deionized water, obtain mixture B;
(3) mixture B is carried out drying, then carburizing sintering 2 ~ 3 hours under the inert gas shielding of 800 DEG C ~ 900 DEG C, obtains described ascorbic acid modified graphite.
embodiment 3
A preparation method for ascorbic acid modified graphite, is characterized in that comprising the following steps:
(1) be 1:0.1 mixing by the mass ratio of native graphite and potassium permanganate, at temperature is 900 DEG C, oxidation processes 30 seconds, obtains mixture A;
(2) by mixture A and ascorbic acid be the ratio mixing of 2:0.5 in mass ratio, and carry out ultrasonic disperse in deionized water, obtain mixture B;
(3) mixture B is carried out drying, then carburizing sintering 2.5 hours under the inert gas shielding of 750 DEG C ~ 850 DEG C, obtains described ascorbic acid modified graphite.

Claims (1)

1. a preparation method for ascorbic acid modified graphite, is characterized in that comprising the following steps:
(1) with potassium permanganate, native graphite is carried out oxidation processes, obtain mixture A;
(2) mixture A and ascorbic acid are mixed in proportion, and carry out ultrasonic disperse in deionized water, obtain mixture B;
(3) mixture B is carried out drying, then carburizing sintering 2 ~ 4 hours under the inert gas shielding of 700 DEG C ~ 900 DEG C, obtains described ascorbic acid modified graphite;
Wherein, the mass ratio of the native graphite described in step (1) and potassium permanganate is 1:(0.05 ~ 0.2);
Oxidation processes described in step (1) comprises the following steps: oxidizing temperature is 800 DEG C ~ 1000 DEG C, and oxidization time is 10 ~ 40 seconds;
The mass ratio of the mixture A described in step (2) and ascorbic acid is 2:(0.5 ~ 1).
CN201310568784.3A 2013-11-15 2013-11-15 The preparation method of ascorbic acid modified graphite Expired - Fee Related CN103647081B (en)

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CN103647081B true CN103647081B (en) 2016-03-02

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Publication number Priority date Publication date Assignee Title
CN107275610A (en) * 2015-05-22 2017-10-20 许婷 A kind of preparation method of porous graphite doped graphite negative material
CN110098443B (en) * 2019-05-17 2021-08-27 浙江卡波恩新材料有限公司 Method for coating waste lithium battery negative electrode material with carbon

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101604750A (en) * 2009-07-09 2009-12-16 上海交通大学 A kind of preparation method of lithium ion battery negative material
CN103199254A (en) * 2013-04-03 2013-07-10 深圳市贝特瑞新能源材料股份有限公司 Graphite negative material of lithium-ion battery and preparation method of negative material

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI405802B (en) * 2010-06-24 2013-08-21 Nat Univ Tsing Hua Method for fabrication of functionalized graphene reinforced composite conducting plate

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101604750A (en) * 2009-07-09 2009-12-16 上海交通大学 A kind of preparation method of lithium ion battery negative material
CN103199254A (en) * 2013-04-03 2013-07-10 深圳市贝特瑞新能源材料股份有限公司 Graphite negative material of lithium-ion battery and preparation method of negative material

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