CN108807942A - A method of preparing ion cathode material lithium using graphene oxide - Google Patents

A method of preparing ion cathode material lithium using graphene oxide Download PDF

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Publication number
CN108807942A
CN108807942A CN201810795289.9A CN201810795289A CN108807942A CN 108807942 A CN108807942 A CN 108807942A CN 201810795289 A CN201810795289 A CN 201810795289A CN 108807942 A CN108807942 A CN 108807942A
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graphene oxide
raw material
purification
lithium
graphene
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闵洁
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Datong Xincheng New Material Co Ltd
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Datong Xincheng New Material Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection 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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Composite Materials (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a kind of methods preparing ion cathode material lithium using graphene oxide, include the following steps：S1：Material prepares：Prepare graphene oxide raw material and cladding is expected, and the weight ratio of graphene oxide raw material and cladding material is 75:25-80:20, it is spare；S2：It mills：Graphene oxide raw material described in S1 is launched and carries out processing of milling into grinding equipment, obtains preliminary working graphene oxide raw material, it is spare；S3：Purification：Preliminary working graphene oxide raw material described in S2 is launched and carries out primary graphitizing purification processes into equipment for purifying, obtains purification graphene raw material, it is spare.The preparation method for the ion cathode material lithium that the present invention uses improves graphitization process technique, can carry out extensive graphitization purification, is different from simple surface catalysis and is graphitized, the battery comprehensive performance made of this material is high.

Description

A method of preparing ion cathode material lithium using graphene oxide
Technical field
The present invention relates to energy storage material preparing technical fields more particularly to a kind of utilization graphene oxide to prepare lithium ion and bear The method of pole material.
Background technology
Graphene is referred to as " dark fund ", is " king of new material ".As carbon material application field is constantly widened, charcoal element row Industry welcomes comprehensively quickly development.It, which is used as, has the spies such as tension, compressive property are strong, good in thermal shock, ablation resistance are strong The carbon material of property, is applied to lithium ion battery negative material, semiconductor, photovoltaic solar, solar energy thermal-power-generating, electrical fire The various fields such as flower and mold processing, nuclear energy, metallurgy, space flight.
Through retrieval, application No. is the patent documents of 201810020684.X to disclose a kind of stone of surface multi-layer graphite alkylene Black lithium ion battery negative material and preparation method belong to energy storage material preparation field.Conventional graphite oxidation is all in aqueous solvent Middle progress needs a large amount of caustic acid and strong oxidizer, and there are security risks for batch production.And when using fused salt as solvent Reaction temperature can be promoted, reduce oxidizer, while fused salt can be with recycling.The present invention is melted with safe, green Salt method carries out high temperature surface oxidation corrosion to crystalline flake graphite, obtains the graphite cathode material for the surface graphite alkylene for being not easy to reunite, So that material has multiple stratification in situ, the enhancing of conductance isotropism improves material electronics electrical conductivity and embedding lithium ability, prepares Material has better cycle performance.
For a long time, many materials are studied and has been explored both at home and abroad, lithium ion battery negative material is with Carbon Materials Based on, mainly there are two kinds of artificial graphite and natural graphite.General preparation method both is to carry out collocation to be used in mixed way, they are common The solution that disadvantage has been unable to get leads to material poor processability.
Natural graphite equally exists that tap density is low, the high feature of specific surface area, as preparing the raw material of negative material also It is not satisfactory.The disadvantages such as that there are specific surface areas is high for common artificial graphite, tap density is low, particle shape is poor, discharge capacity is low Be not suitable for, directly as the condition for preparing negative material, must just being restructured again using such artificial graphite if desired, stone The raising of ink structure stability cannot be guaranteed, and also increase production cost, therefore utilizing oxidation stone we have proposed a kind of Black alkene prepares the method for ion cathode material lithium for solving the above problems.
Invention content
Technical problems based on background technology, the present invention propose that a kind of using graphene oxide to prepare lithium ion negative The method of pole material.
A kind of method preparing ion cathode material lithium using graphene oxide proposed by the present invention, includes the following steps：
S1：Material prepares：Prepare graphene oxide raw material and cladding is expected, and the weight ratio of graphene oxide raw material and cladding material is 75:25-80:20, it is spare；
S2：It mills：Graphene oxide raw material described in S1 is launched and carries out processing of milling into grinding equipment, obtains preliminary working Graphene oxide raw material, it is spare；
S3：Purification：Preliminary working graphene oxide raw material described in S2 is launched into equipment for purifying progress primary graphitizing to carry Pure processing obtains purification graphene raw material, spare；
S4：Classification：Sizing screening is carried out to the purification graphene raw material described in S3, obtains particle diameter graphene raw material, it is spare；
S5：Cladding：By described in S4 particle diameter graphene raw material and S1 described in be cladding material launch in impregnating equipment into Row impregnation obtains mixing material, spare；
S6：Roasting：Mixing material described in S5 is launched into roasting apparatus and is carried out after roasting charing process roasted Mixing material；
S7：It is cooling：Mixing material after roasting described in S6 is cooled to room temperature, charing mixing material is obtained；
S8：Graphitization：Charing mixing material described in S7 is launched and carries out graphitization purification into graphitizing furnace, is aoxidized Graphene negative material；
S9：Mechanical processing：Modification is processed to the graphene oxide negative material described in S8, obtains oval cathode material Material.
Preferably, in the S1, the granularity D of graphene oxide raw material50It is for 1-20 μm, purity 99.0wt%, single layer rate 99.0%。
Preferably, in the S1, the softening point of cladding material medium temperature coal pitch is 83-90 DEG C, coking value is >=48%, ash content ≤ 0.20%, toluene insolubles≤3%, quinoline insolubles≤0.20%, fugitive constituent 60-70%.
Preferably, in the S2, grinding equipment is grinder, milling time 3h.
Preferably, in the S3, equipment for purifying is acheson furnace, purification temperature be 2500~2800 DEG C, purification the time be 192-240h。
Preferably, in the S5, impregnating equipment is impregnating autoclave, and dipping temperature is 250-650 DEG C, impregnation pressure 7-12KPa, Dip time is 8-15h.
Preferably, in the S6, roasting apparatus is roaster, roaster at 120-370 DEG C, heating rate is 2.5 DEG C/ H, 100h, at 370-570 DEG C, heating rate be 3.5 DEG C/h, 57h, at 570-870 DEG C, heating rate be 4 DEG C/h, 75h, At 870-1200 DEG C, heating rate be 3 DEG C/h, 110h.
Preferably, in the S7, when being cooled down to the mixing material after roasting, cooling time is for 24 hours.
Preferably, in the S8, the graphitization purification time is 450-500h, and graphited maximum temperature is 2800-3200 ℃。
Preferably, in the S9, when being processed modification to graphene oxide negative material, rotating speed 700r/min, Modification time is 3-5min.
Compared with prior art, the beneficial effects of the invention are as follows：
By the way that broken, classification and preparation process are studied in detail, the lithium ion prepared using graphene oxide is proposed Cell negative electrode material, with granularity D50For 1-20 μm, purity：99.0wt%, the graphene oxide that single layer rate is up to 99.0% are former material The softening point of material, cladding material medium temperature coal pitch is 83-90 DEG C, and coking value is >=48%, ash content≤0.20%, toluene insolubles≤ 3%, quinoline insolubles≤0.20%, fugitive constituent 60-70% is conducive to improve product qualification rate, and medium temperature coal pitch is in graphite chemical industry Sequence is easy graphitization；
The effect of primary graphitizing purification is to make raw material graphene oxide in mechanical strength, thermal shock resistance, heat-resisting quantity, antioxygen The property changed, corrosion resistance etc. further increase；The characteristic of cladding pitch has covered effect in important influence, main table Present asphalt viscosity, toluene insolubles, quinoline insolubles content, on coking value, coking value is higher, and the volume of product is close after roasting Degree and mechanical strength are bigger, and coking value rises with softening point and increased, therefore using the higher coal tar pitch of softening point as packet Agent is covered, is conducive to the bulk density and mechanical strength that improve product material, but impregnating pitch softening point is higher, and and heating temperature Height is inversely proportional, and the purpose of roasting is will coat material pitch to carbonize, the present invention by heating curve when optimizing and improve roasting, The factors such as the duration of heat improve the coking rate of binder, to ensure that the yield rate of product overall target, graphitization are again The process re-sintered is carbonized, purpose is then to play the role of purification and effect；
The method that the present invention prepares ion cathode material lithium using graphene oxide, prepared material stiffness weaken, and compacting is close Degree is higher, and structure is that single graphene oxide different-grain diameter mixes, this structural material is conducive to the insertion of lithium ion and takes off Go out, further improve the gram volume of negative material, the charge/discharge capacity of battery is made to increase；
The preparation method for the ion cathode material lithium that the present invention uses improves graphitization process technique, can carry out depth graphite Change purification, is different from simple surface catalysis and is graphitized, the battery comprehensive performance made of this material is high.
Specific implementation mode
The present invention is made further to explain with reference to specific embodiment.
Embodiment
A kind of method preparing ion cathode material lithium using graphene oxide, including following step are proposed in the present embodiment Suddenly：
S1：Material prepares：Prepare graphene oxide raw material and cladding is expected, and the weight ratio of graphene oxide raw material and cladding material is 75:25-80:20, it is spare；
S2：It mills：Graphene oxide raw material described in S1 is launched and carries out processing of milling into grinding equipment, obtains preliminary working Graphene oxide raw material, it is spare；
S3：Purification：Preliminary working graphene oxide raw material described in S2 is launched into equipment for purifying progress primary graphitizing to carry Pure processing obtains purification graphene raw material, spare；
S4：Classification：Sizing screening is carried out to the purification graphene raw material described in S3, obtains particle diameter graphene raw material, it is spare；
S5：Cladding：By described in S4 particle diameter graphene raw material and S1 described in be cladding material launch in impregnating equipment into Row impregnation obtains mixing material, spare；
S6：Roasting：Mixing material described in S5 is launched into roasting apparatus and is carried out after roasting charing process roasted Mixing material；
S7：It is cooling：Mixing material after roasting described in S6 is cooled to room temperature, charing mixing material is obtained；
S8：Graphitization：Charing mixing material described in S7 is launched and carries out graphitization purification into graphitizing furnace, is aoxidized Graphene negative material；
S9：Mechanical processing：Modification is processed to the graphene oxide negative material described in S8, obtains oval cathode material Material.
In the present embodiment, in S1, the granularity D of graphene oxide raw material50It is for 1-20 μm, purity 99.0wt%, single layer rate In 99.0%, S1, cladding material medium temperature coal pitch softening point be 83-90 DEG C, coking value be >=48%, ash content≤0.20%, toluene not In molten object≤3%, quinoline insolubles≤0.20%, fugitive constituent 60-70%, S2, grinding equipment is grinder, milling time 3h, S3 In, equipment for purifying is acheson furnace, and purification temperature is 2500~2800 DEG C, and the purification time is 192-240h, in S5, impregnating equipment For impregnating autoclave, dipping temperature is 250-650 DEG C, impregnation pressure 7-12KPa, and in dip time 8-15h, S6, roasting apparatus is Roaster, roaster at 120-370 DEG C, heating rate be 2.5 DEG C/h, 100h, at 370-570 DEG C, heating rate 3.5 DEG C/h, 57h, at 570-870 DEG C, heating rate be 4 DEG C/h, 75h, at 870-1200 DEG C, heating rate be 3 DEG C/h, In 110h, S7, when being cooled down to the mixing material after roasting, cooling time is that for 24 hours, in S8, the graphitization purification time is 450-500h, graphited maximum temperature are 2800-3200 DEG C, in S9, are repaiied being processed to graphene oxide negative material When decorations, rotating speed 700r/min, modification time 3-5min, by broken, classification and preparation process grind in detail Study carefully, the lithium ion battery negative material prepared using graphene oxide is proposed, with granularity D50For 1-20 μm, purity：99.0wt%, The graphene oxide that single layer rate is up to 99.0% is raw material, and the softening point of cladding material medium temperature coal pitch is 83-90 DEG C, coking value It is >=48%, ash content≤0.20%, toluene insolubles≤3%, quinoline insolubles≤0.20%, fugitive constituent 60-70% is conducive to improve Product qualification rate, and medium temperature coal pitch is easy graphitization in graphitization process；The effect of primary graphitizing purification is to make raw material Graphene oxide further increases in mechanical strength, thermal shock resistance, heat-resisting quantity, inoxidizability, corrosion resistance etc.； The characteristic of cladding pitch has covered effect important influence, is mainly manifested in asphalt viscosity, toluene insolubles, quinoline insolubles In content, coking value, coking value is higher, and the bulk density and mechanical strength of product are bigger after roasting, and coking value is with softening point Rise and increase, therefore using the higher coal tar pitch of softening point as covering, is conducive to the bulk density for improving product material And mechanical strength, but impregnating pitch softening point is higher, and be inversely proportional with heating temperature height, the purpose of roasting is will to coat material drip Blueness charing, the present invention improve binder by factors such as heating curve, the durations of heat when optimizing and improve roasting Coking rate, to ensure that the yield rate of product overall target, graphitization are to carbonize the process re-sintered again, purpose is then to play to carry Pure effect and effect；The method that the present invention prepares ion cathode material lithium using graphene oxide, prepared material stiffness subtract Weak, compacted density is higher, and structure is that single graphene oxide different-grain diameter mixes, this structural material is conducive to lithium ion Embedded and abjection, further improves the gram volume of negative material, the charge/discharge capacity of battery is made to increase；The lithium that the present invention uses The preparation method of ion negative material improves graphitization process technique, can carry out extensive graphitization purification, is different from simple Surface catalysis graphitization, the battery comprehensive performance made of this material is high.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (10)

1. a kind of method preparing ion cathode material lithium using graphene oxide, which is characterized in that include the following steps：
S1：Material prepares：Prepare graphene oxide raw material and cladding is expected, and the weight ratio of graphene oxide raw material and cladding material is 75:25-80:20, it is spare；
S2：It mills：Graphene oxide raw material described in S1 is launched and carries out processing of milling into grinding equipment, obtains preliminary working Graphene oxide raw material, it is spare；
S3：Purification：Preliminary working graphene oxide raw material described in S2 is launched into equipment for purifying progress primary graphitizing to carry Pure processing obtains purification graphene raw material, spare；
S4：Classification：Sizing screening is carried out to the purification graphene raw material described in S3, obtains particle diameter graphene raw material, it is spare；
S5：Cladding：By described in S4 particle diameter graphene raw material and S1 described in be cladding material launch in impregnating equipment into Row impregnation obtains mixing material, spare；
S6：Roasting：Mixing material described in S5 is launched into roasting apparatus and is carried out after roasting charing process roasted Mixing material；
S7：It is cooling：Mixing material after roasting described in S6 is cooled to room temperature, charing mixing material is obtained；
S8：Graphitization：Charing mixing material described in S7 is launched and carries out graphitization purification into graphitizing furnace, is aoxidized Graphene negative material；
S9：Mechanical processing：Modification is processed to the graphene oxide negative material described in S8, obtains oval cathode material Material.
2. a kind of method preparing ion cathode material lithium using graphene oxide according to claim 1, feature exist In, in the S1, the granularity D of graphene oxide raw material50For 1-20 μm, purity 99.0wt%, single layer rate be 99.0%.
3. a kind of method preparing ion cathode material lithium using graphene oxide according to claim 1, feature exist In in the S1, the softening point of cladding material medium temperature coal pitch is 83-90 DEG C, coking value is >=48%, ash content≤0.20%, toluene Insoluble matter≤3%, quinoline insolubles≤0.20%, fugitive constituent 60-70%.
4. a kind of method preparing ion cathode material lithium using graphene oxide according to claim 1, feature exist In in the S2, grinding equipment is grinder, milling time 3h.
5. a kind of method preparing ion cathode material lithium using graphene oxide according to claim 1, feature exist In in the S3, equipment for purifying is acheson furnace, and purification temperature is 2500~2800 DEG C, and the purification time is 192-240h.
6. a kind of method preparing ion cathode material lithium using graphene oxide according to claim 1, feature exist In in the S5, impregnating equipment is impregnating autoclave, and dipping temperature is 250-650 DEG C, impregnation pressure 7-12KPa, dip time 8- 15h。
7. a kind of method preparing ion cathode material lithium using graphene oxide according to claim 1, feature exist In, in the S6, roasting apparatus is roaster, and for roaster at 120-370 DEG C, heating rate is 2.5 DEG C/h, 100h, At 370-570 DEG C, heating rate be 3.5 DEG C/h, 57h, at 570-870 DEG C, heating rate be 4 DEG C/h, 75h, in 870- At 1200 DEG C, heating rate be 3 DEG C/h, 110h.
8. a kind of method preparing ion cathode material lithium using graphene oxide according to claim 1, feature exist In in the S7, when being cooled down to the mixing material after roasting, cooling time is for 24 hours.
9. a kind of method preparing ion cathode material lithium using graphene oxide according to claim 1, feature exist In in the S8, the graphitization purification time is 450-500h, and graphited maximum temperature is 2800-3200 DEG C.
10. a kind of method preparing ion cathode material lithium using graphene oxide according to claim 1, feature exist In, in the S9, when being processed modification to graphene oxide negative material, rotating speed 700r/min, modification time 3- 5min。
CN201810795289.9A 2018-07-19 2018-07-19 A method of preparing ion cathode material lithium using graphene oxide Pending CN108807942A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111204754A (en) * 2020-01-14 2020-05-29 大同新成新材料股份有限公司 Preparation method of graphene oxide silicon-carbon composite negative electrode material
CN112430095A (en) * 2020-12-03 2021-03-02 中国科学院山西煤炭化学研究所 Method for preparing high-performance graphite from graphene oxide modified coal pitch
CN113644242A (en) * 2021-07-27 2021-11-12 黑龙江省宝泉岭农垦溢祥石墨有限公司 High-temperature purified graphite carbene lithium ion battery cathode material and preparation method thereof

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CN105977490A (en) * 2016-05-18 2016-09-28 河南田园新能源科技有限公司 Method for preparing graphene composite negative electrode material from modified graphene oxide
CN107732216A (en) * 2017-11-07 2018-02-23 大同新成新材料股份有限公司 A kind of method that ion cathode material lithium is prepared using C/C composite material granulars
CN107851798A (en) * 2016-05-19 2018-03-27 株式会社Lg化学 Composite negative pole material for secondary cell, negative pole and lithium secondary battery comprising the material
CN108281655A (en) * 2018-01-30 2018-07-13 南京红太阳新能源有限公司 The preparation method of silicon/carbon/graphite in lithium ion batteries alkene negative material

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105977490A (en) * 2016-05-18 2016-09-28 河南田园新能源科技有限公司 Method for preparing graphene composite negative electrode material from modified graphene oxide
CN107851798A (en) * 2016-05-19 2018-03-27 株式会社Lg化学 Composite negative pole material for secondary cell, negative pole and lithium secondary battery comprising the material
CN107732216A (en) * 2017-11-07 2018-02-23 大同新成新材料股份有限公司 A kind of method that ion cathode material lithium is prepared using C/C composite material granulars
CN108281655A (en) * 2018-01-30 2018-07-13 南京红太阳新能源有限公司 The preparation method of silicon/carbon/graphite in lithium ion batteries alkene negative material

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111204754A (en) * 2020-01-14 2020-05-29 大同新成新材料股份有限公司 Preparation method of graphene oxide silicon-carbon composite negative electrode material
CN112430095A (en) * 2020-12-03 2021-03-02 中国科学院山西煤炭化学研究所 Method for preparing high-performance graphite from graphene oxide modified coal pitch
CN113644242A (en) * 2021-07-27 2021-11-12 黑龙江省宝泉岭农垦溢祥石墨有限公司 High-temperature purified graphite carbene lithium ion battery cathode material and preparation method thereof

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