CN105633380A - Preparation method for starch-based porous hard carbon negative electrode material of lithium ion battery - Google Patents
Preparation method for starch-based porous hard carbon negative electrode material of lithium ion battery Download PDFInfo
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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
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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
- H01M4/58—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
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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- 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
Abstract
The invention relates to a preparation method for a starch-based porous hard carbon negative electrode material of a lithium ion battery. The method comprises the following steps of firstly, obtaining porous starch through enzymatic hydrolysis of composite bio-enzyme; secondly, reserving a hole morphology of the starch through a pre-carbonization process; and finally, obtaining a porous structured negative electrode material of the lithium ion battery through a carbonization process. The starch-based porous hard carbon for the negative electrode material of the lithium ion battery, obtained through the preparation method, has the characteristics of favorable electrochemical performance, high cycle stability and excellent consistency in batch products, the whole process is suitable for industrial production, and meanwhile, the morphology reservation of the porous starch is promoted. The method has the advantages of simplicity in operation, environmental friendliness in production and easiness in mass production, and the product quality is easy to control.
Description
Technical field
The invention belongs to a kind of field of lithium ion battery cathode material preparation.
Background technology
Lithium ion battery is that eighties of last century starts practical novel high-energy secondary cell the nineties, has operating voltage height, weight is light, specific energy is big, self-discharge is little, have extended cycle life, memory-less effect and the advantage such as environmental pollution is little. Lithium ion battery negative material, based on charcoal, mainly contains synthetic graphite, natural graphite and amorphous carbon. But there is following problem in current graphite cathode: 1, the current potential of current potential platform and metallic lithium is close, easily precipitates out dendrite Li and causes short circuit; 2, SEI film is unstable, and Li easily occurs+Jointly embed graphite linings with organic solvent, cause graphite to be peeled off and efflorescence; 3, graphite C interlamellar spacing (d002�� 0.34nm) < LixC6(��0.37nm), volume change 8%, easily causes graphite linings to be peeled off and efflorescence; 4, graphite and organic solvent generation thermopositive reaction, easily produce inflammable gas, battery easy firing; 5, Li+Spread coefficient is little, difficult rapid charge.
Amorphous carbon can be divided into hard charcoal and soft charcoal by the complexity of greying. With graphite Comparatively speaking, the hard charcoal in amorphous carbon have electrode expand little, there is not warpage in battery, the advantages such as high cycle life-span and good rate capability. Hard charcoal can be divided into biomass and fossil resource two class by source, has environmental protection and low cost and other advantages as hard carbon precursor with biomass starch. For amorphous carbon, micropore is the major cause that the reversible capacity of amorphous carbon exceedes graphite theoretical capacity. Therefore, from heat treatment process, it is possible to introduce micropore consciously, it is to increase the reversible capacity of the negative material of amorphous carbon.
Porous carbon material refers to the carbon materials with certain pore texture, comprises porous charcoal, carbon molecular sieve etc. At present, the technique preparing porous carbon material mainly contains chemical Vapor deposition process, template, hydrothermal synthesis method, catalysis method, emulsion process and arc discharge method etc. But, in these preparation researches existing, great majority have employed unfriendly, the non-renewable raw material of environment as charcoal source, or be the use of complicated experimental installation and condition and can not industrialization produce. Along with the energy-conserving and environment-protective consciousness being more and more taken seriously, adopt biomass material to prepare porous carbon material and have more researching value.
The present invention for lithium ion battery negative material, has simple to operate, production environmental protection, easily large-scale production and the quality product easily advantage such as control by porous hard charcoal that the biomass starch materials such as corn, rice, cassava, potato carry out processing preparation.
Summary of the invention
It is an object of the invention to, a kind of environmental friendliness is provided, easy industrialization, for the preparation method of lithium ion battery starch base porous hard carbon cathode material, the method is to the modification of biomass material shape looks preparation technology and maintenance, by compound biological enzyme enzyme starch, enzymolysis goes out hole, then by pre-carbonization process, the hole type looks of starch are retained, the lithium ion battery negative material with vesicular structure is obtained again by carbonization process, obtained the starch base porous hard charcoal that is used for lithium ion battery negative material to have chemical property good by the method for the invention, good cycling stability and the outstanding feature of batch products consistence, preparation manipulation is simple simultaneously, production environmental protection, easy large-scale production and quality product easily control.
The preparation method of a kind of lithium ion battery starch base porous hard carbon cathode material of the present invention, follows these steps to carry out:
The damping fluid of starch to be W-Gum, Starch rice, tapioca (flour) or yam starch with pH value be 4-7 is that Sodium phosphate dibasic-citric acid, potassium primary phosphate-sodium hydroxide, vulkacit H-hydrochloric acid or acetic acid-ammonium acetate mix by a, in mass ratio 2:3, stir 10 minutes after mixture is added to temperature 55 DEG C, the prozyme adding relative starch mass fraction 1-3% is that ��-amylase and saccharifying enzyme stir 20h, obtains mixture;
B, by the mixture in step a, dry after carrying out taking out for 3 times filter and washing, obtain solids;
C, the solids obtained by step b by mass fraction 5%-10% and dehydration catalyst are one or both Homogeneous phase mixing in ammonium chloride, ammonium sulfate, obtain solid-phase mixture;
D, the solid-phase mixture obtained by step c be pre-carbonization 12h in temperature 170-250 DEG C of vacuum drying oven, obtains the pre-carbonized product of black;
E, the pre-carbonized product that steps d is obtained, carry out taking out filter and the rear drying of washing for 3 times, put into process furnace again, at inert atmosphere nitrogen, argon gas, helium, one or both rise to 900-1100 DEG C with temperature 1-10 DEG C/min, lower the temperature with stove after keeping 1-4h, obtain lithium ion battery starch base porous hard carbon cathode material.
In step a, pH damping fluid is acetic acid-ammonium acetate.
PH of buffer described in step a is 6
Prozyme ��-amylase described in step a and saccharifying enzyme be 5-10:1 mixing in mass ratio.
The preparation method of a kind of lithium ion battery starch base porous hard carbon cathode material of the present invention, the method is by compound biological enzyme enzyme starch, enzymolysis goes out hole, then by pre-carbonization process, the hole type looks of starch are retained, then by carbonization process acquisition, there is porous hard carbon material, duct can store a large amount of electrolytic solution, forming ion buffer pool, pore structure can shorten the distance of lithium ion diffusion and electronic conduction, thus improve velocity of diffusion and improve performance of lithium ion battery. Starch is easily molten in heat-processed to be melted, reunite, expand, therefore the preparation technology of report is only suitable for laboratory preparation starch base hard carbon material on a small scale substantially at present, the present invention is by using for reference viscose based carbon fiber and the ultracapacitor preparation technology of biomass active charcoal, the preparation of the above sample of feather weight can be effectively completed by adding dehydration catalyst, it is applicable to industrialization expanding production, there is very strong commercialization and be worth.
Accompanying drawing illustrates:
Fig. 1 is the SEM figure of lithium ion battery negative material starch base porous hard charcoal of the present invention;
Fig. 2 is the first Zhou Xunhuan discharge curve comparison diagram of 0.1C of lithium ion battery negative material starch base porous hard charcoal of the present invention and the hard carbon of common starch.
Embodiment
Embodiment 1
The damping fluid that W-Gum and pH value are 4 is that potassium primary phosphate-sodium hydroxide mixes by a, in mass ratio 2:3, stir 10 minutes after mixture is added to temperature 55 DEG C, add prozyme ��-amylase and the saccharifying enzyme 5:1 mixing in mass ratio of relative W-Gum mass fraction 1%, stir 20h, obtain mixture;
B, by the mixture in step a, dry after carrying out taking out for 3 times filter and washing, obtain solids;
C, the solids obtained by step b by mass fraction 5% are that ammonium chloride mixes with dehydration catalyst, obtain solid-phase mixture;
D, the solid-phase mixture obtained by step c be pre-carbonization 12h in temperature 170 DEG C of vacuum drying ovens, obtains the pre-carbonized product of black;
E, the pre-carbonized product that steps d is obtained, carry out taking out filter and the rear drying of washing for 3 times, then put into process furnace, in nitrogen inert atmosphere, rise to 900 DEG C with temperature 1 DEG C/min, lower the temperature with stove after keeping 1h, obtain lithium ion battery starch base porous hard carbon cathode material.
Embodiment 2
The damping fluid that Starch rice and pH value are 6 is that acetic acid-ammonium acetate mixes by a, in mass ratio 2:3, stir 10 minutes after mixture is added to temperature 55 DEG C, add prozyme ��-amylase and the saccharifying enzyme 10:1 mixing in mass ratio of relative Starch rice mass fraction 3%, stir 20h, obtain mixture;
B, by the mixture in step a, dry after carrying out taking out for 3 times filter and washing, obtain solids;
C, the solids obtained by step b by mass fraction 5% and dehydration catalyst are ammonium chloride Homogeneous phase mixing, obtain solid-phase mixture;
D, the solid-phase mixture obtained by step c be pre-carbonization 12h in temperature 250 DEG C of vacuum drying ovens, obtains the pre-carbonized product of black;
E, the pre-carbonized product that steps d is obtained, carry out taking out filter and the rear drying of washing for 3 times, then put into process furnace, in nitrogen inert atmosphere, rise to 900 DEG C with temperature 10 DEG C/min, lower the temperature with stove after keeping 4h, obtain lithium ion battery starch base porous hard carbon cathode material.
Embodiment 3
The damping fluid that Starch rice and pH value are 7 is that Sodium phosphate dibasic-citric acid mixes by a, in mass ratio 2:3, stir 10 minutes after mixture is added to temperature 55 DEG C, the prozyme adding relative starch mass fraction 2% is ��-amylase and saccharifying enzyme 8:1 mixing in mass ratio, stir 20h, obtain mixture;
B, by the mixture in step a, dry after carrying out taking out for 3 times filter and washing, obtain solids;
C, the solids obtained by step b by mass fraction 8% and dehydration catalyst are ammonium sulfate Homogeneous phase mixing, obtain solid-phase mixture;
D, the solid-phase mixture obtained by step c be pre-carbonization 12h in temperature 200 DEG C of vacuum drying ovens, obtains the pre-carbonized product of black;
E, the pre-carbonized product that steps d is obtained, carry out taking out filter and the rear drying of washing for 3 times, then put into process furnace, in argon inert atmosphere, rise to 1100 DEG C with temperature 5 DEG C/min, lower the temperature with stove after keeping 2h, obtain lithium ion battery starch base porous hard carbon cathode material.
Embodiment 4
The damping fluid that tapioca (flour) and pH value are 6 is that vulkacit H-hydrochloric acid mixes by a, in mass ratio 2:3, stir 10 minutes after mixture is added to temperature 55 DEG C, the prozyme adding relative starch mass fraction 2% is mass ratio 6:1 ��-amylase: saccharifying enzyme mixes, stir 20h, obtain mixture;
B, by the mixture in step a, dry after carrying out taking out for 3 times filter and washing, obtain solids;
C, solids step b obtained by mass fraction 10% with dehydration catalyst quality than ammonium chloride: ammonium sulfate=1:1 Homogeneous phase mixing, obtains solid-phase mixture;
D, the solid-phase mixture obtained by step c be pre-carbonization 12h in temperature 200 DEG C of vacuum drying ovens, obtains the pre-carbonized product of black;
E, the pre-carbonized product that steps d is obtained, carry out taking out filter and the rear drying of washing for 3 times, then put into process furnace, in helium inert atmosphere, rise to 1100 DEG C with temperature 5 DEG C/min, lower the temperature with stove after keeping 2h, obtain lithium ion battery starch base porous hard carbon cathode material.
Embodiment 5
The damping fluid that yam starch and pH value are 5.5 is that acetic acid-ammonium acetate mixes by a, in mass ratio 2:3, stir 10 minutes after mixture is added to temperature 55 DEG C, the prozyme adding relative starch mass fraction 2.5% is ��-amylase and saccharifying enzyme 5:1 mixing in mass ratio, stir 20h, obtain mixture;
B, by the mixture in step a, dry after carrying out taking out for 3 times filter and washing, obtain solids;
C, solids and dehydration catalyst step b obtained by mass fraction 6% be quality than ammonium chloride: ammonium sulfate=2:1 Homogeneous phase mixing, obtains solid-phase mixture;
D, the solid-phase mixture obtained by step c be pre-carbonization 12h in temperature 250 DEG C of vacuum drying ovens, obtains the pre-carbonized product of black;
E, the pre-carbonized product that steps d is obtained, carry out taking out filter and the rear drying of washing for 3 times, put into process furnace again, 1000 DEG C are risen to temperature 8 DEG C/min in inert atmosphere nitrogen mixes with helium volume ratio 1:1, lower the temperature with stove after keeping 3h, obtain lithium ion battery starch base porous hard carbon cathode material.
Embodiment 6 (testing the chemical property of lithium ion battery negative material starch base porous hard charcoal for example 2)
It is the hard carbon of starch that the identical preparation condition of raw material obtains by the lithium ion battery starch base porous hard carbon cathode material prepared by embodiment 2 and non-enzyme starch, respectively with conductive agent acetylene black, polyfluortetraethylene of binding element emulsion in mass ratio 80:15:5 mix in aqueous, then compressing tablet is on Copper Foil, obtained negative plate, take metal lithium sheet as negative pole, the NSC 11801 of 1mol/L lithium hexafluoro phosphate and the solution of methylcarbonate are as electrolytic solution, Celgard2400 microporous polypropylene membrane is barrier film, it is assembled into CR2025 type button lithium ion battery and carries out discharge and recharge, system is that constant current 0.1C is discharged to 2mV, it is discharged to 1mV with 0.01C again after shelving 10 minutes, finally charge to 2V with 0.1C, obtain shown in its test curve (Fig. 2), non-enzyme starch hard carbon 0.1C first reversible loading capacity be 305mAh/g, coulomb efficiency is 42.8% first, through the porous enzymeization porous-starch hard carbon 0.1C that obtains of process first reversible loading capacity reach 454mAh/g, coulomb efficiency is 66.6% first. effective raising is obtained by the chemical property of starch base porous hard carbon cathode material assembled battery.
Claims (4)
1. the preparation method of a lithium ion battery starch base porous hard carbon cathode material, it is characterised in that follow these steps to carry out:
The damping fluid of starch to be W-Gum, Starch rice, tapioca (flour) or yam starch with pH value be 4-7 is that Sodium phosphate dibasic-citric acid, potassium primary phosphate-sodium hydroxide, vulkacit H-hydrochloric acid or acetic acid-ammonium acetate mix by a, in mass ratio 2:3, stir 10 minutes after mixture is added to temperature 55 DEG C, the prozyme adding relative starch mass fraction 1-3% is that ��-amylase and saccharifying enzyme stir 20h, obtains mixture;
B, by the mixture in step a, dry after carrying out taking out for 3 times filter and washing, obtain solids;
C, the solids obtained by step b by mass fraction 5%-10% and dehydration catalyst are one or both Homogeneous phase mixing in ammonium chloride, ammonium sulfate, obtain solid-phase mixture;
D, the solid-phase mixture obtained by step c be pre-carbonization 12h in temperature 170-250 DEG C of vacuum drying oven, obtains the pre-carbonized product of black;
E, the pre-carbonized product that steps d is obtained, carry out taking out filter and the rear drying of washing for 3 times, put into process furnace again, it is that nitrogen, argon gas, helium rise to 900-1100 DEG C with temperature 1-10 DEG C/min in one or both at inert atmosphere, lower the temperature with stove after keeping 1-4h, obtain lithium ion battery starch base porous hard carbon cathode material.
2. the preparation method of lithium ion battery starch base porous hard carbon cathode material according to claim 1, it is characterised in that in step a, pH damping fluid is acetic acid-ammonium acetate.
3. the preparation method of lithium ion battery starch base porous hard carbon cathode material according to claim 2, it is characterised in that the pH of buffer described in step a is 6.
4. the preparation method of lithium ion battery starch base porous hard carbon cathode material according to claim 1, it is characterised in that the prozyme ��-amylase described in step a and saccharifying enzyme be 5-10:1 mixing in mass ratio.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107359345A (en) * | 2017-08-01 | 2017-11-17 | 河南新太行电源股份有限公司 | A kind of preparation method and applications of cornstarch porous carbon@graphite |
| CN107528063A (en) * | 2017-08-01 | 2017-12-29 | 河南新太行电源股份有限公司 | A kind of preparation method and applications of core shell structure silicon/carbon material of cornstarch porous carbon encapsulation |
| CN107879323A (en) * | 2017-11-15 | 2018-04-06 | 上海空间电源研究所 | A kind of hard carbon material and its preparation method and application |
| CN109921018A (en) * | 2017-12-13 | 2019-06-21 | 宁波杉杉新材料科技有限公司 | The preparation method of sodium-ion battery high capacity biomass hard charcoal negative electrode material |
| CN110877908A (en) * | 2018-09-06 | 2020-03-13 | 天津大学 | Preparation method of corn starch pyrolysis hard carbon electrode material |
| CN114702022A (en) * | 2022-03-15 | 2022-07-05 | 广东邦普循环科技有限公司 | Preparation method and application of hard carbon negative electrode material |
| CN114804064A (en) * | 2022-04-14 | 2022-07-29 | 福建师范大学 | Method for preparing starch-based biomass hard carbon by yeast fermentation and application thereof |
| CN115321517A (en) * | 2022-10-12 | 2022-11-11 | 宁德新能源科技有限公司 | Negative electrode active material, negative electrode plate comprising same, electrochemical device and electricity utilization device |
| CN115445588A (en) * | 2022-08-15 | 2022-12-09 | 东南大学 | Biomass-based porous carbon composite material, preparation method thereof and application thereof in CO 2 Application in adsorption |
| CN115536002A (en) * | 2022-11-02 | 2022-12-30 | 多氟多新能源科技有限公司 | Preparation method of starch-based hard carbon negative electrode material, negative electrode material and sodium ion battery |
| CN116692832A (en) * | 2023-08-09 | 2023-09-05 | 江苏正力新能电池技术有限公司 | Hard carbon anode material and preparation method and application thereof |
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| CN107359345A (en) * | 2017-08-01 | 2017-11-17 | 河南新太行电源股份有限公司 | A kind of preparation method and applications of cornstarch porous carbon@graphite |
| CN107879323A (en) * | 2017-11-15 | 2018-04-06 | 上海空间电源研究所 | A kind of hard carbon material and its preparation method and application |
| CN109921018A (en) * | 2017-12-13 | 2019-06-21 | 宁波杉杉新材料科技有限公司 | The preparation method of sodium-ion battery high capacity biomass hard charcoal negative electrode material |
| CN110877908A (en) * | 2018-09-06 | 2020-03-13 | 天津大学 | Preparation method of corn starch pyrolysis hard carbon electrode material |
| CN114702022B (en) * | 2022-03-15 | 2023-09-12 | 广东邦普循环科技有限公司 | Preparation method and application of hard carbon anode material |
| CN114702022A (en) * | 2022-03-15 | 2022-07-05 | 广东邦普循环科技有限公司 | Preparation method and application of hard carbon negative electrode material |
| CN114804064A (en) * | 2022-04-14 | 2022-07-29 | 福建师范大学 | Method for preparing starch-based biomass hard carbon by yeast fermentation and application thereof |
| CN114804064B (en) * | 2022-04-14 | 2023-09-01 | 福建师范大学 | Method for preparing starch-based biomass hard carbon by utilizing yeast fermentation and application of method |
| CN115445588A (en) * | 2022-08-15 | 2022-12-09 | 东南大学 | Biomass-based porous carbon composite material, preparation method thereof and application thereof in CO 2 Application in adsorption |
| CN115445588B (en) * | 2022-08-15 | 2023-10-17 | 东南大学 | Biomass-based porous carbon composite material, preparation and CO production 2 Application in adsorption |
| CN115321517A (en) * | 2022-10-12 | 2022-11-11 | 宁德新能源科技有限公司 | Negative electrode active material, negative electrode plate comprising same, electrochemical device and electricity utilization device |
| CN115536002A (en) * | 2022-11-02 | 2022-12-30 | 多氟多新能源科技有限公司 | Preparation method of starch-based hard carbon negative electrode material, negative electrode material and sodium ion battery |
| CN116692832A (en) * | 2023-08-09 | 2023-09-05 | 江苏正力新能电池技术有限公司 | Hard carbon anode material and preparation method and application thereof |
| CN116692832B (en) * | 2023-08-09 | 2023-10-10 | 江苏正力新能电池技术有限公司 | Hard carbon anode material and preparation method and application thereof |
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Application publication date: 20160601 |