CN105845914A - Method for preparing lithium ion battery negative electrode composite material - Google Patents
Method for preparing lithium ion battery negative electrode composite material Download PDFInfo
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- CN105845914A CN105845914A CN201610362151.0A CN201610362151A CN105845914A CN 105845914 A CN105845914 A CN 105845914A CN 201610362151 A CN201610362151 A CN 201610362151A CN 105845914 A CN105845914 A CN 105845914A
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- lithium ion
- ion battery
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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
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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
- 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
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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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- 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 discloses a method for preparing a lithium ion battery negative electrode composite material. The method comprises the following steps: uniformly mixing epoxy resin, polycarbonate, butylene succinate, isocyanate and ethyl acetate by stirring, and feeding the mixture into a carbonization furnace for carbonization to obtain a carbonized material I; soaking the carbonized material I with a 1 percent hydrochloric acid solution, filtering the soaked carbonized material I to obtain a solid mixture, flushing the solid mixture with deionized water to neutral, and performing filtering, drying and grinding on the flushed solid mixture to obtain a carbonized material II; adding the carbonized material II, graphene, methylphenyldiaryl silane and dioctyl phthalate into a reaction kettle, heating the materials in the reaction kettle to perform a reaction, and adding ammonium persulfate to obtain an intermediate material; and drying the intermediate material, and grinding the dried intermediate material to obtain the lithium ion battery negative electrode composite material. The lithium ion battery negative electrode composite material prepared by the method has high discharging capacity and high discharging efficiency.
Description
Technical field
The invention belongs to lithium ion battery electrode material preparing technical field, be specifically related to the preparation method of a kind of composite cathode material of lithium ion battery.
Background technology
Lithium ion battery is a kind of secondary cell (rechargeable battery), and it relies primarily on lithium ion and moves work between a positive electrode and a negative electrode.In charge and discharge process, Li+
Come and go between two electrodes and embed and deintercalation: during charging, Li+From positive pole deintercalation, embedding negative pole through electrolyte, negative pole is in rich lithium state；During electric discharge the most contrary.The development of lithium ion battery comes from the nineties in last century, the most only 20 years, and in the past 20 years was the once leap of lithium electricity industry, along with various countries more have, to environment, the attention of new forms of energy, lithium ion battery, the development advanced by leaps and bounds.
The negative material being actually used in lithium ion battery at present is essentially all carbon materials, such as electrographite, native graphite, carbonaceous mesophase spherules (MCMB), petroleum coke, carbon fiber, thermal decomposed resins carbon etc..In battery charge and discharge process, lithium is de-in carbon material used as anode/embedding and forms lithium carbon and inserts people's compound LixC6: the practical research to lithium ion battery negative material works substantially around how improving specific discharge capacity and volume and capacity ratio, first charge-discharge efficiency, cycle performance and reduction these several respects of cost expansion in recent years.By whole to the structural word of various carbon materialses (including graphite), surface modification treatment, is formed and has chlamydate compound material structure, forms nanometer opening structure in material with carbon element, and use nano material new technique, research to make lithium deintercalation process in material with carbon element not only by LiC6Stoichiometry is carried out, and also can carry out by non-stoichiometry, makes the specific capacity of carbon materials by LiC6Theoretical capacity value 372mAh/g, bring up to 500～1000mAh/g.It addition, the progress acquired by terms of non-carbon negative material research, also illustrate the bright prospects of lithium ion battery negative material section development to people.Currently used graphite type material limits lithium ion free diffusing in graphite-structure as li-ion electrode materials, constrains the performance of graphite cathode electrochemistry capacitance.These problems make simple carbon negative pole material be difficult to meet the requirement to high performance lithium ion battery such as growing electronic equipment, electric automobile.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of composite cathode material of lithium ion battery to overcome above the deficiencies in the prior art, improve electrode material capacity and discharge stability performance.
Technical scheme is as follows:
The preparation method of a kind of composite cathode material of lithium ion battery, comprises the following steps:
Step one, in parts by weight, by epoxy resin 5-10 part, Merlon 3-6 part, poly butylene succinate 2-5 part, isocyanates 2-4 part and ethyl acetate 30-40 part are uniformly mixed, and are then fed in retort carrying out carbonization, obtain carbonized material one；
Step 2, first soaks carbonized material one 5-10 minute with 1% hydrochloric acid solution, is filtrated to get solid mixture, and solid mixture uses deionized water rinsing to neutral, and filtering drying also grinds, obtains carbonized material two；
Step 3, in parts by weight, by carbonized material two 40-50 part, Graphene 20-30 part, tolyl allophanamide base silane 3-5 part and dioctyl phthalate 1-2 part, join in reactor, reacting by heating 20-30 minute, it is subsequently adding Ammonium persulfate. 0.5-1 part, continues to keep 10-20 minute, obtain intermediate material；
Step 4, dries centre material and grinds, obtaining composite cathode material of lithium ion battery.
The preparation method of described composite cathode material of lithium ion battery, the mixing speed being uniformly mixed in step one is 80-100 rev/min, mixing time 30-40 minute.
The preparation method of described composite cathode material of lithium ion battery, in step one, carbonization temperature is 900-1000 DEG C, carbonization time 3-5 hour.
The preparation method of described composite cathode material of lithium ion battery, the temperature dried in step 2 is 110-120 DEG C.
The preparation method of described composite cathode material of lithium ion battery, in step 3, the heating-up temperature of reacting by heating is 70-80 DEG C.
The preparation method of described composite cathode material of lithium ion battery, the temperature dried in step 4 is 100-110 DEG C.
The composite cathode material of lithium ion battery that the method that the present invention provides prepares has good discharge capacity and discharging efficiency, and after recycling for 300 times, discharging efficiency remains able to reach more than 96.8%.
Detailed description of the invention:
Embodiment 1
The preparation method of a kind of composite cathode material of lithium ion battery, comprises the following steps:
Step one, in parts by weight, by epoxy resin 5 parts, Merlon 3 parts, poly butylene succinate 2 parts, isocyanates 2 parts and ethyl acetate 30 parts are uniformly mixed, and mixing speed is 80 revs/min, mixing time 30 minutes, it is then fed in retort carrying out carbonization, carbonization temperature is 900 DEG C, carbonization time 3 hours, obtains carbonized material one；
Step 2, first soaks carbonized material one 5 minutes with 1% hydrochloric acid solution, is filtrated to get solid mixture, and solid mixture uses deionized water rinsing to neutral, and filtering drying also grinds, and the temperature of drying is 110 DEG C, obtains carbonized material two；
Step 3, in parts by weight, by carbonized material 2 40 parts, Graphene 20 parts, tolyl allophanamide base silane 3 parts and dioctyl phthalate 1 part, join in reactor, reacting by heating 20 minutes, the heating-up temperature of reacting by heating is 70 DEG C, is subsequently adding Ammonium persulfate. 0.5 part, continue to keep 10 minutes, obtain intermediate material；
Step 4, dries centre material and grinds, and the temperature of drying is 100 DEG C, obtains composite cathode material of lithium ion battery.
Embodiment 2
The preparation method of a kind of composite cathode material of lithium ion battery, comprises the following steps:
Step one, in parts by weight, by epoxy resin 6 parts, Merlon 4 parts, poly butylene succinate 3 parts, isocyanates 2 parts and ethyl acetate 34 parts are uniformly mixed, and mixing speed is 85 revs/min, mixing time 36 minutes, it is then fed in retort carrying out carbonization, carbonization temperature is 920 DEG C, carbonization time 4 hours, obtains carbonized material one；
Step 2, first soaks carbonized material one 6 minutes with 1% hydrochloric acid solution, is filtrated to get solid mixture, and solid mixture uses deionized water rinsing to neutral, and filtering drying also grinds, and the temperature of drying is 113 DEG C, obtains carbonized material two；
Step 3, in parts by weight, by carbonized material 2 43 parts, Graphene 22 parts, tolyl allophanamide base silane 4 parts and dioctyl phthalate 1 part, join in reactor, reacting by heating 23 minutes, the heating-up temperature of reacting by heating is 75 DEG C, is subsequently adding Ammonium persulfate. 0.6 part, continue to keep 13 minutes, obtain intermediate material；
Step 4, dries centre material and grinds, and the temperature of drying is 105 DEG C, obtains composite cathode material of lithium ion battery.
Embodiment 3
The preparation method of a kind of composite cathode material of lithium ion battery, comprises the following steps:
Step one, in parts by weight, by epoxy resin 8 parts, Merlon 5 parts, poly butylene succinate 4 parts, isocyanates 3 parts and ethyl acetate 38 parts are uniformly mixed, and mixing speed is 100 revs/min, mixing time 40 minutes, it is then fed in retort carrying out carbonization, carbonization temperature is 1000 DEG C, carbonization time 5 hours, obtains carbonized material one；
Step 2, first soaks carbonized material one 8 minutes with 1% hydrochloric acid solution, is filtrated to get solid mixture, and solid mixture uses deionized water rinsing to neutral, and filtering drying also grinds, and the temperature of drying is 115 DEG C, obtains carbonized material two；
Step 3, in parts by weight, by carbonized material 2 48 parts, Graphene 26 parts, tolyl allophanamide base silane 4 parts and dioctyl phthalate 2 parts, join in reactor, reacting by heating 30 minutes, the heating-up temperature of reacting by heating is 78 DEG C, is subsequently adding Ammonium persulfate. 0.8 part, continue to keep 20 minutes, obtain intermediate material；
Step 4, dries centre material and grinds, and the temperature of drying is 110 DEG C, obtains composite cathode material of lithium ion battery.
Embodiment 4
The preparation method of a kind of composite cathode material of lithium ion battery, comprises the following steps:
Step one, in parts by weight, by epoxy resin 10 parts, Merlon 6 parts, poly butylene succinate 5 parts, isocyanates 4 parts and ethyl acetate 40 parts are uniformly mixed, and mixing speed is 100 revs/min, mixing time 40 minutes, it is then fed in retort carrying out carbonization, carbonization temperature is 1000 DEG C, carbonization time 5 hours, obtains carbonized material one；
Step 2, first soaks carbonized material one 10 minutes with 1% hydrochloric acid solution, is filtrated to get solid mixture, and solid mixture uses deionized water rinsing to neutral, and filtering drying also grinds, and the temperature of drying is 120 DEG C, obtains carbonized material two；
Step 3, in parts by weight, by carbonized material 2 50 parts, Graphene 30 parts, tolyl allophanamide base silane 5 parts and dioctyl phthalate 2 parts, join in reactor, reacting by heating 30 minutes, the heating-up temperature of reacting by heating is 80 DEG C, is subsequently adding Ammonium persulfate. 1 part, continue to keep 20 minutes, obtain intermediate material；
Step 4, dries centre material and grinds, and the temperature of drying is 110 DEG C, obtains composite cathode material of lithium ion battery.
The composite cathode material of lithium ion battery preparing above example carries out performance test, and result is as follows:
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Discharge capacity mAh/g | 750 | 760 | 780 | 770 |
| Efficiency % first | 85 | 86 | 89 | 88 |
| Discharging efficiency % after 300 circulations | 96.8 | 97.6 | 98.1 | 97.5 |
As can be seen from the above results, the composite cathode material of lithium ion battery that the method that the present invention provides prepares has good discharge capacity and discharging efficiency.
Claims (6)
1. the preparation method of a composite cathode material of lithium ion battery, it is characterised in that comprise the following steps:
Step one, in parts by weight, by epoxy resin 5-10 part, Merlon 3-6 part, poly butylene succinate 2-5 part, isocyanates 2-4 part and ethyl acetate 30-40 part are uniformly mixed, and are then fed in retort carrying out carbonization, obtain carbonized material one；
Step 2, first soaks carbonized material one 5-10 minute with 1% hydrochloric acid solution, is filtrated to get solid mixture, and solid mixture uses deionized water rinsing to neutral, and filtering drying also grinds, obtains carbonized material two；
Step 3, in parts by weight, by carbonized material two 40-50 part, Graphene 20-30 part, tolyl allophanamide base silane 3-5 part and dioctyl phthalate 1-2 part, join in reactor, reacting by heating 20-30 minute, it is subsequently adding Ammonium persulfate. 0.5-1 part, continues to keep 10-20 minute, obtain intermediate material；
Step 4, dries centre material and grinds, obtaining composite cathode material of lithium ion battery.
The preparation method of composite cathode material of lithium ion battery the most according to claim 1, it is characterised in that the mixing speed being uniformly mixed in step one is 80-100 rev/min, mixing time 30-40 minute.
The preparation method of composite cathode material of lithium ion battery the most according to claim 1, it is characterised in that in step one, carbonization temperature is 900-1000 DEG C, carbonization time 3-5 hour.
The preparation method of composite cathode material of lithium ion battery the most according to claim 1, it is characterised in that the temperature dried in step 2 is 110-120 DEG C.
The preparation method of composite cathode material of lithium ion battery the most according to claim 1, it is characterised in that in step 3, the heating-up temperature of reacting by heating is 70-80 DEG C.
The preparation method of composite cathode material of lithium ion battery the most according to claim 1, it is characterised in that the temperature dried in step 4 is 100-110 DEG C.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024021335A1 (en) * | 2022-07-25 | 2024-02-01 | Tcl科技集团股份有限公司 | Composite material and preparation method therefor, and light-emitting diode |
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| CN102730680A (en) * | 2012-07-23 | 2012-10-17 | 清华大学深圳研究生院 | High-density high-rigidity graphene porous carbon material as well as preparation method and applications thereof |
| CN103746119A (en) * | 2014-01-05 | 2014-04-23 | 孟红琳 | Preparation method of grapheme-coated carbon microsphere lithium ion battery cathode material |
| CN104934233A (en) * | 2015-04-23 | 2015-09-23 | 中国科学院福建物质结构研究所 | Porous conductive graphene/carbon nanohorn composite material, and preparation method and applications thereof |
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- 2016-05-26 CN CN201610362151.0A patent/CN105845914A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102730680A (en) * | 2012-07-23 | 2012-10-17 | 清华大学深圳研究生院 | High-density high-rigidity graphene porous carbon material as well as preparation method and applications thereof |
| CN103746119A (en) * | 2014-01-05 | 2014-04-23 | 孟红琳 | Preparation method of grapheme-coated carbon microsphere lithium ion battery cathode material |
| CN104934233A (en) * | 2015-04-23 | 2015-09-23 | 中国科学院福建物质结构研究所 | Porous conductive graphene/carbon nanohorn composite material, and preparation method and applications thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024021335A1 (en) * | 2022-07-25 | 2024-02-01 | Tcl科技集团股份有限公司 | Composite material and preparation method therefor, and light-emitting diode |
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