CN105958065A - Cathode material for lithium battery used in electric automobile - Google Patents
Cathode material for lithium battery used in electric automobile Download PDFInfo
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- CN105958065A CN105958065A CN201610402031.9A CN201610402031A CN105958065A CN 105958065 A CN105958065 A CN 105958065A CN 201610402031 A CN201610402031 A CN 201610402031A CN 105958065 A CN105958065 A CN 105958065A
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- lithium battery
- electric automobile
- anode
- battery material
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 31
- 239000010406 cathode material Substances 0.000 title abstract 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 48
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 44
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 42
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 32
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229920002678 cellulose Polymers 0.000 claims abstract description 19
- 239000001913 cellulose Substances 0.000 claims abstract description 19
- 238000002156 mixing Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 16
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims abstract description 14
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 14
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 14
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 14
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920000193 polymethacrylate Polymers 0.000 claims abstract description 14
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 14
- 239000011734 sodium Substances 0.000 claims abstract description 14
- 239000008117 stearic acid Substances 0.000 claims abstract description 14
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 13
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 229920002401 polyacrylamide Polymers 0.000 claims abstract description 13
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 26
- 125000003118 aryl group Chemical group 0.000 claims description 18
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- JLPULHDHAOZNQI-ZTIMHPMXSA-N 1-hexadecanoyl-2-(9Z,12Z-octadecadienoyl)-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCC\C=C/C\C=C/CCCCC JLPULHDHAOZNQI-ZTIMHPMXSA-N 0.000 claims description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 12
- 238000003763 carbonization Methods 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- INHCSSUBVCNVSK-UHFFFAOYSA-L lithium sulfate Inorganic materials [Li+].[Li+].[O-]S([O-])(=O)=O INHCSSUBVCNVSK-UHFFFAOYSA-L 0.000 claims description 12
- 229940083466 soybean lecithin Drugs 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 229910052717 sulfur Inorganic materials 0.000 claims description 12
- 239000011593 sulfur Substances 0.000 claims description 12
- -1 sulfur sulfoxides Chemical class 0.000 claims description 12
- RBTVSNLYYIMMKS-UHFFFAOYSA-N tert-butyl 3-aminoazetidine-1-carboxylate;hydrochloride Chemical compound Cl.CC(C)(C)OC(=O)N1CC(N)C1 RBTVSNLYYIMMKS-UHFFFAOYSA-N 0.000 claims description 12
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- 239000012300 argon atmosphere Substances 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 5
- 239000004215 Carbon black (E152) Substances 0.000 claims description 5
- RNAHRGJHYXOCID-UHFFFAOYSA-N NN=CN=N.NN=CN=N.C1=CC=CC=C1.Cl Chemical group NN=CN=N.NN=CN=N.C1=CC=CC=C1.Cl RNAHRGJHYXOCID-UHFFFAOYSA-N 0.000 claims description 5
- 229930195733 hydrocarbon Natural products 0.000 claims description 5
- 150000002430 hydrocarbons Chemical class 0.000 claims description 5
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 5
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 5
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 5
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical group OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 5
- SVIJYLPSHPPVQF-UHFFFAOYSA-N 2-[2,2-diaminoethyl(dodecyl)amino]acetic acid Chemical compound CCCCCCCCCCCCN(CC(N)N)CC(O)=O SVIJYLPSHPPVQF-UHFFFAOYSA-N 0.000 claims description 3
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 3
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 3
- RFRMMZAKBNXNHE-UHFFFAOYSA-N 6-[4,6-dihydroxy-5-(2-hydroxyethoxy)-2-(hydroxymethyl)oxan-3-yl]oxy-2-(hydroxymethyl)-5-(2-hydroxypropoxy)oxane-3,4-diol Chemical compound CC(O)COC1C(O)C(O)C(CO)OC1OC1C(O)C(OCCO)C(O)OC1CO RFRMMZAKBNXNHE-UHFFFAOYSA-N 0.000 claims description 2
- 238000007599 discharging Methods 0.000 abstract description 6
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 abstract 2
- 229910000360 iron(III) sulfate Inorganic materials 0.000 abstract 2
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 abstract 2
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 abstract 1
- 244000068988 Glycine max Species 0.000 abstract 1
- 235000010469 Glycine max Nutrition 0.000 abstract 1
- 239000010692 aromatic oil Substances 0.000 abstract 1
- 239000002041 carbon nanotube Substances 0.000 abstract 1
- 229910021393 carbon nanotube Inorganic materials 0.000 abstract 1
- 238000010000 carbonizing Methods 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000000787 lecithin Substances 0.000 abstract 1
- 229940067606 lecithin Drugs 0.000 abstract 1
- 235000010445 lecithin Nutrition 0.000 abstract 1
- 239000004417 polycarbonate Substances 0.000 abstract 1
- 229920000515 polycarbonate Polymers 0.000 abstract 1
- 230000001737 promoting effect Effects 0.000 abstract 1
- 230000004087 circulation Effects 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 229910032387 LiCoO2 Inorganic materials 0.000 description 2
- 229910010710 LiFePO Inorganic materials 0.000 description 2
- 229910052493 LiFePO4 Inorganic materials 0.000 description 2
- 229910003005 LiNiO2 Inorganic materials 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 2
- 239000002011 CNT10 Substances 0.000 description 1
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 229910052609 olivine Inorganic materials 0.000 description 1
- 239000010450 olivine Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- 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
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Carbon And Carbon Compounds (AREA)
- Secondary Cells (AREA)
Abstract
The invention provides a cathode material for a lithium battery used in electric automobiles. The cathode material is prepared from the following raw materials: carbon nano tubes, polycarbonate, polyethylene glycol, citric acid, cellulose, thionyl chloride, graphene, sodium carbonate, aromatic oil, polyacrylamide, soya bean lecithin, ammonium persulfate, lithium ferric sulfate, stearic acid, sodium polymethacrylate and ethyl acetate. A preparation method thereof comprises the following steps: firstly preparing modified carbon nano tubes and modified graphene, then mixing the modified carbon nano tubes and the modified graphene with the lithium ferric sulfate, the stearic acid, the sodium polymethacrylate, the ethyl acetate and a dispersing agent, cleaning with deionized water after carbonizing the mixture, and drying to obtain the cathode material. The cathode material for the lithium battery used in the electric automobiles provided by the invention has higher first discharging efficiency and discharge capacity, and the capacitance loss ratio after manifold cycles is relatively low, so that the discharge capacity is improved, and the cathode material has a high promotional value.
Description
Technical field
The invention belongs to anode material of lithium battery technical field, be specifically related to the anode for lithium battery material that a kind of electric automobile uses.
Background technology
Lithium ion battery is current the most most practicality and the high-energy secondary battery of development prospect, owing in commercial Li-ion battery, the specific capacity of Carbon anode is up to above 300mAh g-1, and the specific capacity of the higher positive electrode of price is relatively low.In order to reach capacity matching, more positive electrode need to be used, positive electrode is made to occupy more than the 40% of whole battery cost, and the safety of battery is also heavily dependent on positive electrode, therefore studies, develop cheap, excellent performance, positive electrode that safety is good is the focus of current Study on Li-ion batteries.At present, widely used positive electrode has LiCoO2、LiNiO2And LiMn2O4Deng, but LiCoO2Actual specific capacity relatively low, and the poisonous resource-constrained of cobalt, in degree of depth charge and discharge process, easily discharge oxygen and produce blast；LiNiO2It is difficult to metering more poor than synthesis, lot stability；LiMn2O4Cyclical stability is poor, and the large-scale commercial of lithium ion battery especially electrokinetic cell is all applied and caused obstacle by these shortcomings.
The LiFePO of olivine structural4High (the theoretical specific capacity 170mAh g of specific capacity-1, actual specific capacity is higher than 130mAh g-1), heat stability and cycle performance are excellent, have good heat stability and safety, and abundant raw material source, cheap, environmental friendliness under full-charge state, being the positive electrode of great potential and Development volue, its large-scale production demand meets the strategy and policy of China's sustainable development.The subject matter restricting its large-scale application at present is its poor electronic conductivity and Ionic diffusion energy, although can improve LiFePO by cladding, doping or morphology control etc.4Chemical property, and wherein LiFePO4The most part industrialization, but LiFePO4The performance of positive electrode also needs to the most perfect, the especially improvement of charge-discharge performance under high magnification, and this for power battery material exploitation it is critical that.
Summary of the invention
Anode for lithium battery material that it is an object of the invention to overcome the deficiencies in the prior art and provide a kind of electric automobile to use and preparation method thereof, this positive electrode has higher discharging efficiency first and a discharge capacity, and repeatedly capacitance loss rate after circulation is relatively low.
The anode for lithium battery material that a kind of electric automobile uses, raw material includes in parts by weight: CNT 5～10 parts, Merlon 2～6 parts, Polyethylene Glycol 2～5 parts, citric acid 1～3 parts, cellulose 3～8 parts, two sulfur sulfoxides 3～7 parts, Graphene 5～10 parts, sodium carbonate 2～6 parts, aromatic naphtha 3～7 parts, polyacrylamide 1～5 parts, soybean lecithin 2～6 parts, Ammonium persulfate. 1～5 parts, lithium sulfate ferrum 10～20 parts, stearic acid 2～5 parts, sodium polymethacrylate 1～7 parts, ethyl acetate 2～6 parts.
Further, described cellulose is hydroxypropyl methyl cellulose or hydroxyethyl cellulose.
Further, described aromatic naphtha is toluene or dimethylbenzene.
Further, described dispersant is Benzene Chloride diformazan hydrocarbon ammonium or dodecyl diamino ethyl glycine.
The preparation method of the anode for lithium battery material that described electric automobile uses, comprises the following steps:
Step 1, takes CNT, Merlon, Polyethylene Glycol, citric acid, cellulose add in water, ultrasonic disperse, drip two sulfur sulfoxides, stirring, 60～90 DEG C of back flow reaction 4～6h, after letting cool through sucking filtration, wash, be dried, obtain modified carbon nano-tube；
Step 2, takes Graphene, sodium carbonate, aromatic naphtha, polyacrylamide, soybean lecithin, Ammonium persulfate., and mixing, at CO2Under atmosphere 50～70 DEG C stirring reaction 3～6h, after letting cool through sucking filtration, wash, be dried, obtain modified graphene；
Step 3, takes modified carbon nano-tube, modified graphene, lithium sulfate ferrum, stearic acid, sodium polymethacrylate, ethyl acetate, dispersant, mixing, and mixture is intensification carbonization in argon atmosphere, will clean with deionized water after being cooled to room temperature, is dried, to obtain final product.
Further, in step 1, the temperature of water is 0～4 DEG C.
Further, in step 1, ultrasonic disperse condition is 30～60KHz, 10～15min.
Further, in step 2, mixing speed is 200～400rpm.
Further, in step 3, carbonization condition is 800～1000 DEG C, 2～4h.
Further, in step 3, baking temperature is 90～120 DEG C.
The anode for lithium battery material discharge capacity first that the electric automobile that the present invention provides uses is at more than 7mAh/g, discharging efficiency has reached more than 70% first, discharge capacity loss rate after 1000 circulations has reached less than 3.2%, electric current 30C discharge capacity has reached more than 695mAh/g, and electric current 30C discharge capacity rate has reached more than 95.3%.
Detailed description of the invention
Embodiment 1
The anode for lithium battery material that a kind of electric automobile uses, raw material includes in parts by weight: CNT 5 parts, Merlon 2 parts, Polyethylene Glycol 2 parts, citric acid 1 part, cellulose 3 parts, two sulfur sulfoxides 3 parts, Graphene 5 parts, sodium carbonate 2 parts, aromatic naphtha 3 parts, polyacrylamide 1 part, soybean lecithin 2 parts, Ammonium persulfate. 1 part, lithium sulfate ferrum 10 parts, stearic acid 2 parts, sodium polymethacrylate 1 part, ethyl acetate 2 parts.
Wherein, described cellulose is hydroxypropyl methyl cellulose, and aromatic naphtha is toluene, and dispersant is Benzene Chloride diformazan hydrocarbon ammonium.
The preparation method of the anode for lithium battery material that described electric automobile uses, comprises the following steps:
Step 1, takes CNT, Merlon, Polyethylene Glycol, citric acid, cellulose add in water, ultrasonic disperse, drip two sulfur sulfoxides, stirring, 60 DEG C of back flow reaction 6h, after letting cool through sucking filtration, wash, be dried, obtain modified carbon nano-tube；
Step 2, takes Graphene, sodium carbonate, aromatic naphtha, polyacrylamide, soybean lecithin, Ammonium persulfate., and mixing, at CO2Atmosphere lower 50 DEG C stirring reaction 6h, after letting cool through sucking filtration, wash, be dried, obtain modified graphene；
Step 3, takes modified carbon nano-tube, modified graphene, lithium sulfate ferrum, stearic acid, sodium polymethacrylate, ethyl acetate, dispersant, mixing, and mixture is intensification carbonization in argon atmosphere, will clean with deionized water after being cooled to room temperature, is dried, to obtain final product.
Wherein, in step 1, the temperature of water is 0 DEG C, and ultrasonic disperse condition is 30KHz, 15min；In step 2, mixing speed is 200rpm；In step 3, carbonization condition is 800 DEG C, 4h, and baking temperature is 90 DEG C.
Embodiment 2
The anode for lithium battery material that a kind of electric automobile uses, raw material includes in parts by weight: CNT 8 parts, Merlon 4 parts, Polyethylene Glycol 3 parts, citric acid 2 parts, cellulose 6 parts, two sulfur sulfoxides 5 parts, Graphene 8 parts, sodium carbonate 3 parts, aromatic naphtha 4 parts, polyacrylamide 2 parts, soybean lecithin 4 parts, Ammonium persulfate. 2 parts, lithium sulfate ferrum 15 parts, stearic acid 3 parts, sodium polymethacrylate 5 parts, ethyl acetate 2 parts.
Wherein, described cellulose is hydroxyethyl cellulose, and aromatic naphtha is dimethylbenzene, and dispersant is dodecyl diamino ethyl glycine.
The preparation method of the anode for lithium battery material that described electric automobile uses, comprises the following steps:
Step 1, takes CNT, Merlon, Polyethylene Glycol, citric acid, cellulose add in water, ultrasonic disperse, drip two sulfur sulfoxides, stirring, 70 DEG C of back flow reaction 5h, after letting cool through sucking filtration, wash, be dried, obtain modified carbon nano-tube；
Step 2, takes Graphene, sodium carbonate, aromatic naphtha, polyacrylamide, soybean lecithin, Ammonium persulfate., and mixing, at CO2Atmosphere lower 60 DEG C stirring reaction 4h, after letting cool through sucking filtration, wash, be dried, obtain modified graphene；
Step 3, takes modified carbon nano-tube, modified graphene, lithium sulfate ferrum, stearic acid, sodium polymethacrylate, ethyl acetate, dispersant, mixing, and mixture is intensification carbonization in argon atmosphere, will clean with deionized water after being cooled to room temperature, is dried, to obtain final product.
Wherein, in step 1, the temperature of water is 4 DEG C, and ultrasonic disperse condition is 50KHz, 10min；In step 2, mixing speed is 300rpm；In step 3, carbonization condition is 900 DEG C, 3h, and baking temperature is 100 DEG C.
Embodiment 3
The anode for lithium battery material that a kind of electric automobile uses, raw material includes in parts by weight: CNT 8 parts, Merlon 5 parts, Polyethylene Glycol 3 parts, citric acid 2 parts, cellulose 4 parts, two sulfur sulfoxides 6 parts, Graphene 9 parts, sodium carbonate 4 parts, aromatic naphtha 6 parts, polyacrylamide 3 parts, soybean lecithin 5 parts, Ammonium persulfate. 3 parts, lithium sulfate ferrum 14 parts, stearic acid 3 parts, sodium polymethacrylate 4 parts, ethyl acetate 3 parts.
Wherein, described cellulose is hydroxypropyl methyl cellulose, and aromatic naphtha is toluene, and dispersant is Benzene Chloride diformazan hydrocarbon ammonium.
The preparation method of the anode for lithium battery material that described electric automobile uses, comprises the following steps:
Step 1, takes CNT, Merlon, Polyethylene Glycol, citric acid, cellulose add in water, ultrasonic disperse, drip two sulfur sulfoxides, stirring, 80 DEG C of back flow reaction 4h, after letting cool through sucking filtration, wash, be dried, obtain modified carbon nano-tube；
Step 2, takes Graphene, sodium carbonate, aromatic naphtha, polyacrylamide, soybean lecithin, Ammonium persulfate., and mixing, at CO2Atmosphere lower 55 DEG C stirring reaction 4h, after letting cool through sucking filtration, wash, be dried, obtain modified graphene；
Step 3, takes modified carbon nano-tube, modified graphene, lithium sulfate ferrum, stearic acid, sodium polymethacrylate, ethyl acetate, dispersant, mixing, and mixture is intensification carbonization in argon atmosphere, will clean with deionized water after being cooled to room temperature, is dried, to obtain final product.
Wherein, in step 1, the temperature of water is 4 DEG C, and ultrasonic disperse condition is 30KHz, 15min；In step 2, mixing speed is 200rpm；In step 3, carbonization condition is 800 DEG C, 4h, and baking temperature is 90～120 DEG C.
Embodiment 4
The anode for lithium battery material that a kind of electric automobile uses, raw material includes in parts by weight: CNT 10 parts, Merlon 6 parts, Polyethylene Glycol 5 parts, citric acid 3 parts, cellulose 8 parts, two sulfur sulfoxides 7 parts, Graphene 10 parts, sodium carbonate 6 parts, aromatic naphtha 7 parts, polyacrylamide 5 parts, soybean lecithin 6 parts, Ammonium persulfate. 5 parts, lithium sulfate ferrum 20 parts, stearic acid 5 parts, sodium polymethacrylate 7 parts, ethyl acetate 6 parts.
Wherein, described cellulose is hydroxypropyl methyl cellulose, and aromatic naphtha is toluene, and dispersant is Benzene Chloride diformazan hydrocarbon ammonium.
The preparation method of the anode for lithium battery material that described electric automobile uses, comprises the following steps:
Step 1, takes CNT, Merlon, Polyethylene Glycol, citric acid, cellulose add in water, ultrasonic disperse, drip two sulfur sulfoxides, stirring, 90 DEG C of back flow reaction 4h, after letting cool through sucking filtration, wash, be dried, obtain modified carbon nano-tube；
Step 2, takes Graphene, sodium carbonate, aromatic naphtha, polyacrylamide, soybean lecithin, Ammonium persulfate., and mixing, at CO2Atmosphere lower 70 DEG C stirring reaction 3h, after letting cool through sucking filtration, wash, be dried, obtain modified graphene；
Step 3, takes modified carbon nano-tube, modified graphene, lithium sulfate ferrum, stearic acid, sodium polymethacrylate, ethyl acetate, dispersant, mixing, and mixture is intensification carbonization in argon atmosphere, will clean with deionized water after being cooled to room temperature, is dried, to obtain final product.
Wherein, in step 1, the temperature of water is 4 DEG C, and ultrasonic disperse condition is 60KHz, 10min；In step 2, mixing speed is 400rpm；In step 3, carbonization condition is 1000 DEG C, 2h, and baking temperature is 120 DEG C.
Embodiment 5
The present embodiment is with the difference of embodiment 3: the raw material of positive electrode does not comprise citric acid.
Embodiment 6
The present embodiment is with the difference of embodiment 3: the raw material of positive electrode does not comprise sodium carbonate.
Embodiment 1 to 6 gained positive electrode is carried out performance test, and result is as follows:
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | |
| Discharge capacity mAh/g first | 742 | 720 | 750 | 715 | 650 | 730 |
| Efficiency % first | 73 | 74 | 78 | 70 | 73 | 59 |
| Discharge capacity mAh/g after 1000 circulations | 708 | 715 | 735 | 710 | 620 | 680 |
| Discharge capacity loss rate % after 1000 circulations | 3.2 | 2.8 | 2.3 | 3.0 | 6 | 5.8 |
| Electric current 30C discharge capacity mAh/g | 695 | 712 | 730 | 725 | 610 | 705 |
| Electric current 30C discharge capacity rate % | 95.3 | 96.5 | 97.3 | 95.6 | 92.7 | 96.3 |
As seen from the above table, the anode for lithium battery material discharge capacity first that the electric automobile that the present invention provides uses is at more than 7mAh/g, discharging efficiency has reached more than 70% first, discharge capacity loss rate after 1000 circulations has reached less than 3.2%, electric current 30C discharge capacity has reached more than 695mAh/g, and electric current 30C discharge capacity rate has reached more than 95.3%.In embodiment 5, owing to not adding citric acid, cause discharge capacity first substantially to reduce, 1000 circulation after discharge capacity loss rate decline the most obvious, electric current 30C discharge capacity also reduces the most serious simultaneously, the addition being possibly due to citric acid can allow CNT present gap structure, increase discharge capacity, improve electric capacity stability；Owing to not adding sodium carbonate in embodiment 6, causing discharging efficiency first to reduce, the discharge capacity loss rate after 1000 circulations also declines simultaneously, shows that the introducing of sodium carbonate can change the structure of Graphene, thus affects discharging efficiency and discharge stability.
Claims (10)
1. the anode for lithium battery material that an electric automobile uses, it is characterized in that: raw material includes in parts by weight: CNT 5～10 parts, Merlon 2～6 parts, Polyethylene Glycol 2～5 parts, citric acid 1～3 parts, cellulose 3～8 parts, two sulfur sulfoxides 3～7 parts, Graphene 5～10 parts, sodium carbonate 2～6 parts, aromatic naphtha 3～7 parts, polyacrylamide 1～5 parts, soybean lecithin 2～6 parts, Ammonium persulfate. 1～5 parts, lithium sulfate ferrum 10～20 parts, stearic acid 2～5 parts, sodium polymethacrylate 1～7 parts, ethyl acetate 2～6 parts.
The anode for lithium battery material that electric automobile the most according to claim 1 uses, it is characterised in that: described cellulose is hydroxypropyl methyl cellulose or hydroxyethyl cellulose.
The anode for lithium battery material that electric automobile the most according to claim 1 uses, it is characterised in that: described aromatic naphtha is toluene or dimethylbenzene.
The anode for lithium battery material that electric automobile the most according to claim 1 uses, it is characterised in that: described dispersant is Benzene Chloride diformazan hydrocarbon ammonium or dodecyl diamino ethyl glycine.
5. the preparation method of the anode for lithium battery material that the electric automobile described in claim 1 uses, it is characterised in that: comprise the following steps:
Step 1, takes CNT, Merlon, Polyethylene Glycol, citric acid, cellulose add in water, ultrasonic disperse, drip two sulfur sulfoxides, stirring, 60～90 DEG C of back flow reaction 4～6h, after letting cool through sucking filtration, wash, be dried, obtain modified carbon nano-tube；
Step 2, takes Graphene, sodium carbonate, aromatic naphtha, polyacrylamide, soybean lecithin, Ammonium persulfate., and mixing, at CO2Under atmosphere 50～70 DEG C stirring reaction 3～6h, after letting cool through sucking filtration, wash, be dried, obtain modified graphene；
Step 3, takes modified carbon nano-tube, modified graphene, lithium sulfate ferrum, stearic acid, sodium polymethacrylate, ethyl acetate, dispersant, mixing, and mixture is intensification carbonization in argon atmosphere, will clean with deionized water after being cooled to room temperature, is dried, to obtain final product.
The preparation method of the anode for lithium battery material that electric automobile the most according to claim 5 uses, it is characterised in that: in step 1, the temperature of water is 0～4 DEG C.
The preparation method of the anode for lithium battery material that electric automobile the most according to claim 5 uses, it is characterised in that: in step 1, ultrasonic disperse condition is 30～60KHz, 10～15min.
The preparation method of the anode for lithium battery material that electric automobile the most according to claim 5 uses, it is characterised in that: in step 2, mixing speed is 200～400rpm.
The preparation method of the anode for lithium battery material that electric automobile the most according to claim 5 uses, it is characterised in that: in step 3, carbonization condition is 800～1000 DEG C, 2～4h.
The preparation method of the anode for lithium battery material that electric automobile the most according to claim 5 uses, it is characterised in that: in step 3, baking temperature is 90～120 DEG C.
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| CN102208622A (en) * | 2011-04-21 | 2011-10-05 | 湖南大学 | Method for preparing linear nano carbon conductive agent coated lithium iron phosphate anode material |
| CN103178244A (en) * | 2011-12-23 | 2013-06-26 | 财团法人工业技术研究院 | Hybrid energy storage element |
| CN103545514A (en) * | 2013-10-30 | 2014-01-29 | 合肥恒能新能源科技有限公司 | Graphene-modified lithium iron phosphate material as well as preparation method thereof |
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| CN102208622A (en) * | 2011-04-21 | 2011-10-05 | 湖南大学 | Method for preparing linear nano carbon conductive agent coated lithium iron phosphate anode material |
| CN103178244A (en) * | 2011-12-23 | 2013-06-26 | 财团法人工业技术研究院 | Hybrid energy storage element |
| CN103545514A (en) * | 2013-10-30 | 2014-01-29 | 合肥恒能新能源科技有限公司 | Graphene-modified lithium iron phosphate material as well as preparation method thereof |
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