CN109346709A - The anode material for lithium-ion batteries and preparation method thereof of super hydrophobic material cladding - Google Patents
The anode material for lithium-ion batteries and preparation method thereof of super hydrophobic material cladding Download PDFInfo
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- CN109346709A CN109346709A CN201811387184.6A CN201811387184A CN109346709A CN 109346709 A CN109346709 A CN 109346709A CN 201811387184 A CN201811387184 A CN 201811387184A CN 109346709 A CN109346709 A CN 109346709A
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- hydrophobic material
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- 239000000463 material Substances 0.000 title claims abstract description 69
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 56
- 239000010405 anode material Substances 0.000 title claims abstract description 27
- 238000005253 cladding Methods 0.000 title claims abstract description 26
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 12
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 51
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 42
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 34
- 238000000926 separation method Methods 0.000 claims description 22
- 239000007787 solid Substances 0.000 claims description 22
- 239000000725 suspension Substances 0.000 claims description 22
- 239000004611 light stabiliser Substances 0.000 claims description 21
- 239000000377 silicon dioxide Substances 0.000 claims description 21
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 20
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 20
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 20
- 229940008099 dimethicone Drugs 0.000 claims description 20
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 20
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims description 20
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 20
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 19
- 229910000077 silane Inorganic materials 0.000 claims description 19
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 14
- 229910052744 lithium Inorganic materials 0.000 claims description 14
- 239000003795 chemical substances by application Substances 0.000 claims description 13
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 12
- 239000003960 organic solvent Substances 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000005955 Ferric phosphate Substances 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 11
- 229910021641 deionized water Inorganic materials 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 229940032958 ferric phosphate Drugs 0.000 claims description 11
- 229910000399 iron(III) phosphate Inorganic materials 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 238000006277 sulfonation reaction Methods 0.000 claims description 11
- 238000010792 warming Methods 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- ZZLCFHIKESPLTH-UHFFFAOYSA-N 4-Methylbiphenyl Chemical compound C1=CC(C)=CC=C1C1=CC=CC=C1 ZZLCFHIKESPLTH-UHFFFAOYSA-N 0.000 claims description 10
- 239000012046 mixed solvent Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 239000011347 resin Substances 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 7
- SLFVYFOEHHLHDW-UHFFFAOYSA-N n-(trifluoromethyl)aniline Chemical compound FC(F)(F)NC1=CC=CC=C1 SLFVYFOEHHLHDW-UHFFFAOYSA-N 0.000 claims description 5
- OKIRBHVFJGXOIS-UHFFFAOYSA-N 1,2-di(propan-2-yl)benzene Chemical group CC(C)C1=CC=CC=C1C(C)C OKIRBHVFJGXOIS-UHFFFAOYSA-N 0.000 claims 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims 2
- 150000003851 azoles Chemical class 0.000 claims 1
- 229920002545 silicone oil Polymers 0.000 claims 1
- 150000003462 sulfoxides Chemical class 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 12
- 230000002209 hydrophobic effect Effects 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 53
- 230000000052 comparative effect Effects 0.000 description 4
- 229910052493 LiFePO4 Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 2
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N 4-methylimidazole Chemical class CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 description 1
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 1
- PFYQFCKUASLJLL-UHFFFAOYSA-N [Co].[Ni].[Li] Chemical compound [Co].[Ni].[Li] PFYQFCKUASLJLL-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910000398 iron phosphate Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 150000001455 metallic ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 silicon Alkane Chemical class 0.000 description 1
- 238000003860 storage 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- 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
- H01M4/5825—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
-
- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
-
- 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)
- Composite Materials (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a kind of anode material for lithium-ion batteries of super hydrophobic material cladding.It improves the cyclicity and safety of anode material for lithium-ion batteries with excellent hydrophobic electrophilic solution fluidity and electric conductivity.The invention also discloses the methods for the anode material for lithium-ion batteries for preparing super hydrophobic material cladding.Preparation method is simple, easy to operate, reproducible, low raw-material cost, and small pollution of the environment is suitable for industrialized production.
Description
Technical field
The invention belongs to field of lithium ion battery anode, and in particular to a kind of lithium-ion electric of super hydrophobic material cladding
Pond positive electrode and preparation method thereof.
Background technique
The application range of lithium ion battery is constantly expanding, and to the density of battery material, safety and performance is recycled
Propose increasingly higher demands.Density, security performance and recycling of the anode material for lithium-ion batteries to lithium ion battery
Performance has especially great influence, and common anode material for lithium-ion batteries has LiFePO4, cobalt acid lithium, LiMn2O4, nickel cobalt
LiMn2O4, nickel cobalt lithium aluminate and rich lithium material etc..
The composite battery prepared after LiFePO4 and Material cladding, is obviously improved, problem although security performance has
It is that battery moisture before fluid injection is higher, the moisture compared to pure material is higher by more than one times, this is because LiFePO4 primary particle size is small, ratio
Surface area is big, the reasons such as hygroscopic cause.Free acid is generated since moisture is reacted with electrolyte, while corroding negative electrode film also
It will lead to positive electrode surface digestion of metallic ion, composite material cycle performance caused to deteriorate.
Therefore lithium iron phosphate positive material and Material cladding with super-hydrophobic material cladding can take into account its peace simultaneously
It is particularly important entirely with the composite battery in service life.Develop that a kind of covered effect is more preferable, realizes anode material for lithium-ion batteries
The anode material for lithium-ion batteries of the electrophilic solution fluidity and higher electric conductivity of surface hydrophobicity, just by bigger promotion lithium ion battery
Storage, safety and the recycling performance of pole material.
Summary of the invention
In view of the deficiencies of the prior art, the purpose of the present invention is to provide a kind of lithium ion batteries of super hydrophobic material cladding
Positive electrode and preparation method thereof, to reduce the moisture content in pole piece, so as to improve using iron phosphate material as positive electrode
The security performance and recycling performance of lithium ion battery.
To achieve this purpose, the present invention adopts the following technical scheme:
A kind of anode material for lithium-ion batteries of super hydrophobic material cladding, preparing raw material includes: cumyl peroxide, SBS
Or sulfonated SBS, light stabilizer 770, irgasfos 168, nano silica, dimethicone, silane coupling agent and organic molten
Agent；
Preferably, prepare raw material include: cumyl peroxide, SBS or sulfonated SBS, light stabilizer 770, irgasfos 168,
Dimethyl sulfoxide, N,N-dimethylformamide, nano silica, dimethicone, silane resin acceptor kh-550 and silane
Coupling agent KH-560；
It is further preferred that it includes: cumyl peroxide, sulfonated SBS, 3- (4- methyl-1 H- imidazoles -1- that it, which prepares raw material,
Base) -5- (trifluoromethyl) aniline, light stabilizer 770, irgasfos 168, dimethyl sulfoxide, N,N-dimethylformamide, nanometer two
Silica, dimethicone, silane resin acceptor kh-550 and silane coupling agent KH-560；
It is further preferred that it includes: cumyl peroxide 0.1-1 parts by weight, sulfonated SBS 1-10 weight that it, which prepares raw material,
Part, 3- (4- methyl-1 H-imidazole-1-group) -5- (trifluoromethyl) aniline 0.1-3 parts by weight, 770 0.1-3 weight of light stabilizer
Part, irgasfos 168 0.1-3 parts by weight, dimethyl sulfoxide 1-10 parts by weight, N,N-dimethylformamide 1-10 parts by weight, nanometer
Silica 0.1-5 parts by weight, dimethicone 0.1-5 parts by weight, silane resin acceptor kh-550 0.1-5 parts by weight and silicon
Alkane coupling agent KH-560 0.1-5 parts by weight；
Most preferably, preparing raw material includes: 0.4 parts by weight of cumyl peroxide, 4 weight of sulfonated SBS (sulfonation degree 15%)
Part, 770 0.5 parts by weight of light stabilizer, 0.3 parts by weight of irgasfos 168,5 parts by weight of dimethyl sulfoxide, N, N- dimethyl formyl
5 parts by weight of amine, 2 parts by weight of nano silica, 0.7 parts by weight of dimethicone, 0.4 parts by weight of silane resin acceptor kh-550
And 0.4 parts by weight of silane coupling agent KH-560,0.5 weight of 3- (4- methyl-1 H-imidazole-1-group) -5- (trifluoromethyl) aniline
Measure part.
The present invention also provides the preparation methods of the anode material for lithium-ion batteries of super hydrophobic material cladding, including following step
It is rapid:
1) by 0.4 parts by weight of cumyl peroxide, 4 parts by weight of sulfonated SBS (sulfonation degree 15%), 770 0.5 weight of light stabilizer
Amount part and 0.3 parts by weight of irgasfos 168 are dissolved in organic solvent (5 parts by weight of dimethyl sulfoxide and N,N-dimethylformamide 5
The mixed solvent of parts by weight) in, form solution；
2) by the resulting solution of step 1) in the ultrasonic wave of 100w power, ultrasonic 45min, temperature is controlled at 40 DEG C；
3) it is even that 2 parts by weight of nano silica, 0.7 parts by weight of dimethicone, silane are added into the resulting solution of step 2
Join 0.4 parts by weight of agent KH-550 and 0.4 parts by weight of silane coupling agent KH-560,3- (4- methyl-1 H-imidazole-1-group) -5-
Then solution is warming up to 80 DEG C of reaction 5h by 0.5 parts by weight of (trifluoromethyl) aniline；
4) then, the resulting solution of step 3) is poured into deionized water, is filtered, and the vacuum by obtained solid at 100 DEG C is dried
3h drying is in case to get super hydrophobic material；
5) by 200 parts of 100 parts of LiFePO4,0.5 part of above-mentioned super hydrophobic material, 800 parts of dehydrated alcohol and chloroform addition stirrings
In device, 60 DEG C are heated to, after 2h then is sufficiently stirred under 800 revs/min, obtains suspension；
6) above-mentioned suspension is filtered, so that be separated by solid-liquid separation；
7) by solid obtained after separation be heated to 400 DEG C, the time maintain 5h to get to super hydrophobic material cladding ferric phosphate
Anode material of lithium battery.
Compared with prior art, the invention has the following advantages:
The anode material for lithium-ion batteries of super hydrophobic material provided by the invention cladding have excellent hydrophobic electrophilic solution fluidity with
Electric conductivity, and improve the cyclicity and safety of anode material for lithium-ion batteries.The present invention prepares super hydrophobic material cladding
The method of anode material for lithium-ion batteries is simple, easy to operate, reproducible, low raw-material cost, small pollution of the environment, fits
Together in industrialized production.
Specific embodiment
Following number is parts by weight.
Embodiment 1
The present invention provides a kind of methods for preparing super hydrophobic material, and steps are as follows:
1) by 0.3 parts by weight of cumyl peroxide, 3 parts by weight of SBS, 770 0.3 parts by weight of light stabilizer and irgasfos 168
0.2 parts by weight are dissolved in organic solvent (mixed solvents of 5 parts by weight of 5 parts by weight of dimethyl sulfoxide and N,N-dimethylformamide)
In, form solution；
2) by the resulting solution of step 1) in the ultrasonic wave of 100w power, ultrasonic 45min, temperature is controlled at 40 DEG C；
3) it is even that 1 parts by weight of nano silica, 0.5 parts by weight of dimethicone, silane are added into the resulting solution of step 2
Join 0.2 parts by weight of agent KH-550 and 0.3 parts by weight of silane coupling agent KH-560, solution is then warming up to 80 DEG C of reactions
5h；
4) then, the resulting solution of step 3) is poured into deionized water, is filtered, and the vacuum by obtained solid at 100 DEG C is dried
3h drying is in case to get super hydrophobic material；
5) by 200 parts of 100 parts of LiFePO4,0.5 part of above-mentioned super hydrophobic material, 800 parts of dehydrated alcohol and chloroform addition stirrings
In device, 60 DEG C are heated to, after 2h then is sufficiently stirred under 800 revs/min, obtains suspension；
6) suspension is filtered, so that be separated by solid-liquid separation；
7) by solid obtained after separation be heated to 400 DEG C, the time maintain 5h to get to super hydrophobic material cladding ferric phosphate
Anode material of lithium battery.
Embodiment 2
The present invention provides a kind of methods for preparing super hydrophobic material, and steps are as follows:
1) by 1 parts by weight of cumyl peroxide, 5 parts by weight of SBS, 770 0.6 parts by weight of light stabilizer and irgasfos 168
0.5 parts by weight are dissolved in organic solvent (mixed solvents of 5 parts by weight of 5 parts by weight of dimethyl sulfoxide and N,N-dimethylformamide)
In, form solution；
2) by the resulting solution of step 1) in the ultrasonic wave of 100w power, ultrasonic 45min, temperature is controlled at 40 DEG C；
3) 3 parts by weight of nano silica, 1 parts by weight of dimethicone, silane coupled are added into the resulting solution of step 2
Then solution is warming up to 80 DEG C of reaction 5h by 0.5 parts by weight of 0.5 parts by weight of agent KH-550 and silane coupling agent KH-560；
4) then, the resulting solution of step 3) is poured into deionized water, is filtered, and the vacuum by obtained solid at 100 DEG C is dried
3h drying is in case to get super hydrophobic material；
5) by 200 parts of 100 parts of LiFePO4,0.5 part of above-mentioned super hydrophobic material, 800 parts of dehydrated alcohol and chloroform addition stirrings
In device, 60 DEG C are heated to, after 2h then is sufficiently stirred under 800 revs/min, obtains suspension；
6) suspension is filtered, so that be separated by solid-liquid separation；
7) by solid obtained after separation be heated to 400 DEG C, the time maintain 5h to get to super hydrophobic material cladding ferric phosphate
Anode material of lithium battery.
Embodiment 3
The present invention provides a kind of methods for preparing super hydrophobic material, and steps are as follows:
1) by 0.4 parts by weight of cumyl peroxide, 4 parts by weight of SBS, 770 0.5 parts by weight of light stabilizer and irgasfos 168
0.3 parts by weight are dissolved in organic solvent (mixed solvents of 5 parts by weight of 5 parts by weight of dimethyl sulfoxide and N,N-dimethylformamide)
In, form solution；
2) by the resulting solution of step 1) in the ultrasonic wave of 100w power, ultrasonic 45min, temperature is controlled at 40 DEG C；
3) it is even that 2 parts by weight of nano silica, 0.7 parts by weight of dimethicone, silane are added into the resulting solution of step 2
Join 0.4 parts by weight of agent KH-550 and 0.4 parts by weight of silane coupling agent KH-560, solution is then warming up to 80 DEG C of reactions
5h；
4) then, the resulting solution of step 3) is poured into deionized water, is filtered, and the vacuum by obtained solid at 100 DEG C is dried
3h drying is in case to get super hydrophobic material；
5) by 200 parts of 100 parts of LiFePO4,0.5 part of above-mentioned super hydrophobic material, 800 parts of dehydrated alcohol and chloroform addition stirrings
In device, 60 DEG C are heated to, after 2h then is sufficiently stirred under 800 revs/min, obtains suspension；
6) suspension is filtered, so that be separated by solid-liquid separation；
7) by solid obtained after separation be heated to 400 DEG C, the time maintain 5h to get to super hydrophobic material cladding ferric phosphate
Anode material of lithium battery.
Embodiment 4
The present invention provides a kind of methods for preparing super hydrophobic material, and steps are as follows:
1) by 0.4 parts by weight of cumyl peroxide, 4 parts by weight of sulfonated SBS (sulfonation degree 10%), 770 0.5 weight of light stabilizer
Amount part and 0.3 parts by weight of irgasfos 168 are dissolved in organic solvent (5 parts by weight of dimethyl sulfoxide and N,N-dimethylformamide 5
The mixed solvent of parts by weight) in, form solution；
2) by the resulting solution of step 1) in the ultrasonic wave of 100w power, ultrasonic 45min, temperature is controlled at 40 DEG C；
3) it is even that 2 parts by weight of nano silica, 0.7 parts by weight of dimethicone, silane are added into the resulting solution of step 2
Join 0.4 parts by weight of agent KH-550 and 0.4 parts by weight of silane coupling agent KH-560, solution is then warming up to 80 DEG C of reactions
5h；
4) then, the resulting solution of step 3) is poured into deionized water, is filtered, and the vacuum by obtained solid at 100 DEG C is dried
3h drying is in case to get super hydrophobic material；
5) by 200 parts of 100 parts of LiFePO4,0.5 part of above-mentioned super hydrophobic material, 800 parts of dehydrated alcohol and chloroform addition stirrings
In device, 60 DEG C are heated to, after 2h then is sufficiently stirred under 800 revs/min, obtains suspension；
6) suspension is filtered, so that be separated by solid-liquid separation；
7) by solid obtained after separation be heated to 400 DEG C, the time maintain 5h to get to super hydrophobic material cladding ferric phosphate
Anode material of lithium battery.
Embodiment 5
The present invention provides a kind of methods for preparing super hydrophobic material, and steps are as follows:
1) by 0.4 parts by weight of cumyl peroxide, 4 parts by weight of sulfonated SBS (sulfonation degree 15%), 770 0.5 weight of light stabilizer
Amount part and 0.3 parts by weight of irgasfos 168 are dissolved in organic solvent (5 parts by weight of dimethyl sulfoxide and N,N-dimethylformamide 5
The mixed solvent of parts by weight) in, form solution；
2) by the resulting solution of step 1) in the ultrasonic wave of 100w power, ultrasonic 45min, temperature is controlled at 40 DEG C；
3) it is even that 2 parts by weight of nano silica, 0.7 parts by weight of dimethicone, silane are added into the resulting solution of step 2
Join 0.4 parts by weight of agent KH-550 and 0.4 parts by weight of silane coupling agent KH-560, solution is then warming up to 80 DEG C of reactions
5h；
4) then, the resulting solution of step 3) is poured into deionized water, is filtered, and the vacuum by obtained solid at 100 DEG C is dried
3h drying is in case to get super hydrophobic material；
5) by 200 parts of 100 parts of LiFePO4,0.5 part of above-mentioned super hydrophobic material, 800 parts of dehydrated alcohol and chloroform addition stirrings
In device, 60 DEG C are heated to, after 2h then is sufficiently stirred under 800 revs/min, obtains suspension；
6) suspension is filtered, so that be separated by solid-liquid separation；
7) by solid obtained after separation be heated to 400 DEG C, the time maintain 5h to get to super hydrophobic material cladding ferric phosphate
Anode material of lithium battery.
Embodiment 6
The present invention provides a kind of methods for preparing super hydrophobic material, and steps are as follows:
1) by 0.4 parts by weight of cumyl peroxide, 4 parts by weight of sulfonated SBS (sulfonation degree 30%), 770 0.5 weight of light stabilizer
Amount part and 0.3 parts by weight of irgasfos 168 are dissolved in organic solvent (5 parts by weight of dimethyl sulfoxide and N,N-dimethylformamide 5
The mixed solvent of parts by weight) in, form solution；
2) by the resulting solution of step 1) in the ultrasonic wave of 100w power, ultrasonic 45min, temperature is controlled at 40 DEG C；
3) it is even that 2 parts by weight of nano silica, 0.7 parts by weight of dimethicone, silane are added into the resulting solution of step 2
Join 0.4 parts by weight of agent KH-550 and 0.4 parts by weight of silane coupling agent KH-560, solution is then warming up to 80 DEG C of reactions
5h；
4) then, the resulting solution of step 3) is poured into deionized water, is filtered, and the vacuum by obtained solid at 100 DEG C is dried
3h drying is in case to get super hydrophobic material；
5) by 200 parts of 100 parts of LiFePO4,0.5 part of above-mentioned super hydrophobic material, 800 parts of dehydrated alcohol and chloroform addition stirrings
In device, 60 DEG C are heated to, after 2h then is sufficiently stirred under 800 revs/min, obtains suspension；
6) suspension is filtered, so that be separated by solid-liquid separation；
7) by solid obtained after separation be heated to 400 DEG C, the time maintain 5h to get to super hydrophobic material cladding ferric phosphate
Anode material of lithium battery.
Embodiment 7
The present invention provides a kind of methods for preparing super hydrophobic material, and steps are as follows:
1) by 0.4 parts by weight of cumyl peroxide, 4 parts by weight of sulfonated SBS (sulfonation degree 15%), 770 0.5 weight of light stabilizer
Part and 0.3 parts by weight of irgasfos 168 are dissolved in organic solvent (5 weight of 5 parts by weight of dimethyl sulfoxide and N,N-dimethylformamide
Measure the mixed solvent of part) in, form solution；
2) by the resulting solution of step 1) in the ultrasonic wave of 100w power, ultrasonic 45min, temperature is controlled at 40 DEG C；
3) it is even that 2 parts by weight of nano silica, 0.7 parts by weight of dimethicone, silane are added into the resulting solution of step 2
Join 0.4 parts by weight of agent KH-550 and 0.4 parts by weight of silane coupling agent KH-560,3- (4- methyl-1 H-imidazole-1-group) -5-
Then solution is warming up to 80 DEG C of reaction 5h by 0.5 parts by weight of (trifluoromethyl) aniline；
4) then, the resulting solution of step 3) is poured into deionized water, is filtered, and the vacuum by obtained solid at 100 DEG C is dried
3h drying is in case to get super hydrophobic material；
5) by 200 parts of 100 parts of LiFePO4,0.5 part of above-mentioned super hydrophobic material, 800 parts of dehydrated alcohol and chloroform addition stirrings
In device, 60 DEG C are heated to, after 2h then is sufficiently stirred under 800 revs/min, obtains suspension；
6) suspension is filtered, so that be separated by solid-liquid separation；
7) by solid obtained after separation be heated to 400 DEG C, the time maintain 5h to get to super hydrophobic material cladding ferric phosphate
Anode material of lithium battery.
Comparative example 1
The present invention provides a kind of methods for preparing super hydrophobic material, and steps are as follows:
1) by 0.4 parts by weight of cumyl peroxide, 4 parts by weight of sulfonated SBS (sulfonation degree 15%), 770 0.5 weight of light stabilizer
Part and 0.3 parts by weight of irgasfos 168 are dissolved in organic solvent (10 parts by weight of dimethyl sulfoxide), form solution；
2) by the resulting solution of step 1) in the ultrasonic wave of 100w power, ultrasonic 45min, temperature is controlled at 40 DEG C；
3) it is even that 2 parts by weight of nano silica, 0.7 parts by weight of dimethicone, silane are added into the resulting solution of step 2
Join 0.4 parts by weight of agent KH-550 and 0.4 parts by weight of silane coupling agent KH-560,3- (4- methyl-1 H-imidazole-1-group) -5-
Then solution is warming up to 80 DEG C of reaction 5h by 0.5 parts by weight of (trifluoromethyl) aniline；
4) then, the resulting solution of step 3) is poured into deionized water, is filtered, and the vacuum by obtained solid at 100 DEG C is dried
3h drying is in case to get super hydrophobic material；
5) by 200 parts of 100 parts of LiFePO4,0.5 part of above-mentioned super hydrophobic material, 800 parts of dehydrated alcohol and chloroform addition stirrings
In device, 60 DEG C are heated to, after 2h then is sufficiently stirred under 800 revs/min, obtains suspension；
6) suspension is filtered, so that be separated by solid-liquid separation；
7) by solid obtained after separation be heated to 400 DEG C, the time maintain 5h to get to super hydrophobic material cladding ferric phosphate
Anode material of lithium battery.
Comparative example 2
The present invention provides a kind of methods for preparing super hydrophobic material, and steps are as follows:
1) by 0.4 parts by weight of cumyl peroxide, 4 parts by weight of sulfonated SBS (sulfonation degree 15%), 770 0.5 weight of light stabilizer
Part and 0.3 parts by weight of irgasfos 168 are dissolved in organic solvent (5 weight of 5 parts by weight of dimethyl sulfoxide and N,N-dimethylformamide
Measure the mixed solvent of part) in, form solution；
2) by the resulting solution of step 1) in the ultrasonic wave of 100w power, ultrasonic 45min, temperature is controlled at 40 DEG C；
3) it is even that 2 parts by weight of nano silica, 0.7 parts by weight of dimethicone, silane are added into the resulting solution of step 2
Join 0.4 parts by weight of agent KH-550 and 0.4 parts by weight of silane coupling agent KH-560,3- (4- methyl-1 H-imidazole-1-group) -5-
Then solution is warming up to 80 DEG C of reaction 5h by 0.5 parts by weight of (trifluoromethyl) aniline；
4) then, the resulting solution of step 3) is poured into deionized water, is filtered, and the vacuum by obtained solid at 100 DEG C is dried
3h drying is in case to get super hydrophobic material；
5) it by 1000 parts of 100 parts of LiFePO4,0.5 part of above-mentioned super hydrophobic material, dehydrated alcohol addition blenders, is heated to
60 DEG C, after 2h then is sufficiently stirred under 800 revs/min, obtain suspension；
6) suspension is filtered, so that be separated by solid-liquid separation；
7) by solid obtained after separation be heated to 400 DEG C, the time maintain 5h to get to super hydrophobic material cladding ferric phosphate
Anode material of lithium battery.
Performance test
The lithium battery for the lithium iron phosphate battery positive material for using the super hydrophobic material of any one of embodiment 1-7 to coat is surveyed
Examination, as a result as shown in the table:
| Example | 100 weeks capacity retention ratios of 10C circulation |
| Embodiment 1 | 87% |
| Embodiment 2 | 83% |
| Embodiment 3 | 90% |
| Embodiment 4 | 96% |
| Embodiment 5 | 95% |
| Embodiment 6 | 88% |
| Embodiment 7 | 98% |
| Comparative example 1 | 86% |
| Comparative example 2 | 84% |
Embodiment described above be only embodiments of the present invention are described, not to the scope of the present invention into
Row limits, and without departing from the spirit of the design of the present invention, those of ordinary skill in the art make technical solution of the present invention
Modification and improvement out should all be fallen into the protection scope that claims of the present invention determines.
Claims (6)
1. a kind of anode material for lithium-ion batteries of super hydrophobic material cladding, which is characterized in that it includes: peroxidating that it, which prepares raw material,
It is diisopropylbenzene (DIPB), SBS or sulfonated SBS, light stabilizer 770, irgasfos 168, nano silica, dimethicone, silane coupled
Agent and organic solvent.
2. material according to claim 1, which is characterized in that its prepare raw material include: cumyl peroxide, SBS or
Sulfonated SBS, light stabilizer 770, irgasfos 168, dimethyl sulfoxide, N,N-dimethylformamide, nano silica, dimethyl
Silicone oil, silane resin acceptor kh-550 and silane coupling agent KH-560.
3. material according to claim 2, which is characterized in that it includes: cumyl peroxide, sulfonation that it, which prepares raw material,
SBS, 3- (4- methyl-1 H-imidazole-1-group) -5- (trifluoromethyl) aniline, light stabilizer 770, irgasfos 168, dimethyl are sub-
Sulfone, N,N-dimethylformamide, nano silica, dimethicone, silane resin acceptor kh-550 and silane coupling agent KH-
560。
4. material according to claim 3, which is characterized in that it includes: cumyl peroxide 0.1-1 weight that it, which prepares raw material,
Measure part, sulfonated SBS 1-10 parts by weight, 3- (4- methyl-1 H-imidazole-1-group) -5- (trifluoromethyl) aniline 0.1-3 parts by weight,
770 0.1-3 parts by weight of light stabilizer, irgasfos 168 0.1-3 parts by weight, dimethyl sulfoxide 1-10 parts by weight, N, N- dimethyl
Formamide 1-10 parts by weight, nano silica 0.1-5 parts by weight, dimethicone 0.1-5 parts by weight, silane coupling agent KH-
550 0.1-5 parts by weight and silane coupling agent KH-560 0.1-5 parts by weight.
5. material according to claim 4, which is characterized in that it includes: 0.4 weight of cumyl peroxide that it, which prepares raw material,
Part, 4 parts by weight of sulfonated SBS (sulfonation degree 15%), 770 0.5 parts by weight of light stabilizer, 0.3 parts by weight of irgasfos 168, diformazan
5 parts by weight of base sulfoxide, 5 parts by weight of N,N-dimethylformamide, 2 parts by weight of nano silica, 0.7 weight of dimethicone
Part, 0.4 parts by weight of 0.4 parts by weight of silane resin acceptor kh-550 and silane coupling agent KH-560,3- (4- methyl-1 H- miaow
Azoles -1- base) 0.5 parts by weight of -5- (trifluoromethyl) aniline.
6. a kind of preparation method of the anode material for lithium-ion batteries of super hydrophobic material cladding, which is characterized in that including following step
It is rapid:
1) by 0.4 parts by weight of cumyl peroxide, 4 parts by weight of sulfonated SBS (sulfonation degree 15%), 770 0.5 weight of light stabilizer
Amount part and 0.3 parts by weight of irgasfos 168 are dissolved in organic solvent (5 parts by weight of dimethyl sulfoxide and N,N-dimethylformamide 5
The mixed solvent of parts by weight) in, form solution；
2) by the resulting solution of step 1) in the ultrasonic wave of 100w power, ultrasonic 45min, temperature is controlled at 40 DEG C；
3) it is even that 2 parts by weight of nano silica, 0.7 parts by weight of dimethicone, silane are added into the resulting solution of step 2
Join 0.4 parts by weight of agent KH-550 and 0.4 parts by weight of silane coupling agent KH-560,3- (4- methyl-1 H-imidazole-1-group) -5-
Then solution is warming up to 80 DEG C of reaction 5h by 0.5 parts by weight of (trifluoromethyl) aniline；
4) then, the resulting solution of step 3) is poured into deionized water, is filtered, and the vacuum by obtained solid at 100 DEG C is dried
3h drying is in case to get super hydrophobic material；
5) by 200 parts of 100 parts of LiFePO4,0.5 part of above-mentioned super hydrophobic material, 800 parts of dehydrated alcohol and chloroform addition stirrings
In device, 60 DEG C are heated to, after 2h then is sufficiently stirred under 800 revs/min, obtains suspension；
6) above-mentioned suspension is filtered, so that be separated by solid-liquid separation；
7) by solid obtained after separation be heated to 400 DEG C, the time maintain 5h to get to super hydrophobic material cladding ferric phosphate
Anode material of lithium battery.
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| CN112382761A (en) * | 2020-10-30 | 2021-02-19 | 东莞东阳光科研发有限公司 | SiO (silicon dioxide)2Coated ternary positive electrode material and preparation method thereof |
| CN113428849A (en) * | 2021-06-16 | 2021-09-24 | 张静 | Modified lithium iron phosphate cathode material and preparation method and application thereof |
| WO2024045028A1 (en) * | 2022-08-31 | 2024-03-07 | 宁德时代新能源科技股份有限公司 | Positive electrode material and preparation method therefor, positive electrode composite material and preparation method therefor, secondary battery, and electric device |
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| CN112382761A (en) * | 2020-10-30 | 2021-02-19 | 东莞东阳光科研发有限公司 | SiO (silicon dioxide)2Coated ternary positive electrode material and preparation method thereof |
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