CN106328253B - Graphene combination electrode material of storing up electricity function admirable and preparation method thereof - Google Patents
Graphene combination electrode material of storing up electricity function admirable and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 69
- 239000007772 electrode material Substances 0.000 title claims abstract description 31
- 230000005611 electricity Effects 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 68
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 54
- -1 polyoxyethylene Polymers 0.000 claims abstract description 43
- 239000000463 material Substances 0.000 claims abstract description 32
- 238000002156 mixing Methods 0.000 claims abstract description 27
- 235000017858 Laurus nobilis Nutrition 0.000 claims abstract description 19
- 239000002033 PVDF binder Substances 0.000 claims abstract description 19
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 19
- 244000125380 Terminalia tomentosa Species 0.000 claims abstract description 19
- 235000005212 Terminalia tomentosa Nutrition 0.000 claims abstract description 19
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims abstract description 19
- 239000001095 magnesium carbonate Substances 0.000 claims abstract description 19
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims abstract description 19
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 18
- UWHCKJMYHZGTIT-UHFFFAOYSA-N Tetraethylene glycol, Natural products OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 claims abstract description 17
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 17
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims abstract description 17
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims abstract description 17
- 235000019864 coconut oil Nutrition 0.000 claims abstract description 17
- 239000003240 coconut oil Substances 0.000 claims abstract description 17
- 235000019837 monoammonium phosphate Nutrition 0.000 claims abstract description 17
- 239000000853 adhesive Substances 0.000 claims abstract description 14
- 230000001070 adhesive effect Effects 0.000 claims abstract description 14
- 235000013847 iso-butane Nutrition 0.000 claims abstract description 14
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 claims abstract description 14
- IJDNQMDRQITEOD-UHFFFAOYSA-N sec-butylidene Natural products CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 claims abstract description 14
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 claims abstract description 13
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical class OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 9
- 235000014380 magnesium carbonate Nutrition 0.000 claims abstract description 9
- 239000002270 dispersing agent Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 24
- 239000007921 spray Substances 0.000 claims description 24
- 238000002347 injection Methods 0.000 claims description 16
- 239000007924 injection Substances 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical group N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- 150000001336 alkenes Chemical class 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 8
- 239000000908 ammonium hydroxide Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- ZHUWIYQJHBMTCY-UHFFFAOYSA-N 3-[ethoxy(2,2,2-triethoxyethoxy)silyl]propan-1-amine Chemical compound NCCC[SiH](OCC(OCC)(OCC)OCC)OCC ZHUWIYQJHBMTCY-UHFFFAOYSA-N 0.000 claims description 6
- YUEDZVRMWQBEPT-UHFFFAOYSA-N CC1=CC=CC(C(C2=CC=CC=C2)C2=CC=CC=C2)=C1C.N=C=O.N=C=O.N=C=O.N=C=O Chemical compound CC1=CC=CC(C(C2=CC=CC=C2)C2=CC=CC=C2)=C1C.N=C=O.N=C=O.N=C=O.N=C=O YUEDZVRMWQBEPT-UHFFFAOYSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 6
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical group CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 6
- 229920002635 polyurethane Polymers 0.000 claims description 6
- 239000004814 polyurethane Substances 0.000 claims description 6
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical class CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 4
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 4
- 229920001568 phenolic resin Polymers 0.000 claims description 4
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims description 4
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- HSRJKNPTNIJEKV-UHFFFAOYSA-N Guaifenesin Chemical compound COC1=CC=CC=C1OCC(O)CO HSRJKNPTNIJEKV-UHFFFAOYSA-N 0.000 claims description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Natural products CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 238000004026 adhesive bonding Methods 0.000 claims 1
- 235000019441 ethanol Nutrition 0.000 claims 1
- 229910000077 silane Inorganic materials 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 5
- 239000011261 inert gas Substances 0.000 abstract description 3
- 238000001694 spray drying Methods 0.000 abstract description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 12
- 150000002169 ethanolamines Chemical class 0.000 description 7
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 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 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 239000001294 propane Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000005211 alkyl trimethyl ammonium group Chemical group 0.000 description 1
- 229940077388 benzenesulfonate Drugs 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- LGRFSURHDFAFJT-UHFFFAOYSA-N phthalic anhydride Chemical compound C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 1
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
Abstract
The invention discloses a kind of graphene combination electrode materials of storing up electricity function admirable, with graphene, aluminium hydroxide, magnesium carbonate, oxalic acid, ammonium dihydrogen phosphate is main component, by adding in polyvinylidene fluoride, tetraethylene glycol, polyoxyethylene laurel ether, tricarboxylic methylpropane glycidol ether, coconut oil, phthalate anhydride, triethanolamine salt, dispersant, silane coupling agent, adhesive, it is aided with ultrasonic disperse, stir mixing, inert gas environment is kneaded, spray drying, the techniques such as material is electrode coated, so that the graphene combination electrode material of storing up electricity function admirable being prepared, its dependable performance, electric conductivity is excellent, store up good electrical property, it is environmentally safe, it disclosure satisfy that the requirement of industry, with preferable application prospect.
Description
Technical field
The present invention relates to electrode material technical field, more particularly to a kind of graphene combination electrode material of storing up electricity function admirable
Material and preparation method thereof.
Background technology
2004, Univ Manchester UK physicist An Deliegaimu and Constantine's Nuo Woxiao loves, into
Work(isolates graphene from graphite, it was demonstrated that therefore it can also obtain 2010 years Nobel's physics jointly with individualism, two people
Learn prize.Before the discovery of 2015 year end boron alkene, graphene is both most thin material and most tough material, fracture strength ratio
Taller 200 times of best steel.It has good elasticity again simultaneously, and stretch range can reach the 20% of own dimensions.Graphene
It is that current nature is most thin, the highest material of intensity, most potential application is the substitute as silicon, manufactures superminiature crystal
Pipe, for producing following supercomputer.Replace silicon with graphene, the speed of service of computer processor will be hundreds of soon
Times.In addition, graphene is almost fully transparent, 2.3% light is only absorbed.On the other hand, it is very fine and close, even minimum
Gas atom（Hydrogen atom）Also it can not penetrate.These features cause it to be highly suitable as the raw material of transparent electron product, such as
Transparent touch display screen, luminescent screen and solar panel.As presently found most thin, maximum intensity, electrical and thermal conductivity
A kind of novel nano-material that can be most strong, graphene is referred to as " dark fund ", is " king of new material ", scientist even foretells graphite
Alkene " will thoroughly change 21 century ".Very likely start a subversiveness new technology new industrial revolution have swept the globe.So this
Project is intended to develop the graphene combination electrode material of a storing up electricity function admirable, using the excellent electrochemical properties of graphene
To meet the needs of electrode material industry and development.
Invention content
In order to solve the above technical problems, the present invention provide a kind of storing up electricity function admirable graphene combination electrode material and its
Preparation method is combined by using specified raw material, coordinates corresponding production technology, the obtained graphite of storing up electricity function admirable
Alkene combination electrode material, dependable performance, electric conductivity is excellent, storage good electrical property, environmentally safe, disclosure satisfy that industry
It is required that with preferable application prospect.
The purpose of the present invention can be achieved through the following technical solutions：
The graphene combination electrode material of storing up electricity function admirable, is made from the following raw materials in parts by weight：Graphene 30-45
Part, 3-6 parts of polyvinylidene fluoride, 5-10 parts of tetraethylene glycol, 2-5 parts of polyoxyethylene laurel ether, tricarboxylic methylpropane glycidol ether
2-5 parts, 3-6 parts of coconut oil, 1-4 parts of phthalate anhydride, 4-7 parts of triethanolamine salt, 3-9 parts of aluminium hydroxide, 4-9 parts of magnesium carbonate,
2-5 parts of oxalic acid, 1-2 parts of ammonium dihydrogen phosphate, 4-7 parts of dispersant, 3-6 parts of silane coupling agent, 3-8 parts of adhesive.
Preferably, the dispersant is selected from n-methyl-2-pyrrolidone, cetyl trimethylammonium bromide, dodecyl
One or more of benzene sulfonic acid sodium salt, sodium lignin sulfonate.
Preferably, the silane coupling agent is selected from vinyltriethoxysilane, 3- aminopropyl trimethoxysilanes, 3- contractings
One or more of water glycerin ether oxygroup propyl trimethoxy silicane, γ-aminopropyltriethoxy diethoxy silane.
Preferably, the adhesive be selected from dimethyl triphenyl methane tetraisocyanate, sodium carboxymethylcellulose, butyronitrile-
One or more of phenolic resin, polyurethane adhesive.
The preparation method of the graphene combination electrode material of the storing up electricity function admirable, includes the following steps：
（1）Each raw material is weighed according to parts by weight；
（2）Graphene is added in the concentrated sulfuric acid and is aoxidized, obtains graphite oxide alkenes material, and by ultrasonic disperse in dispersion
In agent, while add in polyvinylidene fluoride, tetraethylene glycol, polyoxyethylene laurel ether, tricarboxylic methylpropane glycidol ether, coconut
Oil, phthalate anhydride, obtain graphene suspension, ultrasonic power 300-500W, and ultrasonic time is 3-6 hours；
（3）Aluminium hydroxide, magnesium carbonate, oxalic acid, ammonium dihydrogen phosphate are added in blender, stirred evenly, speed of agitator
200-400 revs/min, pH value is adjusted between 2.5-3 with the ammonium hydroxide of 0.2mol/L under stirring, mixing time 30-
45 minutes；
（4）By step（2）Graphene oxide composite material and step（3）Stirring mixture input mixer in, add in three
Ethanolamine salt, silane coupling agent, adhesive are kneaded 1-3 hours, 250-350 revs/min of rotating speed in reducibility gas atmosphere,
Reaction temperature is 560-620 DEG C, is subsequently cooled to 120 DEG C, obtains mixing mixture；
（5）By above-mentioned mixing mixture spray injection drying machine, powder is dried to, spray dryer inlet air temperature is 220 DEG C,
160 DEG C of leaving air temp, it is 84 revs/min that constant flow pump, which turns degree,；
（6）In the material injection Muffle furnace that spray dryer is sprayed, it is coated uniformly on treated electrode, Muffle
520 DEG C of stove preset temperature is cooled to 380 DEG C after adding in material, is forced into 1-2Mpa, while is slowly filled with reducibility gas guarantor
Shield, coats later finished product and 3-5 hours is kept the temperature in reducibility gas, be down to room temperature and get product.
Preferably, the step（4）And step（6）In, reducibility gas atmosphere is nitrogen gas atmosphere.
Compared with prior art, the present invention advantage is：
（1）The present invention storing up electricity function admirable graphene combination electrode material with graphene, aluminium hydroxide, magnesium carbonate,
Oxalic acid, ammonium dihydrogen phosphate are main component, by adding in polyvinylidene fluoride, tetraethylene glycol, polyoxyethylene laurel ether, three carboxymethyls
Propane glycidol ether, coconut oil, phthalate anhydride, triethanolamine salt, dispersant, silane coupling agent, adhesive, are aided with ultrasound
The techniques such as dispersion, stirring mixing, inert gas environment are kneaded, spray drying, material is electrode coated so that the storing up electricity being prepared
The graphene combination electrode material of function admirable, dependable performance, electric conductivity is excellent, storage good electrical property, environmentally safe,
It disclosure satisfy that the requirement of industry, there is preferable application prospect.
（2）The graphene combination electrode material raw material of the storing up electricity function admirable of the present invention is easy to get, is simple for process, suitable for advising greatly
Mould industrialization is used, highly practical.
Specific embodiment
The technical solution of invention is described in detail with reference to specific embodiment.
Embodiment 1
（1）30 parts of graphene, 3 parts of polyvinylidene fluoride, 5 parts of tetraethylene glycol, polyoxyethylene laurel ether 2 are weighed according to parts by weight
Part, 2 parts of tricarboxylic methylpropane glycidol ether, 3 parts of coconut oil, 1 part of phthalate anhydride, 4 parts of triethanolamine salt, aluminium hydroxide 3
Part, 4 parts of magnesium carbonate, 2 parts of oxalic acid, 1 part of ammonium dihydrogen phosphate, 4 parts of n-methyl-2-pyrrolidone, vinyltriethoxysilane 3
Part, 3 parts of dimethyl triphenyl methane tetraisocyanate；
（2）Graphene is added in the concentrated sulfuric acid and is aoxidized, obtains graphite oxide alkenes material, and by ultrasonic disperse in N- first
In base -2-Pyrrolidone, at the same add in polyvinylidene fluoride, tetraethylene glycol, polyoxyethylene laurel ether, tricarboxylic methylpropane shrink it is sweet
Oily ether, coconut oil, phthalate anhydride, obtain graphene suspension, ultrasonic power 300W, and ultrasonic time is 3 hours；
（3）Aluminium hydroxide, magnesium carbonate, oxalic acid, ammonium dihydrogen phosphate are added in blender, stirred evenly, speed of agitator 200
Rev/min, between the ammonium hydroxide of 0.2mol/L adjusting pH value to 2.5 under stirring, mixing time is 30 minutes；
（4）By step（2）Graphene oxide composite material and step（3）Stirring mixture input mixer in, add in three
Ethanolamine salt, vinyltriethoxysilane, dimethyl triphenyl methane tetraisocyanate are kneaded 1 hour in nitrogen atmosphere,
250 revs/min of rotating speed, reaction temperature are 560 DEG C, are subsequently cooled to 120 DEG C, obtain mixing mixture；
（5）By above-mentioned mixing mixture spray injection drying machine, powder is dried to, spray dryer inlet air temperature is 220 DEG C,
160 DEG C of leaving air temp, it is 84 revs/min that constant flow pump, which turns degree,；
（6）In the material injection Muffle furnace that spray dryer is sprayed, it is coated uniformly on treated electrode, Muffle
520 DEG C of stove preset temperature is cooled to 380 DEG C after adding in material, is forced into 1Mpa, while is slowly filled with nitrogen protection, apply coated with
Finished product afterwards keeps the temperature 3 hours in nitrogen atmosphere, is down to room temperature and gets product.
The graphene combination electrode material test result of storing up electricity function admirable obtained is as shown in table 1.
Embodiment 2
（1）35 parts of graphene, 4 parts of polyvinylidene fluoride, 7 parts of tetraethylene glycol, polyoxyethylene laurel ether 3 are weighed according to parts by weight
Part, 3 parts of tricarboxylic methylpropane glycidol ether, 4 parts of coconut oil, 2 parts of phthalate anhydride, 5 parts of triethanolamine salt, aluminium hydroxide 5
Part, 6 parts of magnesium carbonate, 3 parts of oxalic acid, 1 part of ammonium dihydrogen phosphate, 5 parts of cetyl trimethylammonium bromide, 3- aminopropyl trimethoxy silicon
4 parts of alkane, 6 parts of sodium carboxymethylcellulose；
（2）Graphene is added in the concentrated sulfuric acid and is aoxidized, obtains graphite oxide alkenes material, and by ultrasonic disperse in 16
In alkyl trimethyl ammonium bromide, while add in polyvinylidene fluoride, tetraethylene glycol, polyoxyethylene laurel ether, the contracting of tricarboxylic methylpropane
Water glycerin ether, coconut oil, phthalate anhydride, obtain graphene suspension, ultrasonic power 350W, and ultrasonic time is 4 hours；
（3）Aluminium hydroxide, magnesium carbonate, oxalic acid, ammonium dihydrogen phosphate are added in blender, stirred evenly, speed of agitator 250
Rev/min, between the ammonium hydroxide of 0.2mol/L adjusting pH value to 2.7 under stirring, mixing time is 35 minutes；
（4）By step（2）Graphene oxide composite material and step（3）Stirring mixture input mixer in, add in three
Ethanolamine salt, 3- aminopropyl trimethoxysilanes, sodium carboxymethylcellulose are kneaded 1.5 hours, rotating speed 280 in nitrogen atmosphere
Rev/min, reaction temperature is 580 DEG C, is subsequently cooled to 120 DEG C, obtains mixing mixture；
（5）By above-mentioned mixing mixture spray injection drying machine, powder is dried to, spray dryer inlet air temperature is 220 DEG C,
160 DEG C of leaving air temp, it is 84 revs/min that constant flow pump, which turns degree,；
（6）In the material injection Muffle furnace that spray dryer is sprayed, it is coated uniformly on treated electrode, Muffle
520 DEG C of stove preset temperature is cooled to 380 DEG C after adding in material, is forced into 1.3Mpa, while is slowly filled with nitrogen protection, coating
Later finished product keeps the temperature 3.5 hours in nitrogen atmosphere, is down to room temperature and gets product.
The graphene combination electrode material test result of storing up electricity function admirable obtained is as shown in table 1.
Embodiment 3
（1）40 parts of graphene, 5 parts of polyvinylidene fluoride, 9 parts of tetraethylene glycol, polyoxyethylene laurel ether 4 are weighed according to parts by weight
Part, 4 parts of tricarboxylic methylpropane glycidol ether, 5 parts of coconut oil, 3 parts of phthalate anhydride, 6 parts of triethanolamine salt, aluminium hydroxide 8
Part, 8 parts of magnesium carbonate, 4 parts of oxalic acid, 2 parts of ammonium dihydrogen phosphate, 6 parts of neopelex, 3- glycydoxies three
5 parts of methoxy silane, 7 parts of butyronitrile-phenolic resin；
（2）Graphene is added in the concentrated sulfuric acid and is aoxidized, obtains graphite oxide alkenes material, and by ultrasonic disperse in 12
In sodium alkyl benzene sulfonate, at the same add in polyvinylidene fluoride, tetraethylene glycol, polyoxyethylene laurel ether, tricarboxylic methylpropane shrink it is sweet
Oily ether, coconut oil, phthalate anhydride, obtain graphene suspension, ultrasonic power 450W, and ultrasonic time is 5 hours；
（3）Aluminium hydroxide, magnesium carbonate, oxalic acid, ammonium dihydrogen phosphate are added in blender, stirred evenly, speed of agitator 350
Rev/min, between the ammonium hydroxide of 0.2mol/L adjusting pH value to 2.9 under stirring, mixing time is 40 minutes；
（4）By step（2）Graphene oxide composite material and step（3）Stirring mixture input mixer in, add in three
It is small to be kneaded 2.5 in nitrogen atmosphere for ethanolamine salt, 3- glycydoxies trimethoxy silane, butyronitrile-phenolic resin
When, 310 revs/min of rotating speed, reaction temperature is 600 DEG C, is subsequently cooled to 120 DEG C, obtains mixing mixture；
（5）By above-mentioned mixing mixture spray injection drying machine, powder is dried to, spray dryer inlet air temperature is 220 DEG C,
160 DEG C of leaving air temp, it is 84 revs/min that constant flow pump, which turns degree,；
（6）In the material injection Muffle furnace that spray dryer is sprayed, it is coated uniformly on treated electrode, Muffle
520 DEG C of stove preset temperature is cooled to 380 DEG C after adding in material, is forced into 1.7Mpa, while is slowly filled with nitrogen protection, coating
Later finished product keeps the temperature 4.5 hours in nitrogen atmosphere, is down to room temperature and gets product.
The graphene combination electrode material test result of storing up electricity function admirable obtained is as shown in table 1.
Embodiment 4
（1）45 parts of graphene, 6 parts of polyvinylidene fluoride, 10 parts of tetraethylene glycol, polyoxyethylene laurel ether are weighed according to parts by weight
5 parts, 5 parts of tricarboxylic methylpropane glycidol ether, 6 parts of coconut oil, 4 parts of phthalate anhydride, 7 parts of triethanolamine salt, aluminium hydroxide 9
Part, 9 parts of magnesium carbonate, 5 parts of oxalic acid, 2 parts of ammonium dihydrogen phosphate, 7 parts of sodium lignin sulfonate, γ-aminopropyltriethoxy diethoxy silane 6
Part, 8 parts of polyurethane adhesive；
（2）Graphene is added in the concentrated sulfuric acid and is aoxidized, obtains graphite oxide alkenes material, and by ultrasonic disperse in wooden
In plain sodium sulfonate, at the same add in polyvinylidene fluoride, tetraethylene glycol, polyoxyethylene laurel ether, tricarboxylic methylpropane glycidol ether,
Coconut oil, phthalate anhydride, obtain graphene suspension, ultrasonic power 500W, and ultrasonic time is 6 hours；
（3）Aluminium hydroxide, magnesium carbonate, oxalic acid, ammonium dihydrogen phosphate are added in blender, stirred evenly, speed of agitator 400
Rev/min, between the ammonium hydroxide of 0.2mol/L adjusting pH value to 3 under stirring, mixing time is 45 minutes；
（4）By step（2）Graphene oxide composite material and step（3）Stirring mixture input mixer in, add in three
Ethanolamine salt, γ-aminopropyltriethoxy diethoxy silane, polyurethane adhesive are kneaded 3 hours in nitrogen atmosphere, and 350 turns of rotating speed/
Minute, reaction temperature is 620 DEG C, is subsequently cooled to 120 DEG C, obtains mixing mixture；
（5）By above-mentioned mixing mixture spray injection drying machine, powder is dried to, spray dryer inlet air temperature is 220 DEG C,
160 DEG C of leaving air temp, it is 84 revs/min that constant flow pump, which turns degree,；
（6）In the material injection Muffle furnace that spray dryer is sprayed, it is coated uniformly on treated electrode, Muffle
520 DEG C of stove preset temperature is cooled to 380 DEG C after adding in material, is forced into 2Mpa, while is slowly filled with nitrogen protection, apply coated with
Finished product afterwards keeps the temperature 5 hours in nitrogen atmosphere, is down to room temperature and gets product.
The graphene combination electrode material test result of storing up electricity function admirable obtained is as shown in table 1.
Comparative example 1
（1）30 parts of graphene, 3 parts of polyvinylidene fluoride, 2 parts of polyoxyethylene laurel ether, tricarboxylic first are weighed according to parts by weight
2 parts of base propane glycidol ether, 1 part of phthalate anhydride, 4 parts of triethanolamine salt, 4 parts of magnesium carbonate, 2 parts of oxalic acid, ammonium dihydrogen phosphate 1
Part, 4 parts of n-methyl-2-pyrrolidone, 3 parts of vinyltriethoxysilane, 3 parts of dimethyl triphenyl methane tetraisocyanate；
（2）Graphene is added in the concentrated sulfuric acid and is aoxidized, obtains graphite oxide alkenes material, and by ultrasonic disperse in N- first
In base -2-Pyrrolidone, while add in polyvinylidene fluoride, polyoxyethylene laurel ether, tricarboxylic methylpropane glycidol ether, benzene
Dicarboxylic acid anhydride, obtains graphene suspension, ultrasonic power 300W, and ultrasonic time is 3 hours；
（3）Magnesium carbonate, oxalic acid, ammonium dihydrogen phosphate are added in blender, stirred evenly, 200 revs/min of speed of agitator,
With between the ammonium hydroxide of 0.2mol/L adjusting pH value to 2.5 under stirring, mixing time is 30 minutes；
（4）By step（2）Graphene oxide composite material and step（3）Stirring mixture input mixer in, add in three
Ethanolamine salt, vinyltriethoxysilane, dimethyl triphenyl methane tetraisocyanate are kneaded 1 hour in nitrogen atmosphere,
250 revs/min of rotating speed, reaction temperature are 560 DEG C, are subsequently cooled to 120 DEG C, obtain mixing mixture；
（5）By above-mentioned mixing mixture spray injection drying machine, powder is dried to, spray dryer inlet air temperature is 220 DEG C,
160 DEG C of leaving air temp, it is 84 revs/min that constant flow pump, which turns degree,；
（6）In the material injection Muffle furnace that spray dryer is sprayed, it is coated uniformly on treated electrode, Muffle
520 DEG C of stove preset temperature is cooled to 380 DEG C after adding in material, is forced into 1Mpa, while is slowly filled with nitrogen protection, apply coated with
Finished product afterwards keeps the temperature 3 hours in nitrogen atmosphere, is down to room temperature and gets product.
The graphene combination electrode material test result of storing up electricity function admirable obtained is as shown in table 1.
Comparative example 2
（1）45 parts of graphene, 6 parts of polyvinylidene fluoride, 10 parts of tetraethylene glycol, polyoxyethylene laurel ether are weighed according to parts by weight
5 parts, it is 6 parts of coconut oil, 4 parts of phthalate anhydride, 7 parts of triethanolamine salt, 9 parts of aluminium hydroxide, 9 parts of magnesium carbonate, 5 parts of oxalic acid, wooden
Plain 7 parts of sodium sulfonate, γ -6 parts of aminopropyltriethoxy diethoxy silane, 8 parts of polyurethane adhesive；
（2）Graphene is added in the concentrated sulfuric acid and is aoxidized, obtains graphite oxide alkenes material, and by ultrasonic disperse in wooden
In plain sodium sulfonate, while polyvinylidene fluoride, tetraethylene glycol, polyoxyethylene laurel ether, coconut oil, phthalate anhydride are added in, obtained
Graphene suspension, ultrasonic power 500W, ultrasonic time are 6 hours；
（3）Aluminium hydroxide, magnesium carbonate, oxalic acid are added in blender, stirred evenly, 400 revs/min of speed of agitator,
With between the ammonium hydroxide of 0.2mol/L adjusting pH value to 3 under stirring, mixing time is 45 minutes；
（4）By step（2）Graphene oxide composite material and step（3）Stirring mixture input mixer in, add in three
Ethanolamine salt, γ-aminopropyltriethoxy diethoxy silane, polyurethane adhesive are kneaded 3 hours in nitrogen atmosphere, and 350 turns of rotating speed/
Minute, reaction temperature is 620 DEG C, is subsequently cooled to 120 DEG C, obtains mixing mixture；
（5）By above-mentioned mixing mixture spray injection drying machine, powder is dried to, spray dryer inlet air temperature is 220 DEG C,
160 DEG C of leaving air temp, it is 84 revs/min that constant flow pump, which turns degree,；
（6）In the material injection Muffle furnace that spray dryer is sprayed, it is coated uniformly on treated electrode, Muffle
520 DEG C of stove preset temperature is cooled to 380 DEG C after adding in material, is forced into 2Mpa, while is slowly filled with nitrogen protection, apply coated with
Finished product afterwards keeps the temperature 5 hours in nitrogen atmosphere, is down to room temperature and gets product.
The graphene combination electrode material test result of storing up electricity function admirable obtained is as shown in table 1.
The graphene combination electrode material of the storing up electricity function admirable of embodiment 1-4 and comparative example 1-2 is discharged respectively
This several specific capacity, internal resistance, specific capacitance, circulation volume conservation rate performance tests.
Table 1
The graphene combination electrode material of the storing up electricity function admirable of the present invention is with graphene, aluminium hydroxide, magnesium carbonate, grass
Acid, ammonium dihydrogen phosphate are main component, by adding in polyvinylidene fluoride, tetraethylene glycol, polyoxyethylene laurel ether, tricarboxylic methyl-prop
Alkane glycidol ether, coconut oil, phthalate anhydride, triethanolamine salt, dispersant, silane coupling agent, adhesive are aided with ultrasound point
It dissipates, the techniques such as stirring mixing, inert gas environment are kneaded, spray drying, material is electrode coated so that the storing up electricity being prepared
The excellent graphene combination electrode material of energy, dependable performance, electric conductivity is excellent, storage good electrical property, environmentally safe, energy
Enough meet the requirement of industry, there is preferable application prospect.The graphene combination electrode material of the storing up electricity function admirable of the present invention
Raw material is easy to get, is simple for process, is used suitable for heavy industrialization, highly practical.
The foregoing is merely the embodiment of the present invention, are not intended to limit the scope of the invention, every to utilize this hair
The equivalent structure or equivalent flow shift that bright description is made directly or indirectly is used in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (6)
1. the graphene combination electrode material of storing up electricity function admirable, it is characterised in that：It is made from the following raw materials in parts by weight：Graphite
30-45 parts of alkene, 3-6 parts of polyvinylidene fluoride, 5-10 parts of tetraethylene glycol, 2-5 parts of polyoxyethylene laurel ether, tricarboxylic methylpropane shrink
2-5 parts of glycerin ether, 3-6 parts of coconut oil, 1-4 parts of phthalate anhydride, 4-7 parts of triethanolamine salt, 3-9 parts of aluminium hydroxide, magnesium carbonate
4-9 parts, 2-5 parts of oxalic acid, 1-2 parts of ammonium dihydrogen phosphate, 4-7 parts of dispersant, 3-6 parts of silane coupling agent, 3-8 parts of adhesive.
2. the graphene combination electrode material of storing up electricity function admirable according to claim 1, it is characterised in that：The dispersion
Agent is in n-methyl-2-pyrrolidone, cetyl trimethylammonium bromide, neopelex, sodium lignin sulfonate
One or more.
3. the graphene combination electrode material of storing up electricity function admirable according to claim 1, it is characterised in that：The silane
Coupling agent is selected from vinyltriethoxysilane, 3- aminopropyl trimethoxysilanes, 3- glycydoxy trimethoxies
One or more of base silane, γ-aminopropyltriethoxy diethoxy silane.
4. the graphene combination electrode material of storing up electricity function admirable according to claim 1, it is characterised in that：The gluing
Agent in dimethyl triphenyl methane tetraisocyanate, sodium carboxymethylcellulose, butyronitrile-phenolic resin, polyurethane adhesive one
Kind is several.
5. according to the preparation method of the graphene combination electrode material of any storing up electricity function admirable of Claims 1 to 4,
It is characterized in that, includes the following steps：
（1）Each raw material is weighed according to parts by weight；
（2）Graphene is added in the concentrated sulfuric acid and is aoxidized, obtains graphite oxide alkenes material, and by ultrasonic disperse in dispersant
In, at the same add in polyvinylidene fluoride, tetraethylene glycol, polyoxyethylene laurel ether, tricarboxylic methylpropane glycidol ether, coconut oil,
Phthalate anhydride, obtains graphene suspension, ultrasonic power 300-500W, and ultrasonic time is 3-6 hours；
（3）Aluminium hydroxide, magnesium carbonate, oxalic acid, ammonium dihydrogen phosphate are added in blender, stirred evenly, speed of agitator 200-400
Rev/min, pH value is adjusted between 2.5-3 with the ammonium hydroxide of 0.2mol/L under stirring, and mixing time is 30-45 minutes；
（4）By step（2）Graphene oxide composite material and step（3）Stirring mixture input mixer in, add in three ethyl alcohol
Amine salt, silane coupling agent, adhesive are kneaded 1-3 hours, 250-350 revs/min of rotating speed in reducibility gas atmosphere, reaction
Temperature is 560-620 DEG C, is subsequently cooled to 120 DEG C, obtains mixing mixture；
（5）By above-mentioned mixing mixture spray injection drying machine, powder is dried to, spray dryer inlet air temperature is 220 DEG C, outlet air
160 DEG C of temperature, it is 84 revs/min that constant flow pump, which turns degree,；
（6）In the material injection Muffle furnace that spray dryer is sprayed, it is coated uniformly on treated electrode, Muffle furnace is pre-
If 520 DEG C of temperature, 380 DEG C are cooled to after adding in material, is forced into 1-2Mpa, while is slowly filled with reducibility gas protection, is applied
Finished product after keeps the temperature 3-5 hours in reducibility gas, is down to room temperature and gets product.
6. the graphene combination electrode material of storing up electricity function admirable according to claim 5, which is characterized in that the step
（4）And step（6）In, reducibility gas atmosphere is nitrogen gas atmosphere.
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