CN107611392A - A kind of graphene composite material for improving lithium polymer battery mechanical strength - Google Patents
A kind of graphene composite material for improving lithium polymer battery mechanical strength Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 94
- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 229920000642 polymer Polymers 0.000 title claims abstract description 37
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 claims abstract description 18
- 150000004985 diamines Chemical class 0.000 claims abstract description 17
- 230000009467 reduction Effects 0.000 claims abstract description 13
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 24
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 23
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 22
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 22
- 238000006243 chemical reaction Methods 0.000 claims description 21
- UHOVQNZJYSORNB-UHFFFAOYSA-N monobenzene Natural products C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 20
- 229910000851 Alloy steel Inorganic materials 0.000 claims description 18
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 229910001339 C alloy Inorganic materials 0.000 claims description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 13
- 239000006004 Quartz sand Substances 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 13
- 239000004411 aluminium Substances 0.000 claims description 13
- 229910052782 aluminium Inorganic materials 0.000 claims description 13
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 13
- 239000010949 copper Substances 0.000 claims description 13
- 229910052802 copper Inorganic materials 0.000 claims description 13
- QMQXDJATSGGYDR-UHFFFAOYSA-N methylidyneiron Chemical compound [C].[Fe] QMQXDJATSGGYDR-UHFFFAOYSA-N 0.000 claims description 13
- 239000002006 petroleum coke Substances 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 239000004317 sodium nitrate Substances 0.000 claims description 12
- 235000010344 sodium nitrate Nutrition 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- -1 benzene alkene Chemical class 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- 150000001336 alkenes Chemical class 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 9
- 229910000037 hydrogen sulfide Inorganic materials 0.000 claims description 9
- 239000004575 stone Substances 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 150000005208 1,4-dihydroxybenzenes Chemical class 0.000 claims description 7
- 229930185605 Bisphenol Natural products 0.000 claims description 7
- KKDBZWZRJNRBGA-UHFFFAOYSA-L Cl[Ti]Cl.[CH]1C=CC=C1 Chemical compound Cl[Ti]Cl.[CH]1C=CC=C1 KKDBZWZRJNRBGA-UHFFFAOYSA-L 0.000 claims description 7
- 239000004593 Epoxy Substances 0.000 claims description 7
- 229920001577 copolymer Polymers 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 150000001412 amines Chemical class 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 5
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 5
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 5
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 5
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 5
- 125000003963 dichloro group Chemical group Cl* 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 5
- 239000004615 ingredient Substances 0.000 claims description 5
- 239000004571 lime Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- 239000003643 water by type Substances 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 229910052739 hydrogen Inorganic materials 0.000 claims description 3
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 3
- 229910052710 silicon Inorganic materials 0.000 claims description 3
- 239000010703 silicon Substances 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 2
- 239000005864 Sulphur Substances 0.000 claims description 2
- 239000012153 distilled water Substances 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims 1
- 238000003763 carbonization Methods 0.000 claims 1
- 229910001882 dioxygen Inorganic materials 0.000 claims 1
- 230000032683 aging Effects 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 9
- 229910002804 graphite Inorganic materials 0.000 description 6
- 239000010439 graphite Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229910017704 MH-Ni Inorganic materials 0.000 description 1
- 229910017739 MH—Ni Inorganic materials 0.000 description 1
- 229910018502 Ni—H Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000003698 tetramethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
- Primary Cells (AREA)
Abstract
The invention discloses a kind of graphene composite material for improving lithium polymer battery mechanical strength, it is prepared by following steps：（1）Selection；（2）Diamine POSS preparation；（3）The preparation of graphene oxide；（4）The reduction of graphene oxide；（5）The preparation of graphene composite material.The present invention can effectively improve lithium polymer battery mechanical strength, with excellent superconductivity energy, the performance such as mechanical property and heat resistance, it will not be weakened using rear ionic conductivity and electrochemical stability for a long time, lithium polymer battery after a long time use will not aging, increase life-span of battery charging and discharging.
Description
Technical field
The present invention relates to carbon material technical field, more particularly to a kind of graphene for improving lithium polymer battery mechanical strength
Composite.
Background technology
Graphene (Graphene) is the only one layer of atomic thickness for being stripped out from graphite material, being made up of carbon atom
Two dimensional crystal.2004, Univ Manchester UK physicist An Deliegaimu and Constantine's Nuo Woxiao loves,
Graphene is isolated in success from graphite, it was demonstrated that therefore it can also obtain Nobel's thing in 2010 jointly with individualism, two people
Neo-Confucianism prize.Graphene is both most thin material, and most tough material, 200 times more taller than best steel of fracture strength.
It has good elasticity again simultaneously, and stretch range can reach the 20% of own dimensions.It is that current nature is most thin, intensity highest
Material, if making hammock with the graphene of one piece of 1 square metre of area, weight itself can be to bear one less than 1 milligram
One kilogram of cat.Graphene most potential application at present is the substitute as silicon, ultra micro transistor npn npn is manufactured, for producing
Following supercomputer.Substitute silicon with graphene, the speed of service of computer processor will be fast hundreds times.In addition, graphite
Alkene is almost fully transparent, only absorbs 2.3% light.On the other hand, it is very fine and close, even minimum gas atom (helium
Atom) it can not also penetrate.These features cause it to be highly suitable as the raw material of transparent electron product, and such as transparent touch is shown
Screen, luminescent screen and solar panel.
A kind of novel nano-material most strong as the most thin, maximum intensity, electrical and thermal conductivity performance that have now been found that, graphene
It is referred to as " dark fund ", is " king of new material ", scientist even foretells that graphene " will thoroughly change 21 century ".Very likely lift
Play a subversiveness new technology new industrial revolution have swept the globe.
After Pu Lai get in 1859 trial-produces chemical conversion formula lead-acid accumulator successfully, electrochmical power source enters people's bud.
In the evolution of more than 100 years, the electrochmical power source of new range is continuously emerged, and the performance of electrochmical power source is constantly improved.Especially
It is that the development of electrochmical power source is rapider after World War II.Cd-Ni batteries, production the 1980s are generated later
MH-Ni batteries have been given birth to, by the exploration of nearly 20 years, have developed lithium ion battery and lighium polymer in early 1990s finally
Battery, their development have also been arrived i.e. by the stage of commercialization, and at present, lithium ion battery is with its high specific energy density and service life
Grow and be taken seriously, quickly grow, lithium polymer battery is also given priority in the countries and regions such as the U.S., Japan and Taiwan.Lithium gathers
The development of compound battery is swift and violent, progressively substitutes cadmium nickel and Ni-H cell, makees grinding for electrode and electrolyte using polymer
It is particularly noticeable to study carefully exploitation.But the ionic conductivity and mechanical strength of current lithium polymer battery are poor, manufacturing process
Complexity, battery volume is larger, and battery capacity is inadequate, because positive active material and negative electrode active material easily come off, for a long time
Poor using rear ionic conductivity and electrochemical stability, isolating film strength and stability can also become with the use of battery
Change, it is easy to cause lithium polymer battery aging after a long time use, the life-span of discharge and recharge is very restricted.
The invention provides a kind of graphene composite material for improving lithium polymer battery mechanical strength.
The content of the invention
The technical problems to be solved by the invention are：Provide a kind of graphite for improving lithium polymer battery mechanical strength
Alkene composite.
To be answered in order to solve the above technical problems, the invention provides a kind of graphene for improving lithium polymer battery mechanical strength
Condensation material, comprise the following steps：
（1）Selection:Component composition including following parts by weight：The parts by weight of graphene 50, diamine POSS 11-13 parts by weight, close
Golden steel 1-3 parts by weight, concentrated sulfuric acid 35-55 parts by weight, benzene alkene nitrile-St copolymer 4-10 parts by weight, bisphenol epoxies tree
Fat 20-26 parts by weight, carborundum 4-6 parts by weight, sodium nitrate 15-25 parts by weight, hydroxyethyl cellulose 4-8 parts by weight, tetramethyl
Ammonium hydroxide 3-7 parts by weight, nano-zinc oxide powder 4-6 parts by weight, hydrogen sulfide 5-9 parts by weight, hydroquinones 1-5 parts by weight,
Deionized water 55-65 parts by weight, 5% hydrogen peroxide 30-40 parts by weight, absolute ethyl alcohol 60-70 parts by weight, cyclopentadienyl titanium dichloride 10-12
Parts by weight；Wherein, the steel alloy includes iron-carbon alloy, aluminium, copper and mickel；The carborundum includes quartz sand, petroleum coke and not
Sang Shi；
（2）Diamine POSS preparation：Added successively into 500mL three-necked flask 500mL toluene, 75mL deionized waters and
8gTEAOH, magnetic agitation 60min, 15mLAPS and 26mLPTES mixed liquor is then added dropwise, is obtained after being heated to reflux 48h
Transparency liquid, continue to heat 50min volatilization toluene, obtain lime milky product, washed with the mixed solution of tetrahydrofuran and methanol
Product is washed, is freezed under vacuum condition and obtains product diamine POSS；
（3）The preparation of graphene oxide：A, according to step（1）In each parts by weight of raw materials weigh graphite powder keep bath temperature be
The concentrated sulfuric acid is added under 15-25 DEG C of condition of ice bath as solvent, is stirred after 30-40min and is slowly added to sodium nitrate, sulphur successively
Change hydrogen, stir 20-30min；45-55 DEG C, stirring reaction 2-3h is warming up to, 95 DEG C is then heated to and adds deionized water and eight benzene
Base POSS, 30-40min is stirred, stop reaction, add 5% hydrogen peroxide, centrifuged while hot, respectively with appropriate 5% watery hydrochloric acid and distilled water
Washing, graphene oxide first product is made；
B, by graphene oxide first product made from above-mentioned steps a with and carborundum be stirred, adsorbed, be made oxidation stone
Black alkene；
（4）The reduction of graphene oxide：By step（3）After obtained graphene oxide mixes with Nano-Zinc powder, according to heating
Speed is that to be heated to temperature be 950-1050 DEG C to 15-20 DEG C/min, and constant temperature adds TMAH and keeps 24-26h, obtains
Graphene oxide after to reduction；
（5）The preparation of graphene composite material：A, by step（4）Graphene oxide graphene oxide and two after obtained reduction
It is scattered in after first amine POSS mixing using ultrasonic wave in appropriate absolute ethyl alcohol, after stirring, is warming up to 50 DEG C of addition dichloros
Titanocenes, after stirring 25min, solution is transferred in reactor, argon gas is passed through as protection hermetic seal, in 200 DEG C of reactions
48h, stop reaction, after product is filtered, with distillation water washing, freeze under vacuum, at the beginning of obtaining graphene composite material
Product；
B, graphene composite material first product and step（1）In remaining ingredient be placed in mixer, it is 160-170 to control temperature
DEG C, mixed on low speed 8-12min, 190-195 DEG C is then heated to, mixed at high speed 8-10min, obtains compound；Compound is put
In dryer, drying temperature is 105 DEG C, drying time 2-2.6h, and the stone for improving lithium polymer battery mechanical strength is made
Black alkene composite.
Further, the step（1）Selection:Component composition including following parts by weight：The parts by weight of graphene 50, binary
The parts by weight of amine POSS 12, the parts by weight of steel alloy 2, the parts by weight of the concentrated sulfuric acid 45, benzene alkene nitrile-parts by weight of St copolymer 7,
The parts by weight of bisphenol epoxy 23, the parts by weight of carborundum 5, the parts by weight of sodium nitrate 20, the parts by weight of hydroxyethyl cellulose 6, tetramethyl
The parts by weight of ammonium hydroxide 5, the parts by weight of nano-zinc oxide powder 5, the parts by weight of hydrogen sulfide 7, the parts by weight of hydroquinones 3, deionized water
60 parts by weight, 5% parts by weight of hydrogen peroxide 35, the parts by weight of absolute ethyl alcohol 65, the parts by weight of cyclopentadienyl titanium dichloride 11.
Further, the step（1）Described in steel alloy each component mass ratio for iron-carbon alloy 30%, aluminium 10%, copper
35%th, nickel 25%；The mass ratio of the carborundum each component is quartz sand 55%, not petroleum coke 15%, Sang Shi 30%.
Beneficial effects of the present invention：The present invention provides a kind of graphene composite wood for improving lithium polymer battery mechanical strength
Material, can effectively improve lithium polymer battery mechanical strength, have excellent superconductivity energy, mechanical property and heat resistance etc.
Performance, it will not be weakened using rear ionic conductivity and electrochemical stability for a long time, lithium polymer battery is after a long time use
Will not aging, increase life-span of battery charging and discharging.
Embodiment
Describe embodiments of the present invention in detail below with reference to embodiment, whereby to the present invention how application technology hand
Section solves technical problem, and the implementation process for reaching technique effect can fully understand and implement according to this.
It should be noted that writing length to save specification, unnecessary repetition and waste are avoided, in the feelings not conflicted
Under condition, the feature in embodiment and embodiment in the application can be mutually combined.
A kind of graphene composite material for improving lithium polymer battery mechanical strength of embodiment 1
A kind of graphene composite material for improving lithium polymer battery mechanical strength, include the component composition of following parts by weight：Stone
The black parts by weight of alkene 50, the parts by weight of diamine POSS 11, the parts by weight of steel alloy 1, the parts by weight of the concentrated sulfuric acid 35, benzene alkene nitrile-styrene two
The parts by weight of membered copolymer 4, the parts by weight of bisphenol epoxy 20, the parts by weight of carborundum 4, the parts by weight of sodium nitrate 15, hydroxy ethyl fiber
Plain 4 parts by weight, the parts by weight of TMAH 3, the parts by weight of nano-zinc oxide powder 4, the parts by weight of hydrogen sulfide 5, hydroquinones 1
Parts by weight, the parts by weight of deionized water 55,5% parts by weight of hydrogen peroxide 30, the parts by weight of absolute ethyl alcohol 60, the weight of cyclopentadienyl titanium dichloride 10
Part；Wherein, the steel alloy includes iron-carbon alloy, aluminium, copper and mickel；The carborundum includes quartz sand, petroleum coke and Mo Sangshi.
As the priority scheme of the present invention, step of the invention（1）Described in the mass ratio of steel alloy each component be iron carbon
Alloy 30%, aluminium 10%, copper 35%, nickel 25%；The mass ratio of the carborundum each component is quartz sand 55%, petroleum coke 15%, Mo Sang
Stone 30%.
A kind of graphene composite material for improving lithium polymer battery mechanical strength of embodiment 2
A kind of graphene composite material for improving lithium polymer battery mechanical strength, include the component composition of following parts by weight：Stone
The black parts by weight of alkene 50, the parts by weight of diamine POSS 12, the parts by weight of steel alloy 2, the parts by weight of the concentrated sulfuric acid 45, benzene alkene nitrile-styrene two
The parts by weight of membered copolymer 7, the parts by weight of bisphenol epoxy 23, the parts by weight of carborundum 5, the parts by weight of sodium nitrate 20, hydroxy ethyl fiber
Plain 6 parts by weight, the parts by weight of TMAH 5, the parts by weight of nano-zinc oxide powder 5, the parts by weight of hydrogen sulfide 7, hydroquinones 3
Parts by weight, the parts by weight of deionized water 60,5% parts by weight of hydrogen peroxide 35, the parts by weight of absolute ethyl alcohol 65, the weight of cyclopentadienyl titanium dichloride 11
Part；Wherein, the steel alloy includes iron-carbon alloy, aluminium, copper and mickel；The carborundum includes quartz sand, petroleum coke and Mo Sangshi.
As the priority scheme of the present invention, step of the invention（1）Described in the mass ratio of steel alloy each component be iron carbon
Alloy 30%, aluminium 10%, copper 35%, nickel 25%；The mass ratio of the carborundum each component is quartz sand 55%, petroleum coke 15%, Mo Sang
Stone 30%.
A kind of graphene composite material for improving lithium polymer battery mechanical strength of embodiment 3
A kind of graphene composite material for improving lithium polymer battery mechanical strength, include the component composition of following parts by weight：Bag
Include the component composition of following parts by weight：The parts by weight of graphene 50, diamine POSS 11-13 parts by weight, steel alloy 1-3 parts by weight,
Concentrated sulfuric acid 35-55 parts by weight, benzene alkene nitrile-St copolymer 4-10 parts by weight, bisphenol epoxy 20-26 parts by weight,
Carborundum 4-6 parts by weight, sodium nitrate 15-25 parts by weight, hydroxyethyl cellulose 4-8 parts by weight, TMAH 3-7 weight
Part, nano-zinc oxide powder 4-6 parts by weight, hydrogen sulfide 5-9 parts by weight, hydroquinones 1-5 parts by weight, deionized water 55-65 weight
Measure part, 5% hydrogen peroxide 30-40 parts by weight, absolute ethyl alcohol 60-70 parts by weight, cyclopentadienyl titanium dichloride 10-12 parts by weight；Wherein, institute
Stating steel alloy includes iron-carbon alloy, aluminium, copper and mickel；The carborundum includes quartz sand, petroleum coke and Mo Sangshi.
As the priority scheme of the present invention, step of the invention（1）Described in the mass ratio of steel alloy each component be iron carbon
Alloy 30%, aluminium 10%, copper 35%, nickel 25%；The mass ratio of the carborundum each component is quartz sand 55%, petroleum coke 15%, Mo Sang
Stone 30%.
A kind of graphene composite material for improving lithium polymer battery mechanical strength of embodiment 4
A kind of graphene composite material for improving lithium polymer battery mechanical strength, comprises the following steps：
（1）Selection；
（2）Diamine POSS preparation：Added successively into 500mL three-necked flask 500mL toluene, 75mL deionized waters and
8gTEAOH, magnetic agitation 60min, 15mLAPS and 26mLPTES mixed liquor is then added dropwise, is obtained after being heated to reflux 48h
Transparency liquid, continue to heat 50min volatilization toluene, obtain lime milky product, washed with the mixed solution of tetrahydrofuran and methanol
Product is washed, is freezed under vacuum condition and obtains product diamine POSS；
（3）The preparation of graphene oxide：A, according to step（1）In each parts by weight of raw materials weigh graphite powder keep bath temperature be 15
DEG C condition of ice bath under add the concentrated sulfuric acid as solvent, be stirred after 30min and be slowly added to sodium nitrate, hydrogen sulfide successively, stir
Mix 20min；45 DEG C, stirring reaction 2h are warming up to, 95 DEG C is then heated to and adds deionized water and octaphenyl POSS, stirring
30min, stop reaction, add 5% hydrogen peroxide, centrifuge while hot, respectively with appropriate 5% watery hydrochloric acid and distillation water washing, oxidation is made
Graphene first product；
B, by graphene oxide first product made from above-mentioned steps a with and carborundum be stirred, adsorbed, be made oxidation stone
Black alkene；
（4）The reduction of graphene oxide：By step（3）After obtained graphene oxide mixes with Nano-Zinc powder, according to heating
Speed is that to be heated to temperature be 950 DEG C to 15 DEG C/min, and constant temperature adds TMAH and keeps 24h, the oxygen after being reduced
Graphite alkene；
（5）The preparation of graphene composite material：A, by step（4）Graphene oxide graphene oxide and two after obtained reduction
It is scattered in after first amine POSS mixing using ultrasonic wave in appropriate absolute ethyl alcohol, after stirring, is warming up to 50 DEG C of addition dichloros
Titanocenes, after stirring 25min, solution is transferred in reactor, argon gas is passed through as protection hermetic seal, in 200 DEG C of reactions
48h, stop reaction, after product is filtered, with distillation water washing, freeze under vacuum, at the beginning of obtaining graphene composite material
Product；
B, graphene composite material first product and step（1）In remaining ingredient be placed in mixer, control temperature be 160 DEG C, it is low
Speed mixing 8min, then heats to 190 DEG C, mixed at high speed 8min, obtains compound；Compound is placed in dryer, dried
Temperature is 105 DEG C, drying time 2h, and the graphene composite material for improving lithium polymer battery mechanical strength is made.
As the preferred scheme of the present invention, step of the invention（1）Selection uses the constitutive material of embodiment 1.
As the preferred scheme of the present invention, step of the invention（1）Described in the mass ratio of steel alloy each component be iron carbon
Alloy 30%, aluminium 10%, copper 35%, nickel 25%；The mass ratio of the carborundum each component is quartz sand 55%, petroleum coke 15%, Mo Sang
Stone 30%.
A kind of graphene composite material for improving lithium polymer battery mechanical strength of embodiment 5
A kind of graphene composite material for improving lithium polymer battery mechanical strength, comprises the following steps：
（1）Selection；
（2）Diamine POSS preparation：Added successively into 500mL three-necked flask 500mL toluene, 75mL deionized waters and
8gTEAOH, magnetic agitation 60min, 15mLAPS and 26mLPTES mixed liquor is then added dropwise, is obtained after being heated to reflux 48h
Transparency liquid, continue to heat 50min volatilization toluene, obtain lime milky product, washed with the mixed solution of tetrahydrofuran and methanol
Product is washed, is freezed under vacuum condition and obtains product diamine POSS；
（3）The preparation of graphene oxide：A, according to step（1）In each parts by weight of raw materials weigh graphite powder keep bath temperature be 20
DEG C condition of ice bath under add the concentrated sulfuric acid as solvent, be stirred after 35min and be slowly added to sodium nitrate, hydrogen sulfide successively, stir
Mix 20-30min；50 DEG C, stirring reaction 2.5h are warming up to, 95 DEG C is then heated to and adds deionized water and octaphenyl POSS, stir
35min is mixed, stops reaction, adds 5% hydrogen peroxide, centrifuges while hot, respectively with appropriate 5% watery hydrochloric acid and distillation water washing, oxygen is made
Graphite alkene first product；
B, by graphene oxide first product made from above-mentioned steps a with and carborundum be stirred, adsorbed, be made oxidation stone
Black alkene；
（4）The reduction of graphene oxide：By step（3）After obtained graphene oxide mixes with Nano-Zinc powder, according to heating
Speed is that to be heated to temperature be 1000 DEG C to 17 DEG C/min, and constant temperature adds TMAH and keeps 25h, after being reduced
Graphene oxide；
（5）The preparation of graphene composite material：A, by step（4）Graphene oxide graphene oxide and two after obtained reduction
It is scattered in after first amine POSS mixing using ultrasonic wave in appropriate absolute ethyl alcohol, after stirring, is warming up to 50 DEG C of addition dichloros
Titanocenes, after stirring 25min, solution is transferred in reactor, argon gas is passed through as protection hermetic seal, in 200 DEG C of reactions
48h, stop reaction, after product is filtered, with distillation water washing, freeze under vacuum, at the beginning of obtaining graphene composite material
Product；
B, graphene composite material first product and step（1）In remaining ingredient be placed in mixer, control temperature be 165 DEG C, it is low
Speed mixing 10min, then heats to 193 DEG C, mixed at high speed 9min, obtains compound；Compound is placed in dryer, dried
Temperature is 105 DEG C, drying time 2.3h, and the graphene composite material for improving lithium polymer battery mechanical strength is made.
As the preferred scheme of the present invention, step of the invention（1）Selection uses the constitutive material of embodiment 1.
As the preferred scheme of the present invention, step of the invention（1）Described in the mass ratio of steel alloy each component be iron carbon
Alloy 30%, aluminium 10%, copper 35%, nickel 25%；The mass ratio of the carborundum each component is quartz sand 55%, petroleum coke 15%, Mo Sang
Stone 30%.
A kind of graphene composite material for improving lithium polymer battery mechanical strength of embodiment 6
A kind of graphene composite material for improving lithium polymer battery mechanical strength, comprises the following steps：
（1）Selection；
（2）Diamine POSS preparation：Added successively into 500mL three-necked flask 500mL toluene, 75mL deionized waters and
8gTEAOH, magnetic agitation 60min, 15mLAPS and 26mLPTES mixed liquor is then added dropwise, is obtained after being heated to reflux 48h
Transparency liquid, continue to heat 50min volatilization toluene, obtain lime milky product, washed with the mixed solution of tetrahydrofuran and methanol
Product is washed, is freezed under vacuum condition and obtains product diamine POSS；
（3）The preparation of graphene oxide：A, according to step（1）In each parts by weight of raw materials weigh graphite powder keep bath temperature be
The concentrated sulfuric acid is added under 15-25 DEG C of condition of ice bath as solvent, is stirred after 40min and is slowly added to sodium nitrate, vulcanization successively
Hydrogen, stir 30min；55 DEG C, stirring reaction 3h are warming up to, 95 DEG C is then heated to and adds deionized water and octaphenyl POSS, stir
40min is mixed, stops reaction, adds 5% hydrogen peroxide, centrifuges while hot, respectively with appropriate 5% watery hydrochloric acid and distillation water washing, oxygen is made
Graphite alkene first product；
B, by graphene oxide first product made from above-mentioned steps a with and carborundum be stirred, adsorbed, be made oxidation stone
Black alkene；
（4）The reduction of graphene oxide：By step（3）After obtained graphene oxide mixes with Nano-Zinc powder, according to heating
Speed is that to be heated to temperature be 1050 DEG C to 20 DEG C/min, and constant temperature adds TMAH and keeps 26h, after being reduced
Graphene oxide；
（5）The preparation of graphene composite material：A, by step（4）Graphene oxide graphene oxide and two after obtained reduction
It is scattered in after first amine POSS mixing using ultrasonic wave in appropriate absolute ethyl alcohol, after stirring, is warming up to 50 DEG C of addition dichloros
Titanocenes, after stirring 25min, solution is transferred in reactor, argon gas is passed through as protection hermetic seal, in 200 DEG C of reactions
48h, stop reaction, after product is filtered, with distillation water washing, freeze under vacuum, at the beginning of obtaining graphene composite material
Product；
B, graphene composite material first product and step（1）In remaining ingredient be placed in mixer, control temperature be 170 DEG C, it is low
Speed mixing 12min, then heats to 195 DEG C, mixed at high speed 10min, obtains compound；Compound is placed in dryer, dried
Dry temperature is 105 DEG C, drying time 2.6h, and the graphene composite material for improving lithium polymer battery mechanical strength is made.
As the preferred scheme of the present invention, step of the invention（1）Selection uses the constitutive material of embodiment 1.
As the preferred scheme of the present invention, step of the invention（1）Described in the mass ratio of steel alloy each component be iron carbon
Alloy 30%, aluminium 10%, copper 35%, nickel 25%；The mass ratio of the carborundum each component is quartz sand 55%, petroleum coke 15%, Mo Sang
Stone 30%.
All above-mentioned this intellectual properties of primarily implementation, the not this new product of implementation of setting limitation other forms
And/or new method.Those skilled in the art will utilize this important information, the above modification, to realize similar execution feelings
Condition.But all modifications or transformation belong to the right of reservation based on new product of the present invention.
Claims (3)
1. a kind of graphene composite material for improving lithium polymer battery mechanical strength, it is characterised in that by following steps system
It is standby to form：
（1）Selection:Component composition including following parts by weight：The parts by weight of graphene 50, diamine POSS 11-13 parts by weight, close
Golden steel 1-3 parts by weight, concentrated sulfuric acid 35-55 parts by weight, benzene alkene nitrile-St copolymer 4-10 parts by weight, bisphenol epoxies tree
Fat 20-26 parts by weight, carborundum 4-6 parts by weight, sodium nitrate 15-25 parts by weight, hydroxyethyl cellulose 4-8 parts by weight, tetramethyl
Ammonium hydroxide 3-7 parts by weight, nano-zinc oxide powder 4-6 parts by weight, hydrogen sulfide 5-9 parts by weight, hydroquinones 1-5 parts by weight,
Deionized water 55-65 parts by weight, 5% hydrogen peroxide 30-40 parts by weight, absolute ethyl alcohol 60-70 parts by weight, cyclopentadienyl titanium dichloride 10-12
Parts by weight；Wherein, the steel alloy includes iron-carbon alloy, aluminium, copper and mickel；The carborundum includes quartz sand, petroleum coke and not
Sang Shi；
（2）Diamine POSS preparation：Added successively into 500mL three-necked flask 500mL toluene, 75mL deionized waters and
8gTEAOH, magnetic agitation 60min, 15mLAPS and 26mLPTES mixed liquor is then added dropwise, is obtained after being heated to reflux 48h
Transparency liquid, continue to heat 50min volatilization toluene, obtain lime milky product, washed with the mixed solution of tetrahydrofuran and methanol
Product is washed, is freezed under vacuum condition and obtains product diamine POSS；
（3）The preparation of graphene oxide：A, according to step（1）In each parts by weight of raw materials weigh graphite powder keep bath temperature be
The concentrated sulfuric acid is added under 15-25 DEG C of condition of ice bath as solvent, is stirred after 30-40min and is slowly added to sodium nitrate, sulphur successively
Change hydrogen, stir 20-30min；45-55 DEG C, stirring reaction 2-3h is warming up to, 95 DEG C is then heated to and adds deionized water and eight benzene
Base POSS, 30-40min is stirred, stop reaction, add 5% hydrogen peroxide, centrifuged while hot, respectively with appropriate 5% watery hydrochloric acid and distilled water
Washing, graphene oxide first product is made；
B, by graphene oxide first product made from above-mentioned steps a with and carborundum be stirred, adsorbed, be made oxidation stone
Black alkene；
（4）The reduction of graphene oxide：By step（3）After obtained graphene oxide mixes with Nano-Zinc powder, according to heating
Speed is that to be heated to temperature be 950-1050 DEG C to 15-20 DEG C/min, and constant temperature adds TMAH and keeps 24-26h, obtains
Graphene oxide after to reduction；
（5）The preparation of graphene composite material：A, by step（4）Graphene oxide graphene oxide and two after obtained reduction
It is scattered in after first amine POSS mixing using ultrasonic wave in appropriate absolute ethyl alcohol, after stirring, is warming up to 50 DEG C of addition dichloros
Titanocenes, after stirring 25min, solution is transferred in reactor, argon gas is passed through as protection hermetic seal, in 200 DEG C of reactions
48h, stop reaction, after product is filtered, with distillation water washing, freeze under vacuum, at the beginning of obtaining graphene composite material
Product；
B, graphene composite material first product and step（1）In remaining ingredient be placed in mixer, it is 160-170 to control temperature
DEG C, mixed on low speed 8-12min, 190-195 DEG C is then heated to, mixed at high speed 8-10min, obtains compound；Compound is put
In dryer, drying temperature is 105 DEG C, drying time 2-2.6h, and the stone for improving lithium polymer battery mechanical strength is made
Black alkene composite.
A kind of 2. graphene composite material of raising lithium polymer battery mechanical strength according to right 1, it is characterised in that
The step（1）Selection:Component composition including following parts by weight：The parts by weight of graphene 50, the parts by weight of diamine POSS 12,
The parts by weight of steel alloy 2, the parts by weight of the concentrated sulfuric acid 45, benzene alkene nitrile-parts by weight of St copolymer 7, the weight of bisphenol epoxy 23
Measure part, the parts by weight of carborundum 5, the parts by weight of sodium nitrate 20, the parts by weight of hydroxyethyl cellulose 6, the parts by weight of TMAH 5,
The parts by weight of nano-zinc oxide powder 5, the parts by weight of hydrogen sulfide 7, the parts by weight of hydroquinones 3, the parts by weight of deionized water 60,5% dioxygen
The parts by weight of water 35, the parts by weight of absolute ethyl alcohol 65, the parts by weight of cyclopentadienyl titanium dichloride 11.
A kind of 3. graphene composite material of raising lithium polymer battery mechanical strength according to right 1, it is characterised in that
The step（1）Described in steel alloy each component mass ratio for iron-carbon alloy 30%, aluminium 10%, copper 35%, nickel 25%；The carbonization
The mass ratio of silicon each component is quartz sand 55%, not petroleum coke 15%, Sang Shi 30%.
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