CN109280540A - It is a kind of using graphene aerogel as energy storage material of matrix and preparation method thereof - Google Patents
It is a kind of using graphene aerogel as energy storage material of matrix 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 103
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 99
- 238000004146 energy storage Methods 0.000 title claims abstract description 61
- 239000004964 aerogel Substances 0.000 title claims abstract description 59
- 239000011159 matrix material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000011232 storage material Substances 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 32
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 25
- 230000003213 activating effect Effects 0.000 claims abstract description 23
- KBZFDRWPMZESDI-UHFFFAOYSA-N 5-aminobenzene-1,3-dicarboxylic acid Chemical compound NC1=CC(C(O)=O)=CC(C(O)=O)=C1 KBZFDRWPMZESDI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 8
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 8
- 230000002035 prolonged effect Effects 0.000 claims abstract description 8
- 238000002347 injection Methods 0.000 claims abstract description 6
- 239000007924 injection Substances 0.000 claims abstract description 6
- 238000003860 storage Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 55
- 239000008367 deionised water Substances 0.000 claims description 48
- 229910021641 deionized water Inorganic materials 0.000 claims description 48
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- 239000000203 mixture Substances 0.000 claims description 35
- 238000001914 filtration Methods 0.000 claims description 28
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 24
- 238000004321 preservation Methods 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 14
- 235000010288 sodium nitrite Nutrition 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- 229910052786 argon Inorganic materials 0.000 claims description 12
- 239000007789 gas Substances 0.000 claims description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
- WNRGWPVJGDABME-UHFFFAOYSA-N 3,5-Dimethoxyaniline Chemical compound COC1=CC(N)=CC(OC)=C1 WNRGWPVJGDABME-UHFFFAOYSA-N 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 150000003233 pyrroles Chemical class 0.000 claims description 8
- 229920005573 silicon-containing polymer Polymers 0.000 claims description 8
- 238000007598 dipping method Methods 0.000 claims description 6
- 239000012065 filter cake Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 239000002893 slag Substances 0.000 claims description 6
- 238000001291 vacuum drying Methods 0.000 claims description 6
- 238000010792 warming Methods 0.000 claims description 6
- 238000002390 rotary evaporation Methods 0.000 claims description 5
- 238000004821 distillation Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 3
- FSUMZUVANZAHBW-UHFFFAOYSA-N n,n-dimethoxyaniline Chemical compound CON(OC)C1=CC=CC=C1 FSUMZUVANZAHBW-UHFFFAOYSA-N 0.000 claims description 2
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 abstract description 6
- DMLAVOWQYNRWNQ-UHFFFAOYSA-N azobenzene Chemical compound C1=CC=CC=C1N=NC1=CC=CC=C1 DMLAVOWQYNRWNQ-UHFFFAOYSA-N 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 239000003431 cross linking reagent Substances 0.000 abstract description 5
- 239000000178 monomer Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 230000008859 change Effects 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 230000007774 longterm Effects 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 2
- 230000002269 spontaneous effect Effects 0.000 abstract description 2
- -1 methoxyl group Chemical group 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 239000004698 Polyethylene Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000017 hydrogel Substances 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 229920000573 polyethylene Polymers 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
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- 239000002105 nanoparticle Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 230000005355 Hall effect Effects 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000018199 S phase Effects 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000012954 diazonium Substances 0.000 description 1
- 150000001989 diazonium salts Chemical class 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- VIKNJXKGJWUCNN-XGXHKTLJSA-N norethisterone Chemical compound O=C1CC[C@@H]2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1 VIKNJXKGJWUCNN-XGXHKTLJSA-N 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- SIOXPEMLGUPBBT-UHFFFAOYSA-N picolinic acid Chemical compound OC(=O)C1=CC=CC=N1 SIOXPEMLGUPBBT-UHFFFAOYSA-N 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C07C245/08—Azo compounds, i.e. compounds having the free valencies of —N=N— groups attached to different atoms, e.g. diazohydroxides with nitrogen atoms of azo groups bound to carbon atoms of six-membered aromatic rings with the two nitrogen atoms of azo groups bound to carbon atoms of six-membered aromatic rings, e.g. azobenzene
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Abstract
The invention discloses a kind of using graphene aerogel as the energy storage material of matrix and preparation method, belongs to new energy materials field.The present invention introduces rich hydroxyl chain polyvinyl alcohol and links graphene sheet layer, be conducive to the opening and transmission of passage of heat using graphene oxide as raw material；Spontaneous assembling between the graphene oxide and pyrrole monomer that handle through polyvinyl alcohol is improved energy storage efficiency by the present invention；The present invention is occurred graft reaction, increases the long-acting performance of energy storage by vacuum condition of ice bath from stream injection technology, amino and graphene aerogel oxygen-containing group is prolonged；The present invention obtains the energy storage activating agent of azobenzene using 5- amino isophthalic acid as raw material, and azobenzene molecule can be used for the long-term storage of solar energy highly effective；The present invention increases energy storage capacity finally using graphene aerogel as template.The present invention solves the problem of graphene aerogel materials'use crosslinking agent can make the structural unit of graphene oxide change, influence energy-storage property.
Description
Technical field
The invention belongs to new energy materials fields, and in particular to it is a kind of using graphene aerogel as the energy storage material of matrix and
Preparation method.
Background technique
Graphene is both most thin material, and most tough material, and breaking strength is 200 times higher than steel.While it
There is good elasticity again, stretch range can reach the 20% of own dimensions.Graphene most potential application at present is as silicon
Substitute manufactures ultra micro transistor npn npn, for producing following supercomputer.Replace silicon, computer processor with graphene
The speed of service will improve hundreds times.
Graphene is the new carbon with bi-dimensional cellular shape structure, has very high mechanical strength, and elasticity is thermally conductive
Property, electric conductivity and quantum hall effect etc. attract wide attention in recent years.Graphene enhances as a kind of nanoparticle
Epoxy resin composite material has been research hotspot, but graphene nano particle bad dispersibility, easily group in epoxy resin-base
It is poly-, cause the performance of composite material after resin modified not rise anti-drop in some aspects.
Aeroge is a kind of solid matter form, the smallest solid of world's upper density.Density can reach 3kg/m3.It is general normal
The aeroge seen is that silica aerogel was made in 1931.There are many type of aeroge, there is silicon systems, carbon system, sulphur system, metal oxide
System, metal system etc..Any substance aeroge can keep its shape invariance after drying and removing internal solvent substantially, and produce
Object has high porosity, low-density.
Aeroge includes a large amount of hole, and hole ratio is a kind of porous material with nanostructure 80% or more,
The aspects such as mechanics, acoustics, calorifics, optics show its peculiar property.They differ markedly from hole configurations in micron and milli
The porous material of rice magnitude, very thin nanostructure make the thermal conductivity of material extremely low, have great specific surface area airsetting
Glue is more much smaller than traditional porous material to the scattering of light, sound, these unique properties not only make the material in base
It is intriguing in plinth research, and contain broad application prospect in many fields.
Currently, sol-gel method preparation is usually used in aeroge, i.e., it is made wet solidifying first with the crosslinking feature of crosslinking agent
Glue (i.e. hydrogel), then by being dried to obtain.For graphene aerogel, some reports are using graphene oxide and hand over
Join agent mixing, so that the two is crosslinked reaction and obtain graphene oxide colloidal sol (i.e. hydrogel), is then obtained by dry, reduction
Graphene aerogel.But in this method, graphene oxide is crosslinked with crosslinking agent when reacting, the structure of graphene oxide
Unit is changed, and causes the script structure of graphene in graphene aerogel generated to change, to make graphite
The original conduction of alkene, mechanics, energy-storage property are affected.
Summary of the invention
The technical problems to be solved by the invention: can make to aoxidize stone for current graphene aerogel materials'use crosslinking agent
The problem of structural unit of black alkene changes, influences energy-storage property provides a kind of using graphene aerogel as the energy storage of matrix
Material and preparation method thereof.
In order to solve the above technical problems, the present invention is using technical solution as described below:
It is a kind of using graphene aerogel as the energy storage material of matrix, including graphene aerogel matrix object, energy storage activating agent；
The preparation method of the graphene aerogel matrix object, includes the following steps:
(1) it takes graphene oxide 1 ~ 3:30 in mass ratio ~ 50 to be added in deionized water, adds 6 ~ 9 times of graphene oxide quality
Polyvinyl alcohol, in 140 ~ 150 DEG C keep the temperature, be cooled to room temperature, cooled material taken to wash through deionized water, obtain washings, be passed through argon
Gas shielded takes washings to keep the temperature, and is cooled to room temperature, and obtains cooled material a；
(2) take cooled material a 1 ~ 3:10 in mass ratio ~ 20 that deionized water is added, ultrasonic disperse adds cooled material a mass 2 ~ 5%
Pyrroles, ultrasound stands 3 ~ 5 days in 25 ~ 30 DEG C, obtains standing object, takes and stands object 1 ~ 4:30 in mass ratio ~ 40 anhydrous second is added
Alcohol is stood, and dehydrated alcohol is removed in filtering, is repeated that dehydrated alcohol is added, is stood process 5 ~ 8 times, filtering takes final filtration cakes torrefaction, obtains
Dried object；
(3) it takes dimethyl silicone polymer 1 ~ 3:10 in mass ratio ~ 20 that n-hexane is added, is stirred, must mix in 25 ~ 30 DEG C
Liquid takes dried object 1 ~ 3:80 in mass ratio ~ 100 that mixed liquid dipping is added, and is prolonged stream injection naturally, and filtering is taken out and done after impregnating
Dry object is kept the temperature in 50 ~ 55 DEG C, is cooled to room temperature to get graphene aerogel matrix object.
The heat-retaining condition of washings in the step (1) are as follows: be warming up to 750 ~ 800 DEG C of 2 ~ 4h of heat preservation.
Naturally prolong the condition of stream injection in the step (3) are as follows: keep 4 ~ 6h in 2 ~ 4 DEG C, vacuum condition.
The energy storage activating agent the preparation method comprises the following steps:
S1. it takes 5- amino isophthalic acid 2 ~ 4:1 in mass ratio ~ 3:10 ~ 20 that sodium hydroxide, deionized water is added, is stirred in 2 ~ 4 DEG C
Mixing is mixed, the sodium nitrite of 5- amino isophthalic acid quality 40 ~ 60% is added, is stirred, obtains mixture, take mixture
1 ~ 4:5 ~ 9 are added dropwise in hydrochloric acid in mass ratio, are controlled 30 ~ 50min of time for adding, are stirred, obtain stirring mixture；
S2. it takes 3,5- dimethoxyaniline, 1 ~ 5:20 in mass ratio ~ 30 to be added in hydrochloric acid, is stirred, adds in 2 ~ 5 DEG C
The stirring mixture of 3,5- 1 ~ 3 times of dimethoxyaniline quality adjusts pH to 6 ~ 7, is passed through argon gas protection, keeps the temperature in 2 ~ 5 DEG C,
It filters, takes and filter slag through distillation water washing, vacuum drying obtains energy storage activating agent.
That mixture is stirred in the step S1 is stirred condition are as follows: is stirred 1 ~ 3h in -2 ~ 3 DEG C.
It is described using graphene aerogel as the preparation method of the energy storage material of matrix, include the following steps:
Take energy storage activating agent 1 ~ 5:0.2 in mass ratio ~ 0.5:50 ~ 60 that sodium nitrite, deionized water is added, it is stirred 20 ~
30min obtains mixture a, and the hydrochloric acid for adding deionized water quality 30 ~ 40% is stirred, and obtains mixed liquor, takes mixed liquor by matter
Graphene aerogel matrix object, deionized water is added than 40 ~ 50:1 ~ 4:80 ~ 100 in amount, in -4 ~ 1 DEG C of 2 ~ 5h of heat preservation, then at 25 ~
30 DEG C are stirred, and filtering takes filter cake through deionized water, acetone washing, rotary evaporation is to get using graphene aerogel as matrix
Energy storage material.
The mixed liquor is stirred condition are as follows: is stirred 1 ~ 3h in 2 ~ 5 DEG C.
The present invention is compared with other methods, and advantageous effects are:
(1) for the present invention using graphene oxide as raw material, addition polyvinyl alcohol is additive, during the three-dimensional assembling of graphene
It introduces rich hydroxyl chain polyvinyl alcohol and links graphene sheet layer, effectively reduce the π-π overlapping of piece interlayer, obtaining has uniqueness
The bigger serface three-dimension layer secondary aperture carbon of pore system, it is logical that the three-dimensional porous system of the graphene being mutually communicated provides smooth mass transfer
Road and excellent electron-transport network, as the base structure of graphene aerogel, be conducive to passage of heat opening and
Transmission；
(2) present invention is by the spontaneous assembling between the graphene oxide and pyrrole monomer that handle through polyvinyl alcohol, without adding it
His Oxidizing and Reducing Agents prepares composite hydrogel at room temperature, also based on the oxidation between graphene oxide and pyrrole monomer
Original reaction, pyrroles play the role of crosslinking agent, and surface contains weak electropositive pyrroles's phase in electronegative graphene oxide and surface
Mutually attract, is self-assembly of gel through reduction, while pyridine monomer is oxidized graphene oxidation polymerization and forms polypyridine, aoxidizes stone
Conjugation between black alkene lamella makes its gelation, in the case where not changing graphene oxide structural unit, to graphene
It carries out being cross-linked to form gel, is conducive to good thermally conductive, energy-storage property the preservation that graphene this body structure has, improve energy storage
Efficiency；
(3) dimethyl silicone polymer is introduced graphene aerogel by vacuum condition of ice bath from stream injection technology is prolonged by the present invention,
Graft reaction occurs for the amino and graphene aerogel oxygen-containing group of dimethyl silicone polymer, is formed and orderly stablizes π-π connection, protects
It demonstrate,proves three-dimensional grapheme aeroge network skeleton completely to stablize with microcosmic combination interface, so that graphene aerogel internal sheets layer unit
It further regularization and is completely embedded, the complete long-acting holding maintained conducive to capable transport channel of structural framework increases
The long-acting performance of energy storage；
(4) present invention carries out diazo-reaction under the action of sodium nitrite, adds using 5- amino isophthalic acid as raw material
3,5- dimethoxyanilines carry out coupling reaction, obtain the energy storage activating agent of azobenzene, even containing electrophilic carboxyl
Pyridine molecule has different absorption characteristics in cis and trans configuration, its generation can be excited trans- to π * by π by ultraviolet light
Become cis-, and visible light by n to π * excite its it is cis- become trans-, pushed away simultaneous with the azobenzene derivatives molecule of carboxyl
It draws electronic structure and faces a methoxyl group and contraposition/meta position carboxyl functional group's effect, there is biggish isomerisation degree
With longer reply half-life period, is conducive to improve it to the absorption intensity and efficiency of solar energy and keeps good storage steady simultaneously
It is qualitative, it can be used for the long-term storage of solar energy highly effective；
(5) present invention orderly carries energy storage activating agent, improves the energy of azobenzene molecule finally using graphene aerogel as template
Metric density and half-life period, using diazonium salt radical reaction, by azobenzene molecule covalence graft to redox graphene surface,
The optical Response of energy storage is improved, energy storage capacity is increased.
Specific embodiment
Graphene aerogel matrix object the preparation method comprises the following steps:
(1) it takes graphene oxide 1 ~ 3:30 in mass ratio ~ 50 to be added in deionized water, adds 6 ~ 9 times of graphene oxide quality
Polyvinyl alcohol be cooled to room temperature in 140 ~ 150 DEG C of 4 ~ 6h of heat preservation, cooled material taken to wash through deionized water, obtain washings, lead to
Enter argon gas protection, takes washings to be warming up to 750 ~ 800 DEG C of 2 ~ 4h of heat preservation, be cooled to room temperature, obtain cooled material a；
(2) take cooled material a 1 ~ 3:10 in mass ratio ~ 20 that deionized water is added, 30 ~ 40min of ultrasonic disperse adds cooled material a
The pyrroles of quality 2 ~ 5%, 5 ~ 10min of ultrasound stand 3 ~ 5 days in 25 ~ 30 DEG C, obtain standing object, take and stand object 1 ~ 4:30 in mass ratio
~ 40 are added dehydrated alcohol, stand 5 ~ 7h, and dehydrated alcohol is removed in filtering, repeat that dehydrated alcohol is added, stand process 5 ~ 8 times, filtering,
Final filtration cakes torrefaction is taken, dried object is obtained；
(3) it takes dimethyl silicone polymer 1 ~ 3:10 in mass ratio ~ 20 that n-hexane is added, is stirred 30 ~ 40min in 25 ~ 30 DEG C,
Mixed liquor is obtained, takes dried object 1 ~ 3:80 in mass ratio ~ 100 that mixed liquid dipping is added, is prolonged naturally under 2 ~ 4 DEG C, vacuum condition
Stream keeps 4 ~ 6h, and filtering is taken out dried object after impregnating and is cooled to room temperature in 50 ~ 55 DEG C of 10 ~ 12h of heat preservation to get graphene airsetting
Matrix body object.
Energy storage activating agent the preparation method comprises the following steps:
S1. it takes 5- amino isophthalic acid 2 ~ 4:1 in mass ratio ~ 3:10 ~ 20 that sodium hydroxide, deionized water is added, is stirred in 2 ~ 4 DEG C
30 ~ 50min of mixing is mixed, the sodium nitrite of 5- amino isophthalic acid quality 40 ~ 60% is added, is stirred 50 ~ 60min, obtains
Mixture, taking mixture 1 ~ 4:5 ~ 9 to be in mass ratio added dropwise to concentration is to control 30 ~ 50min of time for adding in 1mol/L hydrochloric acid,
It is stirred 1 ~ 3h in -2 ~ 3 DEG C, obtains stirring mixture；
S2. taking 3,5- dimethoxyaniline, 1 ~ 5:20 in mass ratio ~ 30 that concentration is added is to stir in 1mol/L hydrochloric acid in 2 ~ 5 DEG C
30 ~ 40min is mixed, the stirring mixture of 1 ~ 3 times of 3,5- dimethoxyaniline quality is added, pH to 6 ~ 7 is adjusted, is passed through argon
Gas shielded is filtered in 2 ~ 5 DEG C of 1 ~ 3h of heat preservation, is taken and is filtered slag through distillation water washing, vacuum drying obtains energy storage activating agent.
It is a kind of using graphene aerogel as the preparation method of the energy storage material of matrix, include the following steps:
Take energy storage activating agent 1 ~ 5:0.2 in mass ratio ~ 0.5:50 ~ 60 that sodium nitrite, deionized water is added, it is stirred 20 ~
30min obtains mixture a, and the concentration for adding deionized water quality 30 ~ 40% is 1mol/L hydrochloric acid, it is stirred 1 in 2 ~ 5 DEG C ~
3h obtains mixed liquor, takes mixed liquor 40 ~ 50:1 in mass ratio ~ 4:80 ~ 100 that graphene aerogel matrix object, deionized water is added,
In -4 ~ 1 DEG C of 2 ~ 5h of heat preservation, it is stirred 12 ~ 18h then at 25 ~ 30 DEG C, is filtered, takes filter cake through deionized water, acetone washing, rotation
Turn evaporation to get using graphene aerogel as the energy storage material of matrix.
Embodiment 1
Graphene aerogel matrix object the preparation method comprises the following steps:
(1) it takes graphene oxide 1:30 to be in mass ratio added in deionized water, adds 6 times of graphene oxide quality of polyethylene
Alcohol is cooled to room temperature in 140 DEG C of heat preservation 4h, cooled material is taken to wash through deionized water, obtain washings, is passed through argon gas protection, takes and wash
It washs object and is warming up to 750 DEG C of heat preservation 2h, be cooled to room temperature, obtain cooled material a；
(2) take cooled material a 1:10 in mass ratio that deionized water is added, ultrasonic disperse 30min adds cooled material a mass 2%
Pyrroles, ultrasonic 5min stand 3 days in 25 DEG C, obtain standing object, take and stand object 1:30 in mass ratio addition dehydrated alcohol, stand 5h,
Dehydrated alcohol is removed in filtering, repeats that dehydrated alcohol is added, stands process 5 times, filtering takes final filtration cakes torrefaction, obtains dried object；
(3) it takes dimethyl silicone polymer 1:10 in mass ratio that n-hexane is added, is stirred 30min in 25 DEG C, obtains mixed liquor, take
Mixed liquid dipping is added in dried object 1:80 in mass ratio, is prolonged stream naturally under 2 DEG C, vacuum condition and keeps 4h, leaching is taken out in filtering
Dried object is cooled to room temperature in 50 DEG C of heat preservation 10h to get graphene aerogel matrix object after bubble.
Energy storage activating agent the preparation method comprises the following steps:
S1. it takes 5- amino isophthalic acid 2:1:10 in mass ratio that sodium hydroxide, deionized water is added, is stirred in 2 DEG C
30min adds the sodium nitrite of 5- amino isophthalic acid quality 40%, is stirred 50min, obtains mixture, take mixture
It is to control time for adding 30min in 1mol/L hydrochloric acid, be stirred 1h in -2 ~ 3 DEG C, must stir that 1:5 in mass ratio, which is added dropwise to concentration,
Mix mixture；
S2. taking 3,5- dimethoxyaniline 1:20 in mass ratio that concentration is added is to be stirred in 1mol/L hydrochloric acid in 2 DEG C
30min adds the stirring mixture of 1 ~ 3 times of 3,5- dimethoxyaniline quality, adjusts pH to 6, argon gas protection is passed through, in 2
DEG C heat preservation 1h, filter, take filter slag through distill water washing, vacuum drying, obtain energy storage activating agent.
It is a kind of using graphene aerogel as the preparation method of the energy storage material of matrix, include the following steps:
It takes energy storage activating agent 1:0.2:50 in mass ratio that sodium nitrite, deionized water is added, is stirred 20min, obtains mixture
A, add deionized water quality 30% concentration be 1mol/L hydrochloric acid, be stirred 1h in 2 DEG C, obtain mixed liquor, take mixed liquor by
Mass ratio 40:1:80 is added graphene aerogel matrix object, deionized water and is stirred in -4 DEG C of heat preservation 2h then at 25 DEG C
12h, filtering, takes filter cake through deionized water, acetone washing, rotary evaporation is to get using graphene aerogel as the energy storage material of matrix
Material.
Embodiment 2
Graphene aerogel matrix object the preparation method comprises the following steps:
(1) it takes graphene oxide 2:40 to be in mass ratio added in deionized water, adds 7 times of graphene oxide quality of polyethylene
Alcohol is cooled to room temperature in 148 DEG C of heat preservation 5h, cooled material is taken to wash through deionized water, obtain washings, is passed through argon gas protection, takes and wash
It washs object and is warming up to 780 DEG C of heat preservation 3h, be cooled to room temperature, obtain cooled material a；
(2) take cooled material a 2:15 in mass ratio that deionized water is added, ultrasonic disperse 35min adds cooled material a mass 3%
Pyrroles, ultrasonic 8min stand 4 days in 28 DEG C, obtain standing object, take and stand object 3:35 in mass ratio addition dehydrated alcohol, stand 6h,
Dehydrated alcohol is removed in filtering, repeats that dehydrated alcohol is added, stands process 7 times, filtering takes final filtration cakes torrefaction, obtains dried object；
(3) it takes dimethyl silicone polymer 2:15 in mass ratio that n-hexane is added, is stirred 35min in 28 DEG C, obtains mixed liquor, take
Mixed liquid dipping is added in dried object 2:90 in mass ratio, is prolonged stream naturally under 3 DEG C, vacuum condition and keeps 5h, leaching is taken out in filtering
Dried object is cooled to room temperature in 54 DEG C of heat preservation 11h to get graphene aerogel matrix object after bubble.
Energy storage activating agent the preparation method comprises the following steps:
S1. it takes 5- amino isophthalic acid 3:2:15 in mass ratio that sodium hydroxide, deionized water is added, is stirred in 3 DEG C
40min adds the sodium nitrite of 5- amino isophthalic acid quality 50%, is stirred 55min, obtains mixture, take mixture
It is to control time for adding 40min in 1mol/L hydrochloric acid, be stirred 2h in 1 DEG C, must stir that 3:8 in mass ratio, which is added dropwise to concentration,
Mixture；
S2. taking 3,5- dimethoxyaniline 3:25 in mass ratio that concentration is added is to be stirred in 1mol/L hydrochloric acid in 4 DEG C
35min adds the stirring mixture of 2 times of 3,5- dimethoxyaniline quality, adjusts pH to 6.5, argon gas protection is passed through, in 4
DEG C heat preservation 2h, filter, take filter slag through distill water washing, vacuum drying, obtain energy storage activating agent.
It is a kind of using graphene aerogel as the preparation method of the energy storage material of matrix, include the following steps:
It takes energy storage activating agent 4:0.3:55 in mass ratio that sodium nitrite, deionized water is added, is stirred 25min, obtains mixture
A, add deionized water quality 35% concentration be 1mol/L hydrochloric acid, be stirred 2h in 4 DEG C, obtain mixed liquor, take mixed liquor by
Mass ratio 45:3:90 is added graphene aerogel matrix object, deionized water and is stirred in -1 DEG C of heat preservation 4h then at 28 DEG C
16h, filtering, takes filter cake through deionized water, acetone washing, rotary evaporation is to get using graphene aerogel as the energy storage material of matrix
Material.
Embodiment 3
Graphene aerogel matrix object the preparation method comprises the following steps:
(1) it takes graphene oxide 3:50 to be in mass ratio added in deionized water, adds 9 times of graphene oxide quality of polyethylene
Alcohol is cooled to room temperature in 150 DEG C of heat preservation 6h, cooled material is taken to wash through deionized water, obtain washings, is passed through argon gas protection, takes and wash
It washs object and is warming up to 800 DEG C of heat preservation 4h, be cooled to room temperature, obtain cooled material a；
(2) take cooled material a 3:20 in mass ratio that deionized water is added, ultrasonic disperse 40min adds cooled material a mass 5%
Pyrroles, ultrasonic 10min stand 5 days in 30 DEG C, obtain standing object, take and stand object 4:40 in mass ratio addition dehydrated alcohol, stand
Dehydrated alcohol is removed in 7h, filtering, repeats that dehydrated alcohol is added, stands process 8 times, filtering takes final filtration cakes torrefaction, obtains dried object；
(3) it takes dimethyl silicone polymer 3:20 in mass ratio that n-hexane is added, is stirred 40min in 30 DEG C, obtains mixed liquor, take
Mixed liquid dipping is added in dried object 3:100 in mass ratio, is prolonged stream naturally under 4 DEG C, vacuum condition and keeps 6h, filtered, taken out
Dried object is cooled to room temperature in 55 DEG C of heat preservation 12h to get graphene aerogel matrix object after immersion.
Energy storage activating agent the preparation method comprises the following steps:
S1. it takes 5- amino isophthalic acid 4:3:20 in mass ratio that sodium hydroxide, deionized water is added, is stirred in 4 DEG C
50min adds the sodium nitrite of 5- amino isophthalic acid quality 60%, is stirred 60min, obtains mixture, take mixture
It is to control time for adding 50min in 1mol/L hydrochloric acid, be stirred 3h in 3 DEG C, must stir that 4:9 in mass ratio, which is added dropwise to concentration,
Mixture；
S2. taking 3,5- dimethoxyaniline 5:30 in mass ratio that concentration is added is to be stirred in 1mol/L hydrochloric acid in 5 DEG C
40min adds the stirring mixture of 3 times of 3,5- dimethoxyaniline quality, adjusts pH to 7, argon gas protection is passed through, in 5 DEG C
3h is kept the temperature, is filtered, takes and filters slag through distillation water washing, vacuum drying obtains energy storage activating agent.
It is a kind of using graphene aerogel as the preparation method of the energy storage material of matrix, include the following steps:
It takes energy storage activating agent 5:0.5:60 in mass ratio that sodium nitrite, deionized water is added, is stirred 30min, obtains mixture
A, add deionized water quality 40% concentration be 1mol/L hydrochloric acid, be stirred 3h in 5 DEG C, obtain mixed liquor, take mixed liquor by
Mass ratio 50:4:100 is added graphene aerogel matrix object, deionized water and is stirred in 1 DEG C of heat preservation 5h then at 30 DEG C
18h, filtering, takes filter cake through deionized water, acetone washing, rotary evaporation is to get using graphene aerogel as the energy storage material of matrix
Material.
Comparative example 1: it is essentially identical with the preparation method of embodiment 3, it has only the difference is that lacking graphene aerogel matrix
Object.
Comparative example 2: it is essentially identical with the preparation method of embodiment 3, it has only the difference is that lacking energy storage activating agent.
Comparative example 3: the graphene aerogel of company of Wuhan City production is the energy storage material of matrix.
It is the energy storage material of matrix according to GB/T34336-017, GB/ by embodiment and comparative example gained graphene aerogel
T 22473-2008 standard is tested, and test result is as shown in table 1.
Table 1:
In summary, graphene aerogel of the invention is that the energy storage material of matrix is more preferable compared to commercial product effect, is worth
It widelys popularize.
Claims (7)
1. a kind of using graphene aerogel as the energy storage material of matrix, which is characterized in that including graphene aerogel matrix object, storage
It can activating agent；
The preparation method of the graphene aerogel matrix object, includes the following steps:
(1) it takes graphene oxide 1 ~ 3:30 in mass ratio ~ 50 to be added in deionized water, adds 6 ~ 9 times of graphene oxide quality
Polyvinyl alcohol, in 140 ~ 150 DEG C keep the temperature, be cooled to room temperature, cooled material taken to wash through deionized water, obtain washings, be passed through argon
Gas shielded takes washings to keep the temperature, and is cooled to room temperature, and obtains cooled material a；
(2) take cooled material a 1 ~ 3:10 in mass ratio ~ 20 that deionized water is added, ultrasonic disperse adds cooled material a mass 2 ~ 5%
Pyrroles, ultrasound stands 3 ~ 5 days in 25 ~ 30 DEG C, obtains standing object, takes and stands object 1 ~ 4:30 in mass ratio ~ 40 anhydrous second is added
Alcohol is stood, and dehydrated alcohol is removed in filtering, is repeated that dehydrated alcohol is added, is stood process 5 ~ 8 times, filtering takes final filtration cakes torrefaction, obtains
Dried object；
(3) it takes dimethyl silicone polymer 1 ~ 3:10 in mass ratio ~ 20 that n-hexane is added, is stirred, must mix in 25 ~ 30 DEG C
Liquid takes dried object 1 ~ 3:80 in mass ratio ~ 100 that mixed liquid dipping is added, and is prolonged stream injection naturally, and filtering is taken out and done after impregnating
Dry object is kept the temperature in 50 ~ 55 DEG C, is cooled to room temperature to get graphene aerogel matrix object.
2. according to claim 1 using graphene aerogel as the energy storage material of matrix, which is characterized in that the step
(1) heat-retaining condition of washings in are as follows: be warming up to 750 ~ 800 DEG C of 2 ~ 4h of heat preservation.
3. according to claim 1 using graphene aerogel as the energy storage material of matrix, which is characterized in that the step
(3) prolong the condition of stream injection in naturally are as follows: keep 4 ~ 6h in 2 ~ 4 DEG C, vacuum condition.
4. according to claim 1 using graphene aerogel as the energy storage material of matrix, which is characterized in that the energy storage is living
Property agent the preparation method comprises the following steps:
S1. it takes 5- amino isophthalic acid 2 ~ 4:1 in mass ratio ~ 3:10 ~ 20 that sodium hydroxide, deionized water is added, is stirred in 2 ~ 4 DEG C
Mixing is mixed, the sodium nitrite of 5- amino isophthalic acid quality 40 ~ 60% is added, is stirred, obtains mixture, take mixture
1 ~ 4:5 ~ 9 are added dropwise in hydrochloric acid in mass ratio, are controlled 30 ~ 50min of time for adding, are stirred, obtain stirring mixture；
S2. it takes 3,5- dimethoxyaniline, 1 ~ 5:20 in mass ratio ~ 30 to be added in hydrochloric acid, is stirred, adds in 2 ~ 5 DEG C
The stirring mixture of 3,5- 1 ~ 3 times of dimethoxyaniline quality adjusts pH to 6 ~ 7, is passed through argon gas protection, keeps the temperature in 2 ~ 5 DEG C,
It filters, takes and filter slag through distillation water washing, vacuum drying obtains energy storage activating agent.
5. according to claim 4 using graphene aerogel as the energy storage material of matrix, which is characterized in that the step S1
Middle stirring mixture is stirred condition are as follows: is stirred 1 ~ 3h in -2 ~ 3 DEG C.
6. it is a kind of as described in claim 1 ~ 5 any one using graphene aerogel as the preparation side of the energy storage material of matrix
Method, which is characterized in that the preparation method includes the following steps:
Take energy storage activating agent 1 ~ 5:0.2 in mass ratio ~ 0.5:50 ~ 60 that sodium nitrite, deionized water is added, it is stirred 20 ~
30min obtains mixture a, and the hydrochloric acid for adding deionized water quality 30 ~ 40% is stirred, and obtains mixed liquor, takes mixed liquor by matter
Graphene aerogel matrix object, deionized water is added than 40 ~ 50:1 ~ 4:80 ~ 100 in amount, in -4 ~ 1 DEG C of 2 ~ 5h of heat preservation, then at 25 ~
30 DEG C are stirred, and filtering takes filter cake through deionized water, acetone washing, rotary evaporation is to get using graphene aerogel as matrix
Energy storage material.
7. according to claim 6 using graphene aerogel as the preparation method of the energy storage material of matrix, which is characterized in that
The mixed liquor is stirred condition are as follows: is stirred 1 ~ 3h in 2 ~ 5 DEG C.
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