CN109265771A - A kind of graphene/Heveatex composite aerogel and preparation method thereof, application - Google Patents
A kind of graphene/Heveatex composite aerogel and preparation method thereof, application Download PDFInfo
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- CN109265771A CN109265771A CN201811063392.0A CN201811063392A CN109265771A CN 109265771 A CN109265771 A CN 109265771A CN 201811063392 A CN201811063392 A CN 201811063392A CN 109265771 A CN109265771 A CN 109265771A
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- graphene
- composite aerogel
- graphene oxide
- heveatex
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 221
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 204
- 239000004964 aerogel Substances 0.000 title claims abstract description 104
- 239000002131 composite material Substances 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 230000006835 compression Effects 0.000 claims abstract description 11
- 238000007906 compression Methods 0.000 claims abstract description 11
- 238000013329 compounding Methods 0.000 claims abstract description 6
- 239000004094 surface-active agent Substances 0.000 claims description 40
- 239000006185 dispersion Substances 0.000 claims description 37
- 239000003638 chemical reducing agent Substances 0.000 claims description 27
- 239000012190 activator Substances 0.000 claims description 26
- 239000000017 hydrogel Substances 0.000 claims description 25
- 238000007710 freezing Methods 0.000 claims description 22
- 230000008014 freezing Effects 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 18
- 239000000499 gel Substances 0.000 claims description 15
- 239000002904 solvent Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 238000005187 foaming Methods 0.000 claims description 13
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 12
- 239000013078 crystal Substances 0.000 claims description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- 238000006073 displacement reaction Methods 0.000 claims description 8
- 238000004073 vulcanization Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 239000011668 ascorbic acid Substances 0.000 claims description 5
- 235000010323 ascorbic acid Nutrition 0.000 claims description 5
- 229960005070 ascorbic acid Drugs 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 150000001336 alkenes Chemical class 0.000 claims description 4
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000292 calcium oxide Substances 0.000 claims description 4
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- 230000003213 activating effect Effects 0.000 claims description 3
- PGQAXGHQYGXVDC-UHFFFAOYSA-N dodecyl(dimethyl)azanium;chloride Chemical compound Cl.CCCCCCCCCCCCN(C)C PGQAXGHQYGXVDC-UHFFFAOYSA-N 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 235000011187 glycerol Nutrition 0.000 claims description 3
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 3
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 abstract description 6
- 239000010439 graphite Substances 0.000 description 18
- 229910002804 graphite Inorganic materials 0.000 description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 12
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 12
- 239000003292 glue Substances 0.000 description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000010790 dilution Methods 0.000 description 6
- 239000012895 dilution Substances 0.000 description 6
- 239000004816 latex Substances 0.000 description 6
- 229920000126 latex Polymers 0.000 description 6
- 239000007788 liquid Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000000502 dialysis Methods 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000005457 ice water Substances 0.000 description 4
- 239000000376 reactant Substances 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 3
- 238000013019 agitation Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 238000002242 deionisation method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- BVPWJMCABCPUQY-UHFFFAOYSA-N 4-amino-5-chloro-2-methoxy-N-[1-(phenylmethyl)-4-piperidinyl]benzamide Chemical compound COC1=CC(N)=C(Cl)C=C1C(=O)NC1CCN(CC=2C=CC=CC=2)CC1 BVPWJMCABCPUQY-UHFFFAOYSA-N 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- 206010000269 abscess Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000021615 conjugation Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000003916 ethylene diamine group Chemical group 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000693 micelle Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 150000003871 sulfonates Chemical class 0.000 description 1
- 238000000352 supercritical drying Methods 0.000 description 1
- 239000008399 tap water Substances 0.000 description 1
- 235000020679 tap water Nutrition 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/30—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by mixing gases into liquid compositions or plastisols, e.g. frothing with air
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
- C08J2201/0484—Elimination of a frozen liquid phase the liquid phase being aqueous
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2307/00—Characterised by the use of natural rubber
- C08J2307/02—Latex
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
Abstract
The present embodiments relate to the technical fields of aeroge and preparation method thereof, and in particular to a kind of graphene/Heveatex composite aerogel and preparation method thereof, application.Graphene provided in an embodiment of the present invention/Heveatex composite aerogel, by include following components raw material be prepared: graphene oxide, pre-vulcanized natural latex and it is at least one prepare composite aerogel needed for compounding agent.In the present invention, it is for the first time that graphene and Heveatex is compound, tear resistance and the excellent, ultralight graphene/Heveatex composite aerogel of flexibility has been made, overcome the disadvantage that simple graphene aerogel tear resistance in the prior art is poor, compression rubbing is scaling-off, and the graphene/Heveatex composite aerogel is manufactured under normal pressure, preparation method is simple, low in cost.
Description
Technical field
The present invention relates to the technical fields of aeroge and preparation method thereof, and in particular to a kind of graphene/Heveatex is multiple
Close aeroge and preparation method thereof, application.
Background technique
Aeroge is the material that air is dispersed in the three-dimensional porous shape structure formed in solid dielectric, in which: graphene
Aeroge is a kind of aeroge using graphene sheet layer as three-dimensional net structure.Graphene aerogel has both aeroge and graphite
The characteristics of both alkene, has the electric conductivity of superelevation, the thermal conductivity of superelevation and surpasses while keeping low-density, high-specific surface area
High mechanical strength.
Using hydrophilic graphene oxide as raw material, it is set to be self-assembled into three-dimensional water-setting by the method for sol-gel
Glue, then supercritical drying or freeze-drying are carried out, it is the regular course for preparing graphene aerogel.It can also adopt in the prior art
Acquisition graphene aerogel is dried to graphene hydrogel with atmosphere pressure desiccation, technique is simpler, price is lower
It is honest and clean, but the graphene aerogel of atmosphere pressure desiccation preparation, density is larger, and tear resistance and flexibility are poor.
The bubble that Chinese invention CN106517160A is formed using lauryl sodium sulfate is prepared as template by constant pressure and dry
Ultralight graphene aerogel is gone out, but obtained aeroge is stacked by single graphene sheet layer by conjugation
At so that its tear resistance is poor, Repeated Compression kneading will appear scaling-off phenomenon afterwards several times.
The information disclosed in the background technology section is intended only to increase the understanding to general background of the invention, without answering
When being considered as recognizing or imply that the information constitutes the prior art already known to those of ordinary skill in the art in any form.
Summary of the invention
Goal of the invention
To solve the above problems, the purpose of the present invention is to provide a kind of graphene/Heveatex composite aerogel and its
Preparation method, application.It is for the first time that graphene and Heveatex is compound in the present invention, tear resistance has been made and flexibility is excellent
Different, ultralight graphene/Heveatex composite aerogel overcomes simple graphene aerogel tear resistance in the prior art
Energy is poor, scaling-off disadvantage is rubbed in compression, and the graphene/Heveatex composite aerogel is manufactured under normal pressure,
Preparation method is simple, low in cost.
Solution
Purpose to realize the present invention, the embodiment of the invention provides a kind of graphene/Heveatex composite aerogels, by wrapping
The raw material for including following components is prepared: graphene oxide, pre-vulcanized natural latex and at least one prepare composite aerogel institute
The compounding agent needed.
In one possible implementation, the compounding agent includes table to above-mentioned graphene/Heveatex composite aerogel
At least one of face activating agent, activator or reducing agent.
Above-mentioned graphene/Heveatex composite aerogel in one possible implementation, by including following components
Raw material is prepared: graphene oxide, pre-vulcanized natural latex, surfactant, activator and reducing agent.
Above-mentioned graphene/Heveatex composite aerogel in one possible implementation, the mesh number of graphene oxide
For 32-1000 mesh, it is optionally 100-500 mesh, is still optionally further 180 mesh.
Above-mentioned graphene/Heveatex composite aerogel in one possible implementation, pre-vulcanized natural latex
State of cure (vulcanization) is two first-four ends.At the beginning of two first-four ends include: two, in two, two is last, and at the beginning of three, in three, three is last, and at the beginning of four, four neutralize four
End.At the beginning of two, gel is in dough, can be drawn very long and with toughness.In two, gel is in dough, and certain degree can be drawn continuous.Two
End, gel are in dough, are slightly elongated i.e. disconnected but tougher.At the beginning of three, gel is in dough, disconnected once drawing, but micelle is more fine and smooth.
In three, gel is in granular form, and surface is rougher.Three ends, gel is in granular form, and can pinch agglomerating, and after pressure is removed, gel is significant
It shrinks.At the beginning of four, gel is in granular form, and can pinch agglomerating, but particle and conglomeration are rougher, after pressure is removed, slightly shrink.Four
In, gel is in granular form, and is not easy agglomerating, there is trend fine crushing, ungauged regions phenomenon.Four ends, gel is all in nano sized particles state.
In one possible implementation, surfactant includes ten to above-mentioned graphene/Heveatex composite aerogel
At least one of dialkyl sulfonates, dodecyl dimethyl ammonium chloride, polyvinyl alcohol.
Above-mentioned graphene/Heveatex composite aerogel in one possible implementation, activator include zinc oxide,
At least one of frerrous chloride, calcium oxide.
In one possible implementation, reducing agent includes Vitamin C to above-mentioned graphene/Heveatex composite aerogel
At least one of acid, hydrazine hydrate, ethylenediamine, sodium borohydride.
In one possible implementation, graphene oxide is with moisture for above-mentioned graphene/Heveatex composite aerogel
Dispersion liquid form is added；Optionally, the concentration of graphene oxide aqueous dispersions is 4-7mg/mL.
In one possible implementation, graphene oxide is above-mentioned graphene/Heveatex composite aerogel
The graphene oxide that Hummers method or improved Hummers method are prepared.
Above-mentioned graphene/Heveatex composite aerogel in one possible implementation, improved Hummers legal system
The preparation method of standby obtained graphene oxide includes the following steps:
By graphite, the concentrated sulfuric acid, KMnO4It is freezed under the conditions of -25 DEG C；Reaction vessel is placed in ice-water bath, toward reaction
Graphite, the concentrated sulfuric acid and the KMnO by freezing are added in container4, 1-6h is reacted under the conditions of 0-5 DEG C；It is warming up to 40-60 DEG C, instead
Answer 3-10h；Then reactant is poured into deionized water, concentrated hydrochloric acid and hydrogen peroxide is added；It is centrifugally separating to obtain thick liquid
Body, dialysis to pH value are 4-6, obtain graphene oxide aqueous dispersions.
Above-mentioned graphene/Heveatex composite aerogel in one possible implementation,
And/or the additional amount of the concentrated sulfuric acid is 400-800mL in every 10g graphite；
And/or KMnO in every 10g graphite4Additional amount be 20-40g；
And/or the additional amount of concentrated hydrochloric acid is 400-700mL in every 10g graphite；
And/or the additional amount of hydrogen peroxide is 10-30mL in every 10g graphite；
And/or the mass fraction of the concentrated sulfuric acid is 98%；
And/or the mass fraction of the concentrated hydrochloric acid is 36.0-38.0%；
And/or the mass fraction of the hydrogen peroxide is 25-35%.
Above-mentioned graphene/Heveatex composite aerogel in one possible implementation, pre-vulcanized natural latex with
The mass ratio of graphene oxide is 0.1-1: 1.
Above-mentioned graphene/Heveatex composite aerogel in one possible implementation, graphene oxide and surface
The mass ratio of activating agent is (24-42): (20-100)；Optionally, the surfactant is with the surface-active of 40-50mg/mL
Agent solution form is added.
Above-mentioned graphene/Heveatex composite aerogel in one possible implementation, reducing agent and graphite oxide
The mass ratio of alkene is 1-2: 1.
Above-mentioned graphene/Heveatex composite aerogel in one possible implementation, activator and presulfurization day
The mass ratio of right latex is 0.0005-0.01: 1.
The embodiment of the invention also provides a kind of preparation methods of above-mentioned graphene/Heveatex composite aerogel, including
Following step: using include graphene oxide, pre-vulcanized natural latex and it is at least one prepare composite aerogel needed for cooperation
The raw material of agent prepares graphene/Heveatex composite aerogel.
In one possible implementation, the preparation method includes the following steps: above-mentioned preparation method
Pre-vulcanized natural latex, surfactant, activator is added according to the ratio in graphene oxide aqueous dispersions and goes back
Former agent, mixes foaming, and prereduction forms hydrogel；
It will be heat-treated again after hydrogel obtained freezing；
Solvent displacement；
Constant pressure and dry.
In one possible implementation, the mixing foaming step includes: mixed at the low rotational speed to above-mentioned preparation method
It is even, revolving speed foaming is improved, the slow-speed of revolution is 100-800r/min, and the high revolving speed is 1500-2500r/min.
In one possible implementation, pre-reduction procedure includes: to restore under the conditions of 50-90 DEG C to above-mentioned preparation method
60-120min。
In one possible implementation, freezing step includes: cold under the conditions of -10~-30 DEG C to above-mentioned preparation method
Freeze 4-12h；Freezing can be such that ice crystal sufficiently grows in graphene oxide hydrogel.
In one possible implementation, thermal reduction step includes: hot under the conditions of 50-90 DEG C goes back to above-mentioned preparation method
Former 4-10h.
In one possible implementation, solvent swap step includes: with displacement solvent displacement 2-5 to above-mentioned preparation method
It is secondary.
In one possible implementation, the displacement solvent includes methanol, ethyl alcohol, in glycerine to above-mentioned preparation method
At least one.
In one possible implementation, constant pressure and dry step includes: to do under the conditions of 40-80 DEG C to above-mentioned preparation method
Dry 8-24h.
The embodiment of the invention also provides a kind of application of graphene/Heveatex composite aerogel in processing greasy dirt.
The embodiment of the invention also provides a kind of graphene/Heveatex composite aerogels in preparing compression rebound material
Application.
The embodiment of the invention also provides a kind of graphene/Heveatex composite aerogels to rub not scaling-off airsetting in preparation
Application in glue material.
Beneficial effect
(1) multiple using Heveatex for the first time in the graphene provided in the embodiment of the present invention/Heveatex composite aerogel
It closes graphene and elastomeric graphene aerogel is prepared, compared with simple graphene aerogel, the embodiment of the present invention is provided
Graphene/Heveatex composite aerogel have superior tear resistance and flexibility, overcome before simple graphite
Scaling-off disadvantage is rubbed in the compression of alkene aeroge.
(2) in the graphene provided in the embodiment of the present invention/Heveatex composite aerogel, with ice crystal and surfactant
The abscess of formation is double-template, combines green foaming and (promotes surfactant to coat air foaming by machinery mixing, do not produce
Raw waste, free from environmental pollution) and constant pressure and dry technology, so that the compound gas of graphene/natural emulsion provided in an embodiment of the present invention
Gel can be manufactured under normal pressure, simple process and low cost, can industrialized production.
(3) in the graphene provided in the embodiment of the present invention/Heveatex composite aerogel, there is preferable mechanicalness
Can, it can reach 90% compression reaction performance.
(4) in the graphene provided in the embodiment of the present invention/Heveatex composite aerogel, the property with oleophilic drainage
Matter can be used to handle greasy dirt；And it due to the property of its compressible rebound, may be reused.
(5) in the graphene provided in the embodiment of the present invention/Heveatex composite aerogel, have processable well
Property, it can be prepared into various shape.
(6) in the graphene provided in the embodiment of the present invention/Heveatex composite aerogel, the addition of activator can be more
Cooperate the effect of Heveatex well.
Detailed description of the invention
One or more embodiments are illustrated by the picture in corresponding attached drawing, these exemplary theorys
The bright restriction not constituted to embodiment.Dedicated word " exemplary " means " being used as example, embodiment or illustrative " herein.
Here as any embodiment illustrated by " exemplary " should not necessarily be construed as preferred or advantageous over other embodiments.
Figure 1A and Figure 1B is the obtained graphene of the embodiment of the present invention 1/Heveatex composite aerogel scanning electron microscope
Figure.
Fig. 2 is that the obtained graphene of the embodiment of the present invention 3/Heveatex composite aerogel is processed into reality of various shapes
Object figure.
Fig. 3 is graphene/Heveatex composite aerogel compression reaction process schematic in effect example 1 of the present invention.
Fig. 4 is graphene/Heveatex composite aerogel oil absorbency schematic diagram in effect example 2 of the present invention.
Fig. 5 is graphene/Heveatex composite aerogel and the graphene airsetting for being not added with latex in effect example 3 of the present invention
Scaling-off comparison diagram after glue laminated contracting rubbing.
Specific embodiment
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described, it is clear that described embodiments are some of the embodiments of the present invention, rather than
Whole embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work premise
Under every other embodiment obtained, shall fall within the protection scope of the present invention.Unless otherwise explicitly stated, otherwise whole
In a specification and claims, it is to include that the term " include " or its transformations will be understood as
The element or component stated, and do not exclude other elements or other components.
In addition, in order to better illustrate the present invention, numerous details is given in specific embodiment below.
It will be appreciated by those skilled in the art that without certain details, the present invention equally be can be implemented.In some embodiments, right
It is not described in detail in raw material well known to those skilled in the art, element, method, means etc., in order to highlight master of the invention
Purport.
Embodiment 1
A kind of graphene/Heveatex composite aerogel is prepared by the raw material for including following components:
Graphene oxide, pre-vulcanized natural latex, surfactant, activator and reducing agent.
Wherein, graphene oxide be carried out with graphene oxide aqueous dispersions made from improved Hummers method using,
Mesh number be 180 mesh, preparation step the following steps are included:
Weigh graphite, the 600mL concentrated sulfuric acid (mass fraction 98%), 30g KMnO of 180 mesh of 10g4In -25 DEG C of conditions
The graphite by freezing is added into the reaction vessel for be placed in ice-water bath, and is poured slowly into the dense sulphur by freezing by lower freezing 2h
Acid stirs evenly graphite and the concentrated sulfuric acid, is then slowly added to KMnO in the case where magnetic agitation4, reacted under the conditions of 4 DEG C
Then 2h is slowly warming up to 50 DEG C, react 6h；Then reactant is poured slowly into preprepared and fills 1200mL deionization
In the large beaker of water；Then the hydrogen peroxide of 500mL concentrated hydrochloric acid (mass fraction 37%) and 20mL is added, and (mass fraction is
30%) it, is stirred evenly with glass bar；It is finally centrifuged repeatedly to obtain thick liquid, dialysis to pH with the method for centrifuge separation
Value is 6, obtains the aqueous dispersions of the graphene oxide of 180 mesh, adjusts the concentration of graphene oxide aqueous dispersions extremely by dilution
5mg/mL。
At the beginning of the state of cure (vulcanization) of pre-vulcanized natural latex is two, the mass ratio with graphene oxide is 1: 1.
Surfactant is dodecyl sodium sulfate, and 1mL concentration is added in every 6mL graphene oxide aqueous dispersions and is
The mass ratio of the surfactant of 45mg/mL, i.e. graphene oxide and surfactant is 30: 45.
Activator is zinc oxide, and the mass ratio with pre-vulcanized natural latex is 0.01: 1.
Reducing agent is ascorbic acid, and the mass ratio with graphene oxide is 2: 1.
The graphene of above-mentioned formula/Heveatex composite aerogel preparation method includes the following steps:
(1) it takes graphene oxide aqueous dispersions in cylindrical vial, is added in graphene oxide aqueous dispersions
Surfactant, reducing agent, pre-vulcanized natural latex and the activator of said ratio are uniformly mixed under 100r/min revolving speed
Afterwards, revolving speed is improved to 2000r/min foaming；
(2) system made from step (1) is put into baking oven, prereduction 120min under conditions of 50 DEG C, forms water-setting
Glue；
(3) hydrogel made from step (2) is put into refrigerator and carries out freezing 4h under conditions of -10 DEG C, ice crystal is made to exist
It is sufficiently grown in graphene oxide hydrogel；
(4) hydrogel made from step (3) is heated to reduction 4h under conditions of 50 DEG C, is used after being taken out in baking oven later
Methanol impregnates 2 times and is put into 40 DEG C of dry 8h in baking oven to replace after solvent and obtains graphene/Heveatex composite aerogel；It obtains
Graphene/Heveatex composite aerogel scanning electron microscope (SEM) photograph see Figure 1A and Figure 1B.
Embodiment 2
A kind of graphene/Heveatex composite aerogel is prepared by the raw material for including following components:
Graphene oxide, pre-vulcanized natural latex, surfactant, activator and reducing agent.
Wherein, graphene oxide is made by improved Hummers method, and mesh number is 180 mesh, preparation step with embodiment 1,
By the concentration of dilution adjustment graphene oxide aqueous dispersions to 5mg/mL.
At the beginning of the state of cure (vulcanization) of pre-vulcanized natural latex is three, the mass ratio with graphene oxide is 1: 1.
Surfactant is dodecyl sodium sulfate, and 2mL concentration is added in every 6mL graphene oxide aqueous dispersions and is
The mass ratio of the surfactant of 45mg/mL, i.e. graphene oxide and surfactant is 30: 90.
Activator is zinc oxide, and the mass ratio with pre-vulcanized natural latex is 0.01: 1.
Reducing agent is ascorbic acid, and the mass ratio with graphene oxide is 2: 1.
The graphene of above-mentioned formula/Heveatex composite aerogel preparation method includes the following steps:
(1) it takes graphene oxide aqueous dispersions in cylindrical vial, is added in graphene oxide aqueous dispersions
Surfactant, reducing agent, pre-vulcanized natural latex and the activator of said ratio are uniformly mixed under 100r/min revolving speed
Afterwards, revolving speed is improved to 2000r/min foaming；
(2) system made from step (1) is put into baking oven, prereduction 120min under conditions of 50 DEG C, forms water-setting
Glue；
(3) hydrogel made from step (2) is put into refrigerator and carries out freezing 4h under conditions of -10 DEG C, ice crystal is made to exist
It is sufficiently grown in graphene oxide hydrogel；
(4) hydrogel made from step (3) is heated to reduction 4h under conditions of 50 DEG C, is used after being taken out in baking oven later
Methanol impregnates 2 times and is put into 40 DEG C of dry 8h in baking oven to replace after solvent and obtains graphene/Heveatex composite aerogel.
Embodiment 3
A kind of graphene/Heveatex composite aerogel is prepared by the raw material for including following components:
Graphene oxide, pre-vulcanized natural latex, surfactant, activator and reducing agent.
Wherein, graphene oxide is made by improved Hummers method, and mesh number is 180 mesh, preparation step with embodiment 1,
By the concentration of dilution adjustment graphene oxide aqueous dispersions to 5mg/mL.
At the beginning of the state of cure (vulcanization) of pre-vulcanized natural latex is two, the mass ratio with graphene oxide is 1: 1.
Surfactant is polyvinyl alcohol, and it is 45mg/mL's that 1mL concentration is added in every 6mL graphene oxide aqueous dispersions
The mass ratio of surfactant, i.e. graphene oxide and surfactant is 30: 45.
Activator is calcium oxide, and the mass ratio with pre-vulcanized natural latex is 0.01: 1.
Reducing agent is ascorbic acid, and the mass ratio with graphene oxide is 2: 1.
The graphene of above-mentioned formula/Heveatex composite aerogel preparation method includes the following steps:
(1) it takes graphene oxide aqueous dispersions in cylindrical vial, is added in graphene oxide aqueous dispersions
Surfactant, reducing agent, pre-vulcanized natural latex and the activator of said ratio are uniformly mixed under 100r/min revolving speed
Afterwards, revolving speed is improved to 2000r/min foaming；
(2) system made from step (1) is put into baking oven, prereduction 60min under conditions of 50 DEG C, forms water-setting
Glue；
(3) hydrogel made from step (2) is put into refrigerator and carries out freezing 4h under conditions of -10 DEG C, ice crystal is made to exist
It is sufficiently grown in graphene oxide hydrogel；
(4) hydrogel made from step (3) is heated to reduction 4h under conditions of 50 DEG C, is used after being taken out in baking oven later
Methanol impregnates 2 times and is put into 40 DEG C of dry 8h in baking oven to replace after solvent and obtains graphene/Heveatex composite aerogel；
The graphene being prepared/Heveatex composite aerogel is processed into various shape, pictorial diagram is shown in Fig. 2.
Embodiment 4
A kind of graphene/Heveatex composite aerogel is prepared by the raw material for including following components:
Graphene oxide, pre-vulcanized natural latex, surfactant, activator and reducing agent.
Wherein, graphene oxide be carried out with graphene oxide aqueous dispersions made from improved Hummers method using,
Mesh number be 100 mesh, preparation step the following steps are included:
Weigh graphite, the 400mL concentrated sulfuric acid (mass fraction 98%), 20g KMnO of 100 mesh of 10g4In -25 DEG C of conditions
The graphite by freezing is added into the reaction vessel for be placed in ice-water bath, and is poured slowly into the dense sulphur by freezing by lower freezing 4h
Acid stirs evenly graphite and the concentrated sulfuric acid, is then slowly added to KMnO in the case where magnetic agitation4, reacted under the conditions of 0 DEG C
Then 1h is slowly warming up to 40 DEG C, react 3h；Then reactant is poured slowly into preprepared and fills 1200mL deionization
In the large beaker of water；Then the hydrogen peroxide of 400mL concentrated hydrochloric acid (mass fraction 36%) and 10mL is added, and (mass fraction is
25%) it, is stirred evenly with glass bar；It is finally centrifuged repeatedly to obtain thick liquid, dialysis to pH with the method for centrifuge separation
Value is 5, obtains the aqueous dispersions of the graphene oxide of 100 mesh, adjusts the concentration of graphene oxide aqueous dispersions extremely by dilution
4mg/mL。
The state of cure (vulcanization) of pre-vulcanized natural latex is four ends, and the mass ratio with graphene oxide is 0.1: 1.
Surfactant is dodecyl dimethyl ammonium chloride, and it is dense that 0.5mL is added in every 6mL graphene oxide aqueous dispersions
Degree is the surfactant of 45mg/mL, i.e., the mass ratio of graphene oxide and surfactant is 24: 22.5.
Activator is frerrous chloride, and the mass ratio with pre-vulcanized natural latex is 0.0005: 1.
Reducing agent is hydrazine hydrate, and the mass ratio with graphene oxide is 1: 1.
The graphene of above-mentioned formula/Heveatex composite aerogel preparation method includes the following steps:
(1) it takes graphene oxide aqueous dispersions in cylindrical vial, is added in graphene oxide aqueous dispersions
Surfactant, reducing agent, pre-vulcanized natural latex and the activator of said ratio are uniformly mixed under 800r/min revolving speed
Afterwards, revolving speed is improved to 2500r/min foaming；
(2) system made from step (1) is put into baking oven, prereduction 120min under conditions of 90 DEG C, forms water-setting
Glue；
(3) hydrogel made from step (2) is put into refrigerator and carries out freezing 12h under conditions of -30 DEG C, ice crystal is made to exist
It is sufficiently grown in graphene oxide hydrogel；
(4) hydrogel made from step (3) is heated to reduction 5h under conditions of 90 DEG C, is used after being taken out in baking oven later
Ethyl alcohol impregnates 2 times and is put into 80 DEG C of dryings in baking oven to replace after solvent and obtains graphene/Heveatex composite aerogel for 24 hours.
Embodiment 5
A kind of graphene/Heveatex composite aerogel is prepared by the raw material for including following components:
Graphene oxide, pre-vulcanized natural latex, surfactant, activator and reducing agent.
Wherein, graphene oxide be carried out with graphene oxide aqueous dispersions made from improved Hummers method using,
Mesh number be 500 mesh, preparation step the following steps are included:
Weigh graphite, the 800mL concentrated sulfuric acid (mass fraction 98%), 40g KMnO of 500 mesh of 10g4In -25 DEG C of conditions
The graphite by freezing is added into the reaction vessel for be placed in ice-water bath, and is poured slowly into the dense sulphur by freezing by lower freezing 3h
Acid stirs evenly graphite and the concentrated sulfuric acid, is then slowly added to KMnO in the case where magnetic agitation4, reacted under the conditions of 5 DEG C
Then 6h is slowly warming up to 60 DEG C, react 10h；Then by reactant be poured slowly into preprepared fill 1200mL go from
In the large beaker of sub- water；Then the hydrogen peroxide of 700mL concentrated hydrochloric acid (mass fraction 38%) and 30mL is added, and (mass fraction is
35%) it, is stirred evenly with glass bar；It is finally centrifuged repeatedly to obtain thick liquid, dialysis to pH with the method for centrifuge separation
Value is 5, obtains the aqueous dispersions of the graphene oxide of 500 mesh, adjusts the concentration of graphene oxide aqueous dispersions extremely by dilution
7mg/mL。
The state of cure (vulcanization) of pre-vulcanized natural latex is that the mass ratio in three, with graphene oxide is 0.5: 1.
Surfactant is polyvinyl alcohol, and it is 45mg/mL's that 1mL concentration is added in every 6mL graphene oxide aqueous dispersions
The mass ratio of surfactant, i.e. graphene oxide and surfactant is 42: 45.
Activator is calcium oxide, and the mass ratio with pre-vulcanized natural latex is 0.005: 1.
Reducing agent is ethylenediamine, and the mass ratio with graphene oxide is 1.5: 1.
The graphene of above-mentioned formula/Heveatex composite aerogel preparation method includes the following steps:
(1) it takes graphene oxide aqueous dispersions in cylindrical vial, is added in graphene oxide aqueous dispersions
Surfactant, reducing agent, pre-vulcanized natural latex and the activator of said ratio are uniformly mixed under 600r/min revolving speed
Afterwards, revolving speed is improved to 2000r/min foaming；
(2) system made from step (1) is put into baking oven, prereduction 100min under conditions of 70 DEG C, forms water-setting
Glue；
(3) hydrogel made from step (2) is put into refrigerator and carries out freezing 8h under conditions of -20 DEG C, ice crystal is made to exist
It is sufficiently grown in graphene oxide hydrogel；
(4) hydrogel made from step (3) is heated to reduction 8h under conditions of 70 DEG C, is used after being taken out in baking oven later
Glycerine impregnates 2 times and is put into 60 DEG C of dry 18h in baking oven to replace after solvent and obtains graphene/Heveatex composite aerogel.
Comparative example 1
A kind of graphene aerogel being not added with latex is prepared by the raw material for including following components:
Graphene oxide, surfactant and reducing agent.
Wherein, graphene oxide is made by improved Hummers method, and mesh number is 180 mesh, preparation step with embodiment 1,
By the concentration of dilution adjustment graphene oxide aqueous dispersions to 5mg/mL.
Surfactant is polyvinyl alcohol, and it is 45mg/mL's that 1mL concentration is added in every 6mL graphene oxide aqueous dispersions
Surfactant.
Reducing agent is ascorbic acid, and the mass ratio with graphene oxide is 2: 1.
The preparation method of the graphene aerogel of above-mentioned formula includes the following steps:
(1) it takes graphene oxide aqueous dispersions in cylindrical vial, is added in graphene oxide aqueous dispersions
Surfactant, the reducing agent of said ratio under 100r/min revolving speed after mixing improve revolving speed to 2000r/min hair
Bubble；
(2) system made from step (1) is put into baking oven, 60min is restored under conditions of 50 DEG C, form hydrogel；
(3) hydrogel made from step (2) is put into refrigerator and carries out freezing 4h under conditions of -10 DEG C, ice crystal is made to exist
It is sufficiently grown in graphene oxide hydrogel；
(4) hydrogel made from step (3) is heated to reduction 4h under conditions of 50 DEG C, is used after being taken out in baking oven later
Methanol impregnates 2 times and is put into 40 DEG C of dry 8h in baking oven to replace after solvent and obtains graphene aerogel.
Effect example 1
The compression reaction performance test of graphene/Heveatex composite aerogel
The counterweight of 500g is placed on thereon, uses by the graphene that Example 2 is prepared/Heveatex composite aerogel
Steel ruler measures graphene/Heveatex composite aerogel elemental height, graphene/Heveatex composite aerogel height after compression
With remove graphene/Heveatex composite aerogel height after load, whole experiment process is as shown in Figure 3.
Experimental result: graphene/Heveatex composite aerogel elemental height is 22.0mm, and counterweight is placed on aeroge
Afterwards, graphene/Heveatex composite aerogel height is about 2.2mm, after removing load, the compound gas of graphene/Heveatex
Gel Height is 21.5mm；It is iteratively repeated 10 times, graphene/Heveatex composite aerogel height is maintained at after removing load
21.5mm or so.
Effect example 2
The test of graphene/Heveatex composite aerogel oil absorbency
The graphene that Example 2 is prepared/Heveatex composite aerogel uses the silicone oil dyed with the Sudan three
4 drop of test tube drop of 3mL is in the glass culture dish for filling tap water；Graphene/Heveatex composite aerogel is clamped with tweezers
It is moved on the water surface of oil-containing.Experimental result is as shown in figure 4, when graphene/Heveatex composite aerogel contacts oily phase, oily phase
It is absorbed (transient absorption illustrates that aeroge oil absorption is very strong) rapidly；And water cannot suck the compound gas of graphene/Heveatex
In gel.
Effect example 3
Graphene/Heveatex composite aerogel compression rubbing test
The graphene that Example 1 is prepared/Heveatex composite aerogel and the graphene airsetting for being not added with latex
Glue；An A4 paper is put on experimental bench, by graphene/Heveatex composite aerogel that embodiment 1 is prepared and is not added with
The graphene aerogel of latex is put into centre of the palm hand (in the centre of the palm, hand touches aeroge and applies a small power aeroge) rubbing
10 times, observe scaling-off quantity.Experimental result is as shown in figure 5, the compound airsetting of graphene/Heveatex that embodiment 1 is prepared
Glue is not scaling-off, is not added with about 20 pieces of size clast that the graphene aerogel of latex falls.
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of graphene/Heveatex composite aerogel is prepared by the raw material for including following components: graphene oxide,
Pre-vulcanized natural latex and it is at least one prepare composite aerogel needed for compounding agent.
2. graphene according to claim 1/Heveatex composite aerogel, it is characterised in that: the compounding agent includes
At least one of surfactant, activator or reducing agent.
3. graphene according to claim 1/Heveatex composite aerogel, it is characterised in that: by including following components
Raw material be prepared: graphene oxide, pre-vulcanized natural latex, surfactant, activator and reducing agent.
4. graphene according to claim 1-3/Heveatex composite aerogel, it is characterised in that: oxidation stone
The mesh number of black alkene is 32-1000 mesh, is optionally 100-500 mesh, is still optionally further 180 mesh；
And/or graphene oxide is added with aqueous dispersion, optionally, the concentration of graphene oxide aqueous dispersions is 4-
7mg/mL；
And/or graphene oxide is the graphene oxide that Hummers method or improved Hummers method are prepared；
And/or the state of cure (vulcanization) of pre-vulcanized natural latex is two first-four ends；
And/or the mass ratio of pre-vulcanized natural latex and graphene oxide is 0.1-1: 1.
5. graphene according to claim 3/Heveatex composite aerogel, it is characterised in that: surfactant includes
At least one of dodecyl sodium sulfate, dodecyl dimethyl ammonium chloride, polyvinyl alcohol；
And/or activator includes at least one of zinc oxide, frerrous chloride, calcium oxide；
And/or reducing agent includes at least one of ascorbic acid, hydrazine hydrate, ethylenediamine, sodium borohydride.
6. graphene according to claim 3/Heveatex composite aerogel, it is characterised in that: graphene oxide and table
The mass ratio of face activating agent is (24-42): (20-100)；Optionally, the surfactant is living with the surface of 40-50mg/mL
Property agent solution form be added；
And/or the mass ratio of reducing agent and graphene oxide is 1-2: 1；
And/or the mass ratio of activator and pre-vulcanized natural latex is 0.0005-0.01: 1.
7. graphene described in any one of claims 1-6/Heveatex composite aerogel preparation method, including following steps
It is rapid: using include graphene oxide, pre-vulcanized natural latex and it is at least one prepare composite aerogel needed for compounding agent original
Material prepares graphene/Heveatex composite aerogel.
8. preparation method according to claim 7, it is characterised in that: the preparation method includes the following steps:
Pre-vulcanized natural latex, surfactant, activator and reducing agent is added according to the ratio in graphene oxide aqueous dispersions,
Foaming is mixed, prereduction forms hydrogel；It will be heat-treated again after hydrogel obtained freezing；Solvent displacement；Constant pressure and dry.
9. preparation method according to claim 8, it is characterised in that: the mixing foaming step includes: at the low rotational speed
It mixes, improves revolving speed foaming, the slow-speed of revolution is 100-800r/min, and the high revolving speed is 1500-2500r/min；
And/or pre-reduction procedure includes: to restore 60-120min under the conditions of 50-90 DEG C；
And/or freezing step includes: to freeze 4-12h under the conditions of -10~-30 DEG C；Freezing can make ice crystal in graphene oxide water
It is sufficiently grown in gel；
And/or thermal reduction step includes: to heat-treat 4-10h under the conditions of 50-90 DEG C；
And/or solvent swap step includes: with displacement solvent displacement 2-5 times；
And/or the solvent displacement solvent for use includes at least one of methanol, ethyl alcohol, glycerine；
And/or constant pressure and dry step includes: dry 8-24h under the conditions of 40-80 DEG C.
10. graphene described in any one of claims 1-6/any one of Heveatex composite aerogel and claim 7-9 institute
The graphene that the preparation method stated is prepared/Heveatex composite aerogel processing greasy dirt, prepare compression rebound material or
The application in not scaling-off aerogel material is rubbed in preparation.
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