CN108630352A - Nano-cellulose up-stripping graphene and the method for preparing high heat-conductivity conducting film - Google Patents
Nano-cellulose up-stripping graphene and the method for preparing high heat-conductivity conducting film Download PDFInfo
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- CN108630352A CN108630352A CN201810345144.9A CN201810345144A CN108630352A CN 108630352 A CN108630352 A CN 108630352A CN 201810345144 A CN201810345144 A CN 201810345144A CN 108630352 A CN108630352 A CN 108630352A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/16—Non-insulated conductors or conductive bodies characterised by their form comprising conductive material in insulating or poorly conductive material, e.g. conductive rubber
Abstract
The invention discloses a kind of nano-cellulose up-stripping graphene and the methods that prepare high heat-conductivity conducting film, it is by adding few layer graphene or multi-layer graphene in the nanofiber dispersion liquid to TEMPO mediated oxidatives, it is uniformly mixed under the action of lasting shear agitation, then it dries and is molded after mixture being filtered removal filtrate, you can obtain high heat-conductivity conducting film.Grapheme material produced by the present invention has dispersion level high, and thermal conductivity is good, and the feature that preparation process environmental pollution is small.
Description
Technical field
The present invention relates to a kind of preparation method of high heat-conductivity conducting film, especially a kind of nano-cellulose up-stripping stone
Black alkene and the method for preparing high heat-conductivity conducting film.
Background technology
The single layer original graphite alkene prepared by " from top to bottom " mode is used as the first two-dimentional material that people study extensively
Material, has outstanding physical property and wide application prospect.Graphene is the material that known heat conductivility is best in the world,
Intrinsic thermal conductivity is up to 5300W/mK；The same outstanding carrier mobility 200000cm for also having its superelevation2/（vs）And it reaches
To the Young's modulus of 1.06Tpa.However, the preparation of this graphene, transfer and dispersion technology be always lie across in researcher and
Problem in face of enterprise technology personnel.
The height of graphene dispersion level directly affects the key performance of final products, includes being widely used so far
Oxidation of precursor object method, surfactant is covalent modified, foreign atom, exchange of solvent, metal nanoparticles loaded equal very much
Method is suggested to realize the monodisperse and functionalization of graphene.The final dispersion effect of these methods is simultaneously not fully up to expectations,
To also the intrinsic physical property of graphene be influenced by introducing third component, and will cause more environmental pollutions, and can be realized
The example that graphene effectively disperses in water is even more rare, thus limit graphene processing method towards green direction hair
Exhibition.
Nano-cellulose is as natural biomass resource, and environmental-friendly renewable, reserves are very huge.With nanofiber
Functional film material prepared by element has more tough mechanical performance, lower density, lower coefficient of thermal expansion and long-term ruler
Very little stability, future are expected to be widely used as the excellent base material of electronic device.
In view of the huge applications potentiality of graphene and nano-cellulose composite material, we explore it is a kind of very efficiently just
Prompt graphene dispersion, the method for then preparing nano-cellulose graphene composite film, this method are equally applicable to multilayer
The stripping of graphene removes dispersed graphite alkene that is, under shear-induced using nano-cellulose.
Invention content
The present invention proposes to prepare high heat-conductivity conducting film using nano-cellulose up-stripping dispersed graphite alkene.System of the present invention
The graphene composite material obtained has graphene dispersion horizontal high, and thermal conductivity is good, and preparation process environmental pollution is small
The characteristics of.
Technical scheme of the present invention：A kind of nano-cellulose up-stripping graphene and the side for preparing high heat-conductivity conducting film
Method is by TEMPO（That is 22,66- tetramethyl piperidine -1- oxygen radicals）It is added in the nanofiber dispersion liquid of mediated oxidative
Few layer graphene or multi-layer graphene, are uniformly mixed under the action of lasting shear agitation, and mixture is then filtered removal filter
It dries and is molded after liquid, you can obtain high heat-conductivity conducting film.
Nano-cellulose up-stripping graphene above-mentioned and the method for preparing high heat-conductivity conducting film, the TEMPO are situated between
The nanofiber dispersion liquid for leading oxidation be using lumber fibre paper pulp as raw material, by by lumber fibre paper pulp in TEMPO/NaCLO/
It is impregnated in NaBr, and carries out homogenize process, then be made after being cleaned to neutrality with solvent.
Nano-cellulose up-stripping graphene above-mentioned and the method for preparing high heat-conductivity conducting film, the lumber fibre
For needle-leaved wood fibre, broad-leaved wood fiber or herbal wood fibre.
The nano-cellulose up-stripping graphene above-mentioned and method for preparing high heat-conductivity conducting film, the solvent are
One in water, ethyl alcohol, acetone, isopropanol, tetrahydrofuran, isopropanol, methanol, dimethyl pyrrolidone or dimethylformamide
Kind.
Nano-cellulose up-stripping graphene above-mentioned and the method for preparing high heat-conductivity conducting film, the TEMPO are situated between
Lead a concentration of 0.1-20mg/mL of the nanofiber dispersion liquid of oxidation.
Nano-cellulose up-stripping graphene above-mentioned and the method for preparing high heat-conductivity conducting film, few layer graphite
The additive amount of alkene or multi-layer graphene is 0.001%-90wt%.
Nano-cellulose up-stripping graphene above-mentioned and the method for preparing high heat-conductivity conducting film, the lasting shearing
The time of stirring is 5-100h, and rotating speed is more than 100r/min.
Nano-cellulose up-stripping graphene above-mentioned and the method for preparing high heat-conductivity conducting film, the filter of the suction filtration
Membrane aperture is 0.1-0.5 μm.
Nano-cellulose up-stripping graphene above-mentioned and the method for preparing high heat-conductivity conducting film, few layer graphite
Alkene or multi-layer graphene pass through ultrasonication after being added to dispersion liquid.
Nano-cellulose up-stripping graphene above-mentioned and the method for preparing high heat-conductivity conducting film, it is described drying be
40-60 DEG C of drying 20-28h.
Beneficial effects of the present invention
1, the present invention can greatly improve the dispersion effect of graphene by using nanofiber usually up-stripping graphene,
To improve the performance of graphene composite film.
2, the present invention by by the good mechanical performance of nano-cellulose, the lower coefficient of expansion and better stability with
Graphene is combined, and being dispersed in graphene uniform in cellulose by shear agitation, and the film prepared has more
Good mechanical performance, heat conductivility and electric conductivity.It is demonstrated experimentally that when graphene nanometer sheet loading is only 10wt%, 20 DEG C
When thermal diffusion coefficient λ be 13.86mm2/s, be up to 23.4 W/mK in 20 DEG C of thermal conductivities.
3, the present invention is to make an addition to graphene in cellulose dispersion liquid, and cellulose is made of lumber fibre, and dispersion liquid can
Select water as solvent, raw material is green material, greatly reduces environmental pollution.
Description of the drawings
Fig. 1 is the graphene dispersion by nano-cellulose aid dispersion 0.001wt% concentration prepared by the embodiment of the present invention
Liquid；
Fig. 2 be graphene dispersing solution by nano-cellulose aid dispersion 0.15wt% concentration prepared by the embodiment of the present invention with
The sonicated 15min of graphene water slurry without nano-cellulose, stands picture after a week；
Fig. 3 is the photograph that solvent film forming is removed by nano-cellulose aid dispersion 0.1wt% graphenes prepared by the embodiment of the present invention
Piece；
Fig. 4 is the photograph that solvent film forming is removed by nano-cellulose aid dispersion 90wt% graphenes prepared by the embodiment of the present invention
Piece；
Fig. 5 is the scanning electron microscope diagram of the graphene fiber element laminated film cross section prepared.
Specific implementation mode
With reference to embodiment, the present invention is further illustrated, but is not intended as the foundation limited the present invention.
The embodiment of the present invention
Embodiment 1：A kind of nano-cellulose up-stripping graphene and the method for preparing high heat-conductivity conducting film, steps are as follows：
1）Using needle-leaved wood fibre as raw material, 0.1 g TEMPO and 1.0 g Na Br are dissolved in 5L deionized waters；Then will
Treated that needle wood pulp is scattered in above-mentioned solution by 0.5g, and is slowly added to NaCLO solution thereto under stiring；With dilute
System pH is adjusted to 10.0-10.2 by HCL solution, and be swift in response generation；Then reaction system is adjusted with dilute NaOH solution
PH is maintained in the range of 10.0-10.2；5m L ethyl alcohol is finally added into system and terminates reaction, and is abundant using deionized water
Diafiltration product is to neutrality；Insoluble part is collected, its moisture is measured after equilibrium water conten, and stored at 4 DEG C, prevents from going bad, institute
TEMPO oxycelluloses dispersion liquid through high speed homogenisation mechanical treatment until gained dispersion liquid becomes clear state,
The nanofiber dispersion liquid of TEMPO mediated oxidatives is obtained, the concentration of dispersion liquid is about 0.1mg/mL；
2）The graphene that 0.001wt% is added into the nanofiber dispersion liquid of TEMPO mediated oxidatives, after continuing shear agitation 5h
Be uniformly mixed, then by mixture use aperture be 0.1 μm filter membrane filter remove filtrate, then at 40 DEG C drying 20h and at
Type, you can obtain high heat-conductivity conducting film.
Embodiment 2：A kind of nano-cellulose up-stripping graphene and the method for preparing high heat-conductivity conducting film, step is such as
Under：
1）Using broad-leaved wood fiber as raw material, 0.5 g TEMPO and 5.0 g Na Br are dissolved in 2500 mL deionized waters；With
By 25.0 g, treated that broad-leaved wood pulp is scattered in above-mentioned solution afterwards, and is slowly added to specified amount thereto under stiring
NaCLO solution；System pH is adjusted to 10.0-10.2 with dilute HCL solution, be swift in response generation；Then use dilute NaOH solution
The pH for adjusting reaction system is maintained in the range of 10.0-10.2；25m L ethyl alcohol is finally added into system and terminates reaction, and
Use the abundant diafiltration product of deionized water to neutrality；Insoluble part is collected, its moisture is measured after equilibrium water conten, and at 4 DEG C
Storage, prevents from going bad, and the dispersion liquids of gained TEMPO oxycelluloses is through high speed homogenisation mechanical treatment until gained dispersion liquid becomes
For clear state, the nanofiber dispersion liquid of TEMPO mediated oxidatives is obtained, dispersion liquid concentration is about 10mg/ml；
2）The graphene that 20wt% is added into the nanofiber dispersion liquid of TEMPO mediated oxidatives mixes after continuing shear agitation 30h
It closes uniformly, then uses aperture to filter removal filtrate for 0.2 μm of filter membrane in mixture, 22h is then dried at 45 DEG C and be molded,
It can be obtained high heat-conductivity conducting film.
Embodiment 3：A kind of nano-cellulose up-stripping graphene and the method for preparing high heat-conductivity conducting film, step is such as
Under：
1）Using herbal wood fibre as raw material.0.8 g TEMPO and 8.0 g Na Br are dissolved in 4L deionized waters
In；Then by 60.0 g, treated that paper pulp is scattered in above-mentioned solution, and is slowly added to specified amount thereto under stiring
NaCLO solution；System pH is adjusted to 10.0-10.2 with dilute HCL solution, be swift in response generation；Then use dilute NaOH solution
The pH for adjusting reaction system is maintained in the range of 10.0-10.2；40m L ethyl alcohol is finally added into system and terminates reaction, and
Use the abundant diafiltration product of deionized water to neutrality；Insoluble part is collected, its moisture is measured after equilibrium water conten, and at 4 DEG C
Storage, prevents from going bad, and the dispersion liquids of gained TEMPO oxycelluloses is through high speed homogenisation mechanical treatment until gained dispersion liquid becomes
For clear state, the nanofiber dispersion liquid of TEMPO mediated oxidatives is obtained, dispersion liquid concentration is about 15mg/ml；
2）The graphene that 50wt% is added into the nanofiber dispersion liquid of TEMPO mediated oxidatives mixes after continuing shear agitation 50h
It closes uniformly, then uses aperture to filter removal filtrate for 0.3 μm of filter membrane in mixture, then dry for 24 hours and be molded at 50 DEG C,
It can be obtained high heat-conductivity conducting film.
Embodiment 4：A kind of nano-cellulose up-stripping graphene and the method for preparing high heat-conductivity conducting film, step is such as
Under：
1）Using needle-leaved wood fibre as raw material, 0.1 g TEMPO and 1.0 g Na Br are dissolved in 1L deionized waters；Then will
Treated that paper pulp is scattered in above-mentioned solution by 5.0 g, and is slowly added to specified amount NaCLO solution thereto under stiring；With
System pH is adjusted to 10.2 or so by dilute HCL solution, and be swift in response generation；Then reaction system is adjusted with dilute NaOH solution
PH is maintained in the range of 10.0-10.2；5m L ethyl alcohol is finally added into system and terminates reaction, and is abundant using deionized water
Diafiltration product is to neutrality；Insoluble part is collected, its moisture is measured after equilibrium water conten, and stored at 4 DEG C, prevents from going bad.Institute
TEMPO oxycelluloses dispersion liquid through 15000r high speed homogenisations mechanical treatment until gained dispersion liquid becomes clear
State, obtains the nanofiber dispersion liquid of TEMPO mediated oxidatives, and dispersion liquid concentration is about 5mg/ml；
2）The multi-layer graphene that 70wt% is added into the nanofiber dispersion liquid of TEMPO mediated oxidatives, continues shear agitation 80h
After be uniformly mixed, then by mixture use aperture for 0.4 μm filter membrane filter removal filtrate, then at 55 DEG C dry 26h simultaneously
Molding, you can obtain high heat-conductivity conducting film.
Embodiment 5：A kind of nano-cellulose up-stripping graphene and the method for preparing high heat-conductivity conducting film, step is such as
Under：
1）0.1 g TEMPO and 1.0 g Na Br are dissolved in 500 mL deionized waters；Then by 10.0 g treated paper
Slurry is scattered in above-mentioned solution, and is slowly added to specified amount NaCLO solution thereto under stiring；With dilute HCL solution by system
PH value is adjusted to 10.2 or so, and be swift in response generation；The pH that reaction system is then adjusted with dilute NaOH solution is maintained at 10.0-
In the range of 10.2；5m L ethyl alcohol is finally added into system and terminates reaction, and using the abundant diafiltration product of deionized water into
Property；Insoluble part is collected, its moisture is measured after equilibrium water conten, and stored at 4 DEG C, prevents from going bad.Gained TEMPO oxidations are fine
The dispersion liquid of element is tieed up through 15000r high speed homogenisations mechanical treatment until gained dispersion liquid becomes clear state, obtains TEMPO
The nanofiber dispersion liquid of mediated oxidative, dispersion liquid concentration are about 20mg/ml；
2）The multi-layer graphene that 90wt% is added into the nanofiber dispersion liquid of TEMPO mediated oxidatives, continues shear agitation 100h
After be uniformly mixed, then by mixture use aperture for 0.5 μm filter membrane filter removal filtrate, then at 60 DEG C dry 28h simultaneously
Molding, you can obtain high heat-conductivity conducting film.
Claims (10)
1. a kind of nano-cellulose up-stripping graphene and the method for preparing high heat-conductivity conducting film, it is characterised in that：It is logical
It crosses and adds graphene into the nanofiber dispersion liquid of TEMPO mediated oxidatives, be uniformly mixed under the action of lasting shear agitation,
Then it dries and is molded after mixture being filtered removal filtrate, you can obtain high heat-conductivity conducting film.
2. nano-cellulose up-stripping graphene according to claim 1 and the method for preparing high heat-conductivity conducting film,
It is characterized in that：The nanofiber dispersion liquid of the TEMPO mediated oxidatives is using lumber fibre paper pulp as raw material, by by timber
Fibre pulp impregnates in TEMPO/NaCLO/NaBr solution systems, and carries out homogenize process, then is cleaned to neutrality with solvent
After be made.
3. nano-cellulose up-stripping graphene according to claim 2 and the method for preparing high heat-conductivity conducting film,
It is characterized in that：The lumber fibre is needle-leaved wood fibre, broad-leaved wood fiber or herbal wood fibre.
4. nano-cellulose up-stripping graphene according to claim 2 and the method for preparing high heat-conductivity conducting film,
It is characterized in that：The solvent is water, ethyl alcohol, acetone, isopropanol, tetrahydrofuran, isopropanol, methanol, dimethyl pyrrolidone
Or one kind in dimethylformamide.
5. nano-cellulose up-stripping graphene according to claim 1 and the method for preparing high heat-conductivity conducting film,
It is characterized in that：A concentration of 0.1-20mg/mL of the nanofiber dispersion liquid of the TEMPO mediated oxidatives.
6. nano-cellulose up-stripping graphene according to claim 1 and the method for preparing high heat-conductivity conducting film,
It is characterized in that：The additive amount of few layer graphene or multi-layer graphene is 0.001%-90 wt%.
7. nano-cellulose up-stripping graphene according to claim 1 and the method for preparing high heat-conductivity conducting film,
It is characterized in that：The time for continuing shear agitation is 5-100h, and rotating speed is more than 100r/min.
8. nano-cellulose up-stripping graphene according to claim 1 and the method for preparing high heat-conductivity conducting film,
It is characterized in that：The filter sizes of the suction filtration are 0.1-0.5 μm.
9. nano-cellulose up-stripping graphene according to claim 1 and the method for preparing high heat-conductivity conducting film,
It is characterized in that：Few layer graphene or multi-layer graphene pass through ultrasonication after being added to dispersion liquid.
10. nano-cellulose up-stripping graphene according to claim 1 and the method for preparing high heat-conductivity conducting film,
It is characterized in that：The drying is drying 20-28h at 40-60 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665519A (en) * | 2019-01-25 | 2019-04-23 | 复旦大学 | A method of cellulose up-stripping graphene in alkali systems altogether |
| CN111910420A (en) * | 2020-03-24 | 2020-11-10 | 贵州大学 | Method for preparing thin high-strength composite heat-conducting functional film with sandwich structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20130184144A1 (en) * | 2012-01-18 | 2013-07-18 | Northwestern University | Methods of making non-covalently bonded carbon-titania nanocomposite thin films and applications of the same |
| CN103387686A (en) * | 2013-08-19 | 2013-11-13 | 南京林业大学 | Method for preparing micro/nanofiber graphene composite membrane from recycled corrugated paper |
| CN103451988A (en) * | 2013-08-30 | 2013-12-18 | 华南理工大学 | Method for bleaching paper pulp by using TEMPO/NaBr/NaClO oxidation system |
| CN107293377A (en) * | 2017-07-07 | 2017-10-24 | 齐鲁工业大学 | A kind of preparation method of tough graphene/cellulose composite heat-conducting conductive film |
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2018
- 2018-04-17 CN CN201810345144.9A patent/CN108630352A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130184144A1 (en) * | 2012-01-18 | 2013-07-18 | Northwestern University | Methods of making non-covalently bonded carbon-titania nanocomposite thin films and applications of the same |
| CN103387686A (en) * | 2013-08-19 | 2013-11-13 | 南京林业大学 | Method for preparing micro/nanofiber graphene composite membrane from recycled corrugated paper |
| CN103451988A (en) * | 2013-08-30 | 2013-12-18 | 华南理工大学 | Method for bleaching paper pulp by using TEMPO/NaBr/NaClO oxidation system |
| CN107293377A (en) * | 2017-07-07 | 2017-10-24 | 齐鲁工业大学 | A kind of preparation method of tough graphene/cellulose composite heat-conducting conductive film |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665519A (en) * | 2019-01-25 | 2019-04-23 | 复旦大学 | A method of cellulose up-stripping graphene in alkali systems altogether |
| CN111910420A (en) * | 2020-03-24 | 2020-11-10 | 贵州大学 | Method for preparing thin high-strength composite heat-conducting functional film with sandwich structure |
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Application publication date: 20181009 |