CN116553533A - Preparation method of graphene sealing material - Google Patents
Preparation method of graphene sealing material Download PDFInfo
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- CN116553533A CN116553533A CN202310516486.3A CN202310516486A CN116553533A CN 116553533 A CN116553533 A CN 116553533A CN 202310516486 A CN202310516486 A CN 202310516486A CN 116553533 A CN116553533 A CN 116553533A
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- graphene
- sealing material
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 146
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 129
- 239000003566 sealing material Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000006185 dispersion Substances 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 239000000654 additive Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- 238000003490 calendering Methods 0.000 claims abstract description 10
- 239000011248 coating agent Substances 0.000 claims abstract description 10
- 238000000576 coating method Methods 0.000 claims abstract description 10
- 239000000758 substrate Substances 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 230000000996 additive effect Effects 0.000 claims description 6
- 229910052799 carbon Inorganic materials 0.000 claims description 6
- 238000005187 foaming Methods 0.000 claims description 6
- 238000005096 rolling process Methods 0.000 claims description 6
- 229920002799 BoPET Polymers 0.000 claims description 5
- 239000004743 Polypropylene Substances 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 5
- 229920002678 cellulose Polymers 0.000 claims description 5
- 239000001913 cellulose Substances 0.000 claims description 5
- 229920002401 polyacrylamide Polymers 0.000 claims description 5
- -1 polypropylene Polymers 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims 17
- 238000007789 sealing Methods 0.000 abstract description 11
- 238000009991 scouring Methods 0.000 abstract description 4
- 229910002804 graphite Inorganic materials 0.000 description 11
- 239000010439 graphite Substances 0.000 description 11
- 238000005516 engineering process Methods 0.000 description 5
- 239000010425 asbestos Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052895 riebeckite Inorganic materials 0.000 description 2
- 230000032683 aging Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C01B32/184—Preparation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- C01B32/194—After-treatment
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/10—Materials in mouldable or extrudable form for sealing or packing joints or covers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2200/00—Chemical nature of materials in mouldable or extrudable form for sealing or packing joints or covers
- C09K2200/02—Inorganic compounds
- C09K2200/0204—Elements
- C09K2200/0208—Carbon
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a graphene sealing material, which comprises the following steps: s1, taking graphene oxide, graphene microplates and additives, and mixing according to the following steps of 1:0.7:0.1-1:0.05: mixing in a proportion of 0.01 to obtain graphene oxide dispersion liquid; s2, coating the graphene oxide dispersion liquid on a substrate to obtain a graphene oxide film; s3, carrying out high-temperature reduction treatment on the graphene oxide film at 2400-3200 ℃ to obtain a graphene film; s4, calendaring the graphene film to obtain a graphene film with the density of 0.2g/cm 3 ‑1.5g/cm 3 Is a graphene sealing material. The graphene sealing material has the advantages of high strength, good wear resistance, capability of performing a scouring test and the like, and can better meet the sealing requirement.
Description
Technical Field
The invention relates to a sealing material, in particular to a preparation method of a graphene sealing material.
Background
With the development of high and new industrial technologies such as modern technology and superconducting technology, the traditional asbestos sealing material cannot meet the increasing requirements of the high and new technology industry on engineering sealing materials in performance. Therefore, in recent years, flexible graphite sealing materials are gradually developed internationally, and the flexible graphite sealing materials replace asbestos sealing materials in some sealing fields due to good sealing performance, but the application range of the flexible graphite sealing materials in high and new technologies is still limited due to the defects of low density, large specific surface area, poor fluidity, fragility, inconvenience in stamping and the like. Meanwhile, since the flexible graphite sealing material is a material with gaps, the surface of the flexible graphite sealing material can absorb a certain amount of water or oil, so that the connection surface has cohesiveness, and if the flexible graphite sealing material is directly used as the sealing material, the sealing is difficult to achieve. Furthermore, the flexible graphite sealing material is composed of graphite worms, and if no binder is used, the internal bonding of the material is formed only by mechanical biting force, so that the flexible graphite sealing material has low strength, poor wear resistance and no anti-scouring test, and therefore, the flexible graphite sealing material needs to be improved.
Disclosure of Invention
Aiming at the defects of low strength, poor wear resistance, no anti-scouring test and the like of the flexible graphite sealing material in the prior art, the invention provides a novel preparation method of the graphene sealing material.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the preparation method of the graphene sealing material comprises the following steps:
s1, taking graphene oxide, graphene microplates and additives, and mixing according to the following steps of 1:0.7:0.1-1:0.05: mixing in a proportion of 0.01 to obtain graphene oxide dispersion liquid;
s2, coating the graphene oxide dispersion liquid on a substrate to obtain a graphene oxide film;
s3, carrying out high-temperature reduction treatment on the graphene oxide film at 2400-3200 ℃ to obtain a graphene film;
s4, calendaring the graphene film to obtain a graphene film with the density of 0.2g/cm 3 -1.5g/cm 3 Is a graphene sealing material.
Through the coating of the step S2, the graphene oxide dispersion liquid can realize the transverse arrangement of graphene oxide sheets after the coating is completed, a multilayer structure is formed, and the sealing performance of the obtained graphene sealing material is improved. Step S3 can eliminate oxygen-containing functional groups in the resulting graphene oxide film, thereby enabling the resulting graphene sealing material to be used at high temperatures. Step S4 can ensure uniformity of the obtained graphene sealing material, the density is limited in the range, the graphene sealing material has moderate elasticity and compressibility, and sealing performance of the graphene sealing material in use is improved.
The graphene sealing material has the advantages of high strength, good wear resistance, capability of performing a scouring test and the like, and can better meet the sealing requirement.
Preferably, in the preparation method of the graphene sealing material, the additive is polyvinyl alcohol, polyacrylamide or cellulose.
The additive is selected from the materials, so that the cohesiveness among the materials can be better increased, and the situation that the obtained graphene sealing material is layered or powder falls is prevented.
Preferably, in the preparation method of the graphene sealing material, the solid content of the graphene oxide dispersion liquid obtained in the step S1 is 2% -10%.
If the solid content of the graphene oxide dispersion liquid is too low, drying after coating is difficult, and if the solid content of the graphene oxide dispersion liquid is too high, the problems of insufficient peeling and poor leveling property can be caused when the graphene oxide dispersion liquid is coated, so that the solid content is in the above range, and the coating quality of the graphene oxide dispersion liquid can be better ensured.
Preferably, in the preparation method of the graphene sealing material, the high-temperature reduction treatment environment is a vacuum environment or an inert atmosphere environment.
In the above environment, oxygen-containing functional groups in the environment can be eliminated, thereby better improving the effect of the high-temperature reduction treatment.
Preferably, in the preparation method of the graphene sealing material, the carbon content of the graphene film is greater than 95%.
The carbon content of the graphene film is more than 95%, so that the sealing performance and the ageing resistance of the obtained graphene sealing material can be better ensured.
Preferably, in the preparation method of the graphene sealing material, the specific surface area of the graphene microchip is larger than 20 square meters per gram.
The specific surface area of the graphene microplates is larger than 20 square meters per gram, and the single-layer property of the graphene microplates can be improved, so that the sealing performance of the finally obtained graphene sealing material is improved.
Preferably, in the preparation method of the graphene sealing material, the foaming ratio of the graphene film during high-temperature reduction treatment is 2-20 times.
The foaming multiplying power of the graphene film is 2-20 times, and better pre-conditions can be provided for subsequent calendaring and sealing, so that the sealing performance of the finally obtained graphene sealing material is improved.
Preferably, in the preparation method of the graphene sealing material, the rolling is flat rolling or rolling.
The density of the obtained graphene sealing material can be better controlled by flattening or rolling.
Preferably, in the preparation method of the graphene sealing material, the substrate is a PET film or a polypropylene air-permeable film.
The base material is made of the above materials, so that the drying uniformity and the flatness of the base material can be better ensured.
Detailed Description
The invention is described in further detail below in connection with the following detailed description, but they are not limiting of the invention:
example 1
The preparation method of the graphene sealing material comprises the following steps:
s1, taking graphene oxide, graphene microplates and additives, and mixing according to the following steps of 1:0.7: mixing in a ratio of 0.1 to obtain graphene oxide dispersion liquid;
s2, coating the graphene oxide dispersion liquid on a substrate to obtain a graphene oxide film;
s3, carrying out high-temperature reduction treatment on the graphene oxide film at 2400 ℃ to obtain a graphene film;
s4, calendaring the graphene film to obtain a graphene film with the density of 0.2g/cm 3 Is a graphene sealing material.
Preferably, the additive is polyvinyl alcohol or polyacrylamide or cellulose.
Preferably, the solid content of the graphene oxide dispersion liquid obtained in the step S1 is 2%.
Preferably, the high-temperature reduction treatment is performed in a vacuum atmosphere or an inert atmosphere.
Preferably, the carbon content of the graphene film is greater than 95%.
Preferably, the specific surface area of the graphene microplates is greater than 20 square meters per gram.
Preferably, the graphene film has a foaming ratio of 2 in the high-temperature reduction treatment.
Preferably, the calendering is flat or roll pressing.
Preferably, the substrate is a PET film or a polypropylene breathable film.
Example 2
The preparation method of the graphene sealing material comprises the following steps:
s1, taking graphene oxide, graphene microplates and additives, and mixing according to the following steps of 1:0.05: mixing in a proportion of 0.01 to obtain graphene oxide dispersion liquid;
s2, coating the graphene oxide dispersion liquid on a substrate to obtain a graphene oxide film;
s3, carrying out high-temperature reduction treatment on the graphene oxide film at 3200 ℃ to obtain a graphene film;
s4, calendaring the graphene film to obtain a graphene film with a density of 1.5g/cm 3 Is a graphene sealing material.
Preferably, the additive is polyvinyl alcohol or polyacrylamide or cellulose.
Preferably, the solid content of the graphene oxide dispersion liquid obtained in the step S1 is 10%.
Preferably, the high-temperature reduction treatment is performed in a vacuum atmosphere or an inert atmosphere.
Preferably, the carbon content of the graphene film is greater than 95%.
Preferably, the specific surface area of the graphene microplates is greater than 20 square meters per gram.
Preferably, the graphene film has a foaming ratio of 20 times in the high-temperature reduction treatment.
Preferably, the calendering is flat or roll pressing.
Preferably, the substrate is a PET film or a polypropylene breathable film.
Example 3
The preparation method of the graphene sealing material comprises the following steps:
s1, taking graphene oxide, graphene microplates and additives, and mixing according to the following steps of 1:0.3: mixing in a proportion of 0.05 to obtain graphene oxide dispersion liquid;
s2, coating the graphene oxide dispersion liquid on a substrate to obtain a graphene oxide film;
s3, carrying out high-temperature reduction treatment on the graphene oxide film at 2800 ℃ to obtain a graphene film;
s4, calendaring the graphene film to obtain a graphene film with the density of 0.8g/cm 3 Is a graphene sealing material.
Preferably, the additive is polyvinyl alcohol or polyacrylamide or cellulose.
Preferably, the solid content of the graphene oxide dispersion liquid obtained in the step S1 is 6%.
Preferably, the high-temperature reduction treatment is performed in a vacuum atmosphere or an inert atmosphere.
Preferably, the carbon content of the graphene film is greater than 95%.
Preferably, the specific surface area of the graphene microplates is greater than 20 square meters per gram.
Preferably, the graphene film has a foaming ratio of 11 times in the high-temperature reduction treatment.
Preferably, the calendering is flat or roll pressing.
Preferably, the substrate is a PET film or a polypropylene breathable film.
In summary, the foregoing description is only of the preferred embodiments of the present invention, and all equivalent changes and modifications that come within the scope of the present invention are desired to be covered thereby.
Claims (9)
1. A preparation method of a graphene sealing material is characterized by comprising the following steps: the method comprises the following steps:
s1, taking graphene oxide, graphene microplates and additives, and mixing according to the following steps of 1:0.7:0.1-1:0.05: mixing in a proportion of 0.01 to obtain graphene oxide dispersion liquid;
s2, coating the graphene oxide dispersion liquid on a substrate to obtain a graphene oxide film;
s3, carrying out high-temperature reduction treatment on the graphene oxide film at 2400-3200 ℃ to obtain a graphene film;
s4, calendaring the graphene film to obtain a graphene film with the density of 0.2g/cm 3 -1.5g/cm 3 Is a graphene sealing material.
2. The method for preparing the graphene sealing material according to claim 1, wherein the method comprises the following steps: the additive is polyvinyl alcohol or polyacrylamide or cellulose.
3. The method for preparing the graphene sealing material according to claim 1, wherein the method comprises the following steps: the solid content of the graphene oxide dispersion liquid obtained in the step S1 is 2% -10%.
4. The method for preparing the graphene sealing material according to claim 1, wherein the method comprises the following steps: the high-temperature reduction treatment environment is a vacuum environment or an inert atmosphere environment.
5. The method for preparing the graphene sealing material according to claim 1, wherein the method comprises the following steps: the carbon content of the graphene film is more than 95%.
6. The method for preparing the graphene sealing material according to claim 1, wherein the method comprises the following steps: the specific surface area of the graphene microplates is larger than 20 square meters per gram.
7. The method for preparing the graphene sealing material according to claim 1, wherein the method comprises the following steps: the foaming multiplying power of the graphene film in high-temperature reduction treatment is 2-20 times.
8. The method for preparing the graphene sealing material according to claim 1, wherein the method comprises the following steps: the rolling is flat pressing or rolling.
9. The method for preparing the graphene sealing material according to claim 1, wherein the method comprises the following steps: the base material is a PET film or a polypropylene breathable film.
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Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103864059A (en) * | 2012-12-18 | 2014-06-18 | 中国科学院兰州化学物理研究所 | Graphene high-efficiency preparation method based on extraction purification technology |
CN104592950A (en) * | 2014-12-26 | 2015-05-06 | 苏州格瑞丰纳米科技有限公司 | High-thermal conductivity graphite alkenyl polymer heat conducting film and preparation method thereof |
CN105254302A (en) * | 2015-10-12 | 2016-01-20 | 上海应用技术学院 | Preparing method for graphene heat conduction sheet |
CN105860939A (en) * | 2016-03-30 | 2016-08-17 | 上海上大瑞沪微系统集成技术有限公司 | Preparation method for graphene film with high thermal conductivity and heat dissipation method based on graphene film |
CN108329495A (en) * | 2017-12-20 | 2018-07-27 | 上海交通大学 | Graphene with biomimetic features-Cellulose nanocrystal composite heat-conducting film and its preparation |
CN110234181A (en) * | 2019-03-06 | 2019-09-13 | 上海交通大学 | A kind of preparation method of the graphene-based compound electric film of self-supporting |
CN110540193A (en) * | 2019-09-20 | 2019-12-06 | 上海大学 | preparation method of pressure graphitized graphene film |
CN111286309A (en) * | 2020-03-24 | 2020-06-16 | 昆山印可达新材料科技有限公司 | High-performance graphene heat dissipation film, and preparation method and application thereof |
CN111924830A (en) * | 2020-09-18 | 2020-11-13 | 山东海科创新研究院有限公司 | Preparation method of graphene heat-conducting film and product obtained by preparation method |
CN114381022A (en) * | 2020-10-19 | 2022-04-22 | 苏州南诣科技有限公司 | Graphene film and graphene film reinforced heat-conducting composite film |
-
2023
- 2023-05-09 CN CN202310516486.3A patent/CN116553533A/en active Pending
Patent Citations (10)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103864059A (en) * | 2012-12-18 | 2014-06-18 | 中国科学院兰州化学物理研究所 | Graphene high-efficiency preparation method based on extraction purification technology |
CN104592950A (en) * | 2014-12-26 | 2015-05-06 | 苏州格瑞丰纳米科技有限公司 | High-thermal conductivity graphite alkenyl polymer heat conducting film and preparation method thereof |
CN105254302A (en) * | 2015-10-12 | 2016-01-20 | 上海应用技术学院 | Preparing method for graphene heat conduction sheet |
CN105860939A (en) * | 2016-03-30 | 2016-08-17 | 上海上大瑞沪微系统集成技术有限公司 | Preparation method for graphene film with high thermal conductivity and heat dissipation method based on graphene film |
CN108329495A (en) * | 2017-12-20 | 2018-07-27 | 上海交通大学 | Graphene with biomimetic features-Cellulose nanocrystal composite heat-conducting film and its preparation |
CN110234181A (en) * | 2019-03-06 | 2019-09-13 | 上海交通大学 | A kind of preparation method of the graphene-based compound electric film of self-supporting |
CN110540193A (en) * | 2019-09-20 | 2019-12-06 | 上海大学 | preparation method of pressure graphitized graphene film |
CN111286309A (en) * | 2020-03-24 | 2020-06-16 | 昆山印可达新材料科技有限公司 | High-performance graphene heat dissipation film, and preparation method and application thereof |
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CN114381022A (en) * | 2020-10-19 | 2022-04-22 | 苏州南诣科技有限公司 | Graphene film and graphene film reinforced heat-conducting composite film |
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