CN116120682B - Preparation method and application of polyvinylidene fluoride/expanded graphite composite material - Google Patents
Preparation method and application of polyvinylidene fluoride/expanded graphite composite material Download PDFInfo
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- CN116120682B CN116120682B CN202211515387.5A CN202211515387A CN116120682B CN 116120682 B CN116120682 B CN 116120682B CN 202211515387 A CN202211515387 A CN 202211515387A CN 116120682 B CN116120682 B CN 116120682B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000002033 PVDF binder Substances 0.000 title claims abstract description 74
- 229920002981 polyvinylidene fluoride Polymers 0.000 title claims abstract description 74
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 72
- 239000010439 graphite Substances 0.000 title claims abstract description 72
- 239000002131 composite material Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000004519 manufacturing process Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000004020 conductor Substances 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 4
- 239000002216 antistatic agent Substances 0.000 claims description 3
- 239000003989 dielectric material Substances 0.000 claims description 3
- 238000004898 kneading Methods 0.000 claims 1
- 239000006185 dispersion Substances 0.000 abstract description 13
- 230000008569 process Effects 0.000 abstract description 13
- 230000009471 action Effects 0.000 abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 7
- 239000001257 hydrogen Substances 0.000 abstract description 7
- 230000003993 interaction Effects 0.000 abstract description 7
- 238000002844 melting Methods 0.000 abstract description 4
- 230000008018 melting Effects 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 12
- 230000000694 effects Effects 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 6
- 239000002861 polymer material Substances 0.000 description 6
- 239000008187 granular material Substances 0.000 description 5
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000000155 melt Substances 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000006352 cycloaddition reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1535—Five-membered rings
- C08K5/1539—Cyclic anhydrides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- 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
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Electromagnetism (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Carbon And Carbon Compounds (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a preparation method and application of a polyvinylidene fluoride/expanded graphite composite material, and relates to the field of composite materials. The method for adding the maleic anhydride, the expanded graphite and the polyvinylidene fluoride into the melting chamber of the internal mixer for mixing promotes the dispersion of the expanded graphite in the polyvinylidene fluoride, and has the advantages of simple and easy operation process, easy control, short processing period, low production cost, easy popularization and wide application prospect. In addition, the invention enhances the interaction between the polyvinylidene fluoride and the expanded graphite by utilizing the hydrogen bond action between the maleic anhydride and the polyvinylidene fluoride and the covalent bond action formed between the maleic anhydride and the negative electron active points at the edge of the expanded graphite sheet layer in the mixing process, so as to promote the dispersion of the expanded graphite.
Description
Technical Field
The invention relates to the field of composite material preparation, in particular to a preparation method and application of a polyvinylidene fluoride/expanded graphite composite material.
Background
Expanded graphite has excellent heat conductivity (thermal conductivity of about 5000Wm due to its high strength and hardness -1 K -1 ) Has wide application prospect in the field of high polymer material modification, in particular heat conduction. The thermal conductivity of the polymer/expanded graphite composite is mainly determined by the following 3 aspects: (1) thermal conductivity of a polymer material matrix; (2) a dispersed state of the expanded graphite; (3) And the interface between the high polymer material and the expanded graphite. However, the interface between the expanded graphite and the polymer material is generally poor, the specific surface area is large, and agglomeration is very easy to occur in the process of preparing the composite material, so that the improvement of the performance of the polymer material is not ideal.
The polyvinylidene fluoride has the advantages of excellent chemical corrosion resistance, excellent hydrolysis resistance, high mechanical strength, good rigidity and the like, and has bright application prospect in the fields of photoelectricity, energy storage devices and the like. However, the functional characteristics of the material cannot fully meet the actual application requirements. The thermal conductivity, the electric conductivity, the dielectric property and the like of the composite material can be improved by adding the expanded graphite into polyvinylidene fluoride to prepare the composite material. However, since the interface between polyvinylidene fluoride and expanded graphite is poor, it is difficult to exert the function of expanded graphite.
In general, the surface modification of the expanded graphite can improve the dispersion of the expanded graphite in a polymer material matrix, but the traditional surface modification needs various chemical reagents, and the production process is complicated and discontinuous. In addition, the lattice structure of the expanded graphite may be greatly changed, resulting in a significant deterioration of the functional characteristics. Therefore, a preparation method for promoting the dispersion of the expanded graphite in the polyvinylidene fluoride matrix by improving the production efficiency and keeping the lattice integrity of the expanded graphite as much as possible is needed, so that the polyvinylidene fluoride/expanded graphite composite material with obviously improved performance is obtained.
Disclosure of Invention
Based on the problems, in order to solve the problems of poor dispersibility of graphite in polyvinylidene fluoride and poor interface bonding in the prior art, the invention provides a preparation method of a polyvinylidene fluoride/expanded graphite composite material, which comprises the following specific technical scheme:
a method for preparing a polyvinylidene fluoride/expanded graphite composite material, which comprises the following steps:
premixing graphite and maleic anhydride in proportion to obtain a mixture for standby;
and adding the mixture and polyvinylidene fluoride into mixing equipment according to a proportion to perform melt mixing, so as to obtain the polyvinylidene fluoride/expanded graphite composite material.
Further, the mass ratio of the graphite to the maleic anhydride is 1:10-10:1.
Further, the mass ratio of the mixture to the polyvinylidene fluoride is 1:100-20:100.
Further, the rotation speed of the melt mixing is 20 r/min-500 r/min, and the temperature is 180 ℃ to 300 ℃.
Further, the graphite is expandable graphite.
In addition, the application further provides application of the polyvinylidene fluoride/expanded graphite composite material, and the polyvinylidene fluoride/expanded graphite composite material is used for manufacturing one or more of a heat conducting material, a dielectric material, a conductive material, an electromagnetic shielding material and an antistatic material.
The method for adding the maleic anhydride, the expanded graphite and the polyvinylidene fluoride into the melting chamber of the internal mixer for mixing promotes the dispersion of the expanded graphite in the polyvinylidene fluoride, and has the advantages of simple and easy operation process, easy control, short processing period, low production cost, easy popularization and wide application prospect.
In addition, the invention enhances the interaction between the polyvinylidene fluoride and the expanded graphite by utilizing the hydrogen bond action between the maleic anhydride and the polyvinylidene fluoride and the covalent bond action formed between the maleic anhydride and the negative electron active points at the edge of the expanded graphite sheet layer in the mixing process, so as to promote the dispersion of the expanded graphite.
Drawings
FIG. 1 is a graph of thermal conductivity as a function of EG content for the composites of the examples and the composites of the comparative examples; in fig. 1, curve 1 corresponds to comparative example 1 and comparative example 2, and curve 2 corresponds to example 1 and example 2;
FIG. 2 is a scanning electron microscope image of a PVDF/EG/MA composite according to example 2 of the present application;
FIG. 3 is a scanning electron microscope image of the polyvinylidene fluoride/expanded graphite composite material of comparative example 2.
Detailed Description
The present invention will be described in further detail with reference to the following examples thereof in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the detailed description and specific examples are intended for purposes of illustration only and are not intended to limit the scope of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The preparation method of the polyvinylidene fluoride/expanded graphite composite material in one embodiment of the invention comprises the following steps:
premixing graphite and maleic anhydride in proportion to obtain a mixture for standby;
and adding the mixture and polyvinylidene fluoride into mixing equipment according to a proportion to perform melt mixing, so as to obtain the polyvinylidene fluoride/expanded graphite composite material.
In one embodiment, the mass ratio of the graphite to the maleic anhydride is 1:10-10:1.
In one embodiment, the mass ratio of the mixture to the polyvinylidene fluoride is 1:100 to 20:100.
In one embodiment, the melt mixing is one of an internal mixer, a single screw extruder, and a twin screw extruder.
In one embodiment, the rotational speed of the melt-mixing is 20r/min to 500r/min, and the temperature is 180 ℃ to 300 ℃.
In one embodiment, the graphite is expandable graphite. The expanded graphite expands by heating in the mixing process, and is continuously stripped and dispersed in the polyvinylidene fluoride melt under the shearing action of the screw.
In addition, the application further provides application of the polyvinylidene fluoride/expanded graphite composite material, and the polyvinylidene fluoride/expanded graphite composite material is used for manufacturing one or more of a heat conducting material, a dielectric material, a conductive material, an electromagnetic shielding material and an antistatic material.
In the application, the maleic anhydride molecules are added and dispersed in the polyvinylidene fluoride melt, so that the lubricating agent is used in the melt mixing process, and the fluidity of the polyvinylidene fluoride molecular chain is promoted. And the maleic anhydride molecules and the polyvinylidene fluoride molecular chains form a hydrogen bond effect, and the covalent bond effect formed between the maleic anhydride molecules and negative electron active points at the edge of the expanded graphite sheet layer enhances the interaction between the expanded graphite and the polyvinylidene fluoride and promotes the dispersion of the expanded graphite in the polyvinylidene fluoride matrix.
The method for adding the maleic anhydride, the expanded graphite and the polyvinylidene fluoride into the melting chamber of the internal mixer for mixing promotes the dispersion of the expanded graphite in the polyvinylidene fluoride, and has the advantages of simple and easy operation process, easy control, short processing period, low production cost, easy popularization and wide application prospect.
In addition, the invention enhances the interaction between the polyvinylidene fluoride and the expanded graphite by utilizing the hydrogen bond action between the maleic anhydride and the polyvinylidene fluoride and the covalent bond action formed between the maleic anhydride and the negative electron active points at the edge of the expanded graphite sheet layer in the mixing process, so as to promote the dispersion of the expanded graphite.
Embodiments of the present invention will be described in detail below with reference to specific examples.
Example 1:
the mass ratio is 1:2, placing graphite and maleic anhydride in a mechanical stirrer to be uniformly stirred to prepare a premix;
setting the temperature of a mixing cavity of an internal mixer to 220 ℃ and the rotating speed of a rotor to 100rpm, taking 50g of PVDF granules, adding 4.5g of premix into the mixing cavity, and mixing for 5min to obtain the polyvinylidene fluoride/expanded graphite composite material. In the embodiment, in the mixing process, the carbonyl of MA and the CH2 group of PVDF form a hydrogen bond effect, and cycloaddition reaction is carried out with the negative electron active point at the edge of the EG sheet layer to form a covalent bond effect, so that the interaction between EG and PVDF is enhanced, and the dispersion of EG in a PVDF matrix is promoted.
Example 2:
the mass ratio is 1:2, placing graphite and maleic anhydride in a mechanical stirrer to be uniformly stirred to prepare a premix;
the temperature of the mixing chamber of the internal mixer was set at 220℃and the rotational speed of the rotor was 100rpm, 50g of PVDF pellets were taken and added to the mixing chamber, followed by adding 10.5g of the premix and mixing for 5 minutes, to obtain a polyvinylidene fluoride/expanded graphite composite. In the embodiment, in the mixing process, a hydrogen bond effect is formed between MA molecules and PVDF molecular chains, and a covalent bond effect is formed between MA molecules and negative electron active points at the edge of the EG sheet layer, so that the interaction between EG and PVDF is enhanced, and the dispersion of EG in a PVDF matrix is promoted.
Comparative example 1:
setting the temperature of a mixing cavity of an internal mixer to 220 ℃, taking 50g of PVDF granules, adding the PVDF granules into the mixing cavity, adding 1.5g of graphite powder, and mixing for 5min to obtain the PVDF/EG composite material, wherein the rotating speed of a rotor is 100 rpm.
Comparative example 2:
setting the temperature of a mixing cavity of an internal mixer to 220 ℃, taking 50g of PVDF granules, adding the PVDF granules into the mixing cavity, adding 3.5g of graphite powder, and mixing for 5min to obtain the PVDF/EG composite material, wherein the rotating speed of a rotor is 100 rpm.
FIG. 1 is a graph of thermal conductivity as a function of EG content for the composites of the examples and the composites of the comparative examples; in fig. 1, curve 1 corresponds to comparative example 1 and comparative example 2, and curve 2 corresponds to example 1 and example 2, it can be seen that the thermal conductivity of PVDF increases with the addition of EG, and further increases with the increase in EG content; the PVDF/EG/MA composite materials prepared by the method have significantly higher thermal conductivity than that of comparative examples 1 and 2. In particular, the PVDF/EG/MA composite prepared in example 2 has a thermal conductivity of 0.73W/mK, which is about 33% greater than the PVDF/EG composite prepared in comparative example 2. SEM photographs from the brittle cross-section of the composite material of fig. 2-3. It can be seen that EG formed larger agglomerates in the composite material prepared in comparative example 2, and EG dispersed state in the composite material prepared in example 2 was significantly improved, indicating that EG was better exfoliated and dispersed in the composite material.
Therefore, the method for adding the maleic anhydride, the expandable graphite and the polyvinylidene fluoride into the melting chamber of the internal mixer for mixing promotes the dispersion of the expandable graphite in the polyvinylidene fluoride, and has the advantages of simple and easy operation process, easy control, short processing period, low production cost, easy popularization and wide application prospect. The invention enhances the interaction between the polyvinylidene fluoride and the expanded graphite by utilizing the hydrogen bond action between the maleic anhydride and the polyvinylidene fluoride and the covalent bond action formed between the maleic anhydride and the negative electron active point at the edge of the expanded graphite sheet layer in the mixing process, thereby promoting the dispersion of the expanded graphite.
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (5)
1. The preparation method of the polyvinylidene fluoride/expanded graphite composite material is characterized by comprising the following steps of:
premixing graphite and maleic anhydride in proportion to obtain a mixture for standby;
and adding the mixture and polyvinylidene fluoride into mixing equipment according to a proportion to perform melt mixing, so as to obtain the polyvinylidene fluoride/expanded graphite composite material.
2. The preparation method according to claim 1, wherein the mass ratio of graphite to maleic anhydride is 1:10-10:1.
3. The preparation method according to claim 1, wherein the mass ratio of the mixture to the polyvinylidene fluoride is 1:100 to 20:100.
4. The method according to claim 1, wherein the rotational speed of the melt-kneading is 20 to 500r/min and the temperature is 180 to 300 ℃.
5. The use of the polyvinylidene fluoride/expanded graphite composite material prepared by the preparation method of the polyvinylidene fluoride/expanded graphite composite material according to claim 1, wherein the polyvinylidene fluoride/expanded graphite composite material is used for manufacturing one or more of a heat conducting material, a dielectric material, an electric conducting material, an electromagnetic shielding material and an antistatic material.
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| KR102135844B1 (en) * | 2017-03-30 | 2020-08-27 | 사빅 글로벌 테크놀러지스 비.브이. | Graphite-based composition with increased volume resistivity |
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