CN117024936A - Heat-conducting and lubricating dual-functional composite resin and preparation method thereof - Google Patents
Heat-conducting and lubricating dual-functional composite resin and preparation method thereof Download PDFInfo
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- CN117024936A CN117024936A CN202311121973.6A CN202311121973A CN117024936A CN 117024936 A CN117024936 A CN 117024936A CN 202311121973 A CN202311121973 A CN 202311121973A CN 117024936 A CN117024936 A CN 117024936A
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- 239000000805 composite resin Substances 0.000 title claims abstract description 55
- 230000001050 lubricating effect Effects 0.000 title claims description 9
- 238000002360 preparation method Methods 0.000 title abstract description 22
- 239000003094 microcapsule Substances 0.000 claims abstract description 54
- 229920005989 resin Polymers 0.000 claims abstract description 54
- 239000011347 resin Substances 0.000 claims abstract description 54
- 238000005461 lubrication Methods 0.000 claims abstract description 42
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 30
- 239000011159 matrix material Substances 0.000 claims abstract description 28
- 239000002923 metal particle Substances 0.000 claims abstract description 25
- 239000000945 filler Substances 0.000 claims abstract description 24
- 239000000843 powder Substances 0.000 claims abstract description 15
- 239000011257 shell material Substances 0.000 claims abstract description 15
- 239000011162 core material Substances 0.000 claims abstract description 14
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 9
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000010687 lubricating oil Substances 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims description 39
- 239000002105 nanoparticle Substances 0.000 claims description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 19
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 17
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 17
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 12
- 239000004917 carbon fiber Substances 0.000 claims description 12
- 229920006337 unsaturated polyester resin Polymers 0.000 claims description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 10
- 239000000835 fiber Substances 0.000 claims description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- 239000000377 silicon dioxide Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 9
- 238000011049 filling Methods 0.000 claims description 8
- 238000000465 moulding Methods 0.000 claims description 8
- 239000002041 carbon nanotube Substances 0.000 claims description 7
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 7
- 239000003365 glass fiber Substances 0.000 claims description 7
- 229910021389 graphene Inorganic materials 0.000 claims description 7
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims description 7
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 229920002748 Basalt fiber Polymers 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 5
- 239000005995 Aluminium silicate Substances 0.000 claims description 5
- 229910052582 BN Inorganic materials 0.000 claims description 5
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 5
- 229920000877 Melamine resin Polymers 0.000 claims description 5
- 239000004642 Polyimide Substances 0.000 claims description 5
- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 5
- 235000012211 aluminium silicate Nutrition 0.000 claims description 5
- 239000010425 asbestos Substances 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- GBAOBIBJACZTNA-UHFFFAOYSA-L calcium sulfite Chemical compound [Ca+2].[O-]S([O-])=O GBAOBIBJACZTNA-UHFFFAOYSA-L 0.000 claims description 5
- 235000010261 calcium sulphite Nutrition 0.000 claims description 5
- 239000006229 carbon black Substances 0.000 claims description 5
- 239000004927 clay Substances 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 5
- 239000010439 graphite Substances 0.000 claims description 5
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 5
- 239000010445 mica Substances 0.000 claims description 5
- 229910052618 mica group Inorganic materials 0.000 claims description 5
- 229920001568 phenolic resin Polymers 0.000 claims description 5
- 239000005011 phenolic resin Substances 0.000 claims description 5
- 229920000647 polyepoxide Polymers 0.000 claims description 5
- 229920001721 polyimide Polymers 0.000 claims description 5
- 239000004814 polyurethane Substances 0.000 claims description 5
- 229920002635 polyurethane Polymers 0.000 claims description 5
- 229910052895 riebeckite Inorganic materials 0.000 claims description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 239000000454 talc Substances 0.000 claims description 3
- 229910052623 talc Inorganic materials 0.000 claims description 3
- 238000000935 solvent evaporation Methods 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 230000009977 dual effect Effects 0.000 claims 4
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 claims 2
- 239000002131 composite material Substances 0.000 abstract description 9
- 230000007547 defect Effects 0.000 abstract description 5
- 230000005672 electromagnetic field Effects 0.000 abstract description 5
- 230000017525 heat dissipation Effects 0.000 abstract description 5
- 230000001105 regulatory effect Effects 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 description 21
- 239000000463 material Substances 0.000 description 12
- 239000002904 solvent Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 8
- 235000012239 silicon dioxide Nutrition 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- WFUGQJXVXHBTEM-UHFFFAOYSA-N 2-hydroperoxy-2-(2-hydroperoxybutan-2-ylperoxy)butane Chemical compound CCC(C)(OO)OOC(C)(CC)OO WFUGQJXVXHBTEM-UHFFFAOYSA-N 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- AMFIJXSMYBKJQV-UHFFFAOYSA-L cobalt(2+);octadecanoate Chemical compound [Co+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AMFIJXSMYBKJQV-UHFFFAOYSA-L 0.000 description 5
- 239000012071 phase Substances 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 230000001588 bifunctional effect Effects 0.000 description 4
- 239000010949 copper Substances 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000004696 Poly ether ether ketone Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229920002530 polyetherether ketone Polymers 0.000 description 2
- 235000012222 talc Nutrition 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229920002430 Fibre-reinforced plastic Polymers 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 101100407037 Oryza sativa subsp. japonica PAO6 gene Proteins 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229920000891 common polymer Polymers 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
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- 238000001704 evaporation Methods 0.000 description 1
- 239000011151 fibre-reinforced plastic Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
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- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 229920001778 nylon Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
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- 238000012876 topography Methods 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/06—Unsaturated polyesters
-
- 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
- C08K3/08—Metals
- C08K2003/0806—Silver
-
- 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
- C08K3/08—Metals
- C08K2003/085—Copper
-
- 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
- C08K3/08—Metals
- C08K2003/0856—Iron
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a heat conduction-lubrication dual-function composite resin and a preparation method thereof. The composite resin comprises a thermosetting resin matrix, modified filler and a heat conduction-lubrication dual-function microcapsule; the core material of the heat conduction-lubrication dual-function microcapsule comprises nano metal particles and lubricating oil, and the shell material is resin. The composite resin has compact structure, no crack, no hole and other defects, and greatly improved heat conducting performance without affecting mechanical performance and tribological performance. The nano metal particles with electromagnetic properties such as nano iron powder, nano cobalt powder and nano nickel powder can be further optimized, the position of the microcapsule in the composite material can be directionally regulated and controlled in an electromagnetic field mode, and the heat dissipation rate of a high-temperature local area is improved.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a heat conduction-lubrication dual-function composite resin and a preparation method thereof.
Background
The thermosetting resin (thermosetting resin) is a resin which is chemically changed after being heated, gradually hardened and molded, and is not softened nor dissolved after being heated. The thermosetting resin matrix composite material is also called fiber reinforced plastic, is a multiphase material composed of a thermosetting resin matrix, a fiber reinforced material and other fillers, has better performance than a single material, effectively overcomes the defects of poor mechanical performance of the single resin matrix and the like, and is a composite material with mature technology and most wide application at present.
Because of the extreme use conditions of high-tip equipment, high temperature becomes a common working condition in equipment use, and thus, higher requirements are put on the temperature resistance and the thermal conductivity of composite materials in the equipment, the thermal conductivity coefficient of common polymer resin is generally less than 1W/(m.K), and polymer composite materials with high thermal conductivity coefficients are getting more and more attention.
Disclosure of Invention
The invention aims to provide a heat conduction-lubrication dual-function composite resin and a preparation method thereof. The thermal conductivity of the composite resin is greatly improved on the premise of not affecting the mechanical property and tribological property of the resin, and the continuous high temperature and fault occurrence of a mechanical device applying the composite resin can be reduced.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the invention provides a heat conduction-lubrication dual-function composite resin, which comprises a thermosetting resin matrix, a modified filler and heat conduction-lubrication dual-function microcapsules; the mass ratio of the modified filler is 0.1-50%, preferably 1-20%, more preferably 4-10% based on 100% of the mass of the thermosetting resin matrix; the heat conduction-lubrication dual-function microcapsule accounts for 0.1-50%, preferably 10-50%, more preferably 20-40%;
the core material of the heat conduction-lubrication dual-function microcapsule comprises nano metal particles and lubricating oil, and the shell material is resin;
in the heat conduction-lubrication dual-function microcapsule, the mass ratio of the nano metal particles is 1% -10%, preferably 1% -9%, more preferably 3% -9%; the mass ratio of the lubricating oil is 10% -20%, and the balance is the resin shell material.
According to the heat conductive-lubricating dual-function composite resin of the present invention, the mass ratio of the nano-metal particles is preferably 0.001% to 5%, more preferably 0.1% to 5%, and still more preferably 1% to 4% based on 100% of the mass of the thermosetting resin matrix.
According to the heat-conducting-lubricating dual-function composite resin of the present invention, preferably, the core material of the heat-conducting-lubricating dual-function microcapsule further comprises lubricating particles; in the heat conduction-lubrication dual-function microcapsule, the mass ratio of the lubrication particles is 10% -30%, more preferably 25% -30%.
According to the heat-conducting-lubricating dual-function composite resin of the present invention, preferably, the core material of the heat-conducting-lubricating dual-function microcapsule further comprises fibers; in the heat conduction-lubrication dual-function microcapsule, the mass ratio of the fiber is 10% -20%.
According to the heat conductive-lubricating dual-function composite resin of the present invention, preferably, the shell material adopts at least one of epoxy resin, phenolic resin, unsaturated polyester resin, melamine-formaldehyde resin, urea resin, polyurethane and polyimide.
According to the heat conduction-lubrication dual-function composite resin, the heat conduction performance of the resin can be effectively improved by adding the nano metal particles. Preferably, the nano metal particles are at least one selected from nano silver powder, nano copper powder, nano molybdenum powder, nano aluminum powder, nano iron powder, nano cobalt powder and nano nickel powder. More preferably, the nano metal particles are at least one of nano metal particles with electromagnetic properties, such as nano iron powder, nano cobalt powder, nano nickel powder and the like, and the nano metal particles also have electromagnetic properties, so that the positions of the microcapsules in the composite material can be directionally regulated and controlled in an electromagnetic field mode, and the heat dissipation rate of a high-temperature local area is improved.
According to the heat conduction-lubrication dual-function composite resin, the lubrication particles have good lubrication effect. Preferably, the lubricating particles are at least one selected from graphene, carbon nanotubes, polytetrafluoroethylene nanoparticles, graphite and molybdenum disulfide.
According to the heat conduction-lubrication dual-function composite resin, the fiber has the function of enhancing mechanical properties, and can improve the compression resistance. Preferably, the fibers are selected from at least one of carbon fibers, glass fibers, basalt fibers.
According to the heat conductive-lubricating dual-function composite resin of the present invention, preferably, the thermosetting resin matrix is selected from at least one of epoxy resin, phenolic resin, unsaturated polyester resin, melamine-formaldehyde resin, urea resin, polyurethane, polyimide. The thermosetting resin matrix preferably remains consistent with the shell material of the microcapsules, having good affinity.
According to the heat conductive-lubricating dual-function composite resin of the present invention, preferably, the modified filler is at least one selected from the group consisting of calcium carbonate, clay, kaolin, talc, asbestos, mica, carbon black, calcium sulfate, calcium sulfite, carbon fiber, glass fiber, silica, graphene, carbon nanotube, polytetrafluoroethylene nanoparticle, graphite, molybdenum disulfide, boron nitride, and zirconia. The addition of modified fillers to the thermoset resin matrix can help to improve the strength, toughness, and abrasion resistance of the resin. Specifically, if the modified filler is at least one selected from talcum powder, asbestos, mica, carbon black, calcium sulfate, calcium sulfite, metal powder, molybdenum disulfide, boron nitride, zirconium oxide and polytetrafluoroethylene nano particles, the wear resistance of the resin can be well improved, and if the modified filler is at least one selected from calcium carbonate, clay, kaolin, carbon fiber, glass fiber, silicon dioxide, graphene and carbon nano tube, the strength and toughness of the resin can be well improved at the same time, so that the performance and reliability of the resin are improved.
The invention also provides a preparation method of the heat conduction-lubrication dual-function composite resin, which comprises the following steps:
synthesizing the heat conduction-lubrication dual-function microcapsule;
mixing the thermosetting resin matrix, the modified filler and the heat conduction-lubrication dual-function microcapsule to obtain a mixed raw material;
vacuumizing the mixed raw materials, and pouring and filling a forming space; and then vacuumizing the molding space, and curing to obtain the composite resin.
In the embodiment of the invention, the width of the molding space is set to be 0.1 mm-10 mm for the convenience of experimental test. In practical application, the molding space can be set according to specific requirements.
According to the preparation method of the present invention, preferably, the heat conductive-lubricating dual-function microcapsule has a mass ratio of 0.1% to 50%, preferably 10% to 50%, more preferably 20% to 40%, based on the thermosetting resin matrix.
According to the production method of the present invention, preferably, the mass ratio of the modified filler is 0.1% to 50%, preferably 1% to 20%, more preferably 4% to 10%, based on the thermosetting resin matrix.
According to the production method of the present invention, preferably, the mass ratio of the nano-metal particles is 0.001% to 5%, more preferably 0.1% to 5%, still more preferably 1% to 4%, based on the thermosetting resin matrix.
According to the production method of the present invention, preferably, the vacuum degree of the vacuuming treatment is-0.09 MPa to-0.1 MPa.
According to the production method of the present invention, the temperature of the curing treatment is preferably 40 to 300 ℃, more preferably 80 to 220 ℃.
According to the preparation method of the present invention, preferably, the heat conduction-lubrication dual-function microcapsule is synthesized by a solvent evaporation method. More preferably, the synthesis of the heat-conducting and lubricating dual-function microcapsules comprises the following steps:
and adding the shell material and the core material into a solvent, evaporating the solvent after the shell material solvent forms a stable system, coating the core material with the shell material, and washing and drying to obtain the microcapsule.
The solvent volatilization method has mild reaction conditions, the solvent can be recycled, the resource waste is reduced, and the reaction system is stable.
According to the production method of the present invention, preferably, the solvent is selected from water, ethanol, acetone, and the like.
The composite resin obtained by the preparation method has compact structure, no defects such as cracks and holes, and the like, and the heat conduction performance is greatly improved on the premise of not affecting the mechanical property and the tribological property. The nano metal particles with electromagnetic properties such as nano iron powder, nano cobalt powder and nano nickel powder can be further optimized, the position of the microcapsule in the composite material can be directionally regulated and controlled in an electromagnetic field mode, and the heat dissipation rate of a high-temperature local area is improved.
Drawings
FIG. 1 is a schematic diagram of a heat-conducting and lubricating dual-function microcapsule used in the present invention.
FIG. 2 is a graph showing the friction coefficient of the composite resin material in examples 1 to 3 and comparative example 1.
FIG. 3 is a topography of basalt fibers dispersed in an ethanol solution.
Detailed Description
In order to more clearly illustrate the present invention, the present invention will be further described with reference to preferred embodiments. It is to be understood by persons skilled in the art that the following detailed description is illustrative and not restrictive, and that this invention is not limited to the details given herein.
The invention provides a preparation method of a heat conduction-lubrication dual-function composite resin, which comprises the following steps of referring to table 1 for specific raw materials and the dosage of the embodiment of the invention.
Step 1: preparation of heat-conducting and lubricating double-function microcapsule
The microcapsule is prepared by adopting a solvent volatilization method, firstly, a shell material and a core material are added into a solvent, the shell material is required to be added with the solvent to form a stable system, then the solvent is removed, the wall material is coated on the core material, and the microcapsule is obtained after washing and drying. The method has the advantages of mild reaction conditions, recycling of the solvent, reduction of resource waste and stable reaction system.
Step 2: mixing and fully stirring the thermosetting resin matrix, the modified filler and the heat conduction-lubrication dual-function microcapsule to obtain a mixed raw material.
According to an embodiment of the present invention, the thermosetting resin matrix is selected from at least one of epoxy resin, phenolic resin, unsaturated polyester resin, melamine-formaldehyde resin, urea resin, polyurethane, polyimide. The preparation method can be used for preparing the composite resin material which has good thermal conductivity and is compact and free of void defects, so that the preparation method can be applied to most thermosetting resins and even thermoplastic resins (such as nylon and polyether ether ketone (PEEK)) and has a wide application range.
According to an embodiment of the present invention, the modified filler is selected from at least one of calcium carbonate, clay, kaolin, talc, asbestos, mica, carbon black, calcium sulfate, calcium sulfite, carbon fiber, glass fiber, silica, graphene, carbon nanotubes, polytetrafluoroethylene nanoparticles, graphite, molybdenum disulfide, boron nitride, zirconium oxide. The modified filler can help to improve the strength, toughness and wear resistance of the resin. Specifically, if the modified filler is at least one selected from talcum powder, asbestos, mica, carbon black, calcium sulfate, calcium sulfite, metal powder, molybdenum disulfide, boron nitride, zirconium oxide and polytetrafluoroethylene nano particles, the wear resistance of the resin can be well improved, and if the modified filler is at least one selected from calcium carbonate, clay, kaolin, carbon fiber, glass fiber, silicon dioxide, graphene and carbon nano tube, the strength and toughness of the resin can be well improved at the same time, so that the performance and reliability of the resin are improved.
According to an embodiment of the present invention, the heat conductive-lubricating dual-function microcapsule has a mass ratio of 0.1% to 50%, preferably 10% to 50%, more preferably 20% to 40%, based on the thermosetting resin matrix in mass%.
According to an embodiment of the present invention, the modified filler is present in an amount of 0.1 to 50% by mass, preferably 1 to 20% by mass, more preferably 4 to 10% by mass, based on the thermosetting resin matrix. Therefore, the mass ratio of the modified filler can be flexibly set by the person skilled in the art according to the requirements on the strength and toughness of the resin, the specific materials of the modified filler and other practical conditions, so long as the good usability of the resin is ensured. For example, in some of the following examples, the modified filler is present in a mass ratio of 4.5% to 9%.
According to an embodiment of the present invention, the nano metal particles in the microcapsule are selected from at least one of nano silver powder, nano copper powder, nano molybdenum powder, nano aluminum powder, nano iron powder, nano cobalt powder, and nano nickel powder. The added metal nano particles can effectively improve the heat conducting property of the resin. More preferably, the nano metal particles are at least one selected from nano metal particles with electromagnetic properties, such as nano iron powder, nano cobalt powder, nano nickel powder and the like; because the nano metal particles also have electromagnetic properties, the positions of the microcapsules in the composite material can be directionally regulated and controlled in an electromagnetic field mode, and the heat dissipation rate of a high-temperature local area is improved.
According to an embodiment of the present invention, the mass ratio of the nano metal particles is 0.001% to 5%, more preferably 0.1% to 5%, still more preferably 1% to 4% by mass based on the thermosetting resin matrix.
According to embodiments of the invention, the stirring rate is 10-500 r/min, e.g. 10r/min, 50r/min, 100r/min, 150r/min, 200r/min, 250r/min, 300r/min, 350r/min, 400r/min, 450r/min, 500r/min etc. Therefore, under the condition of the stirring rate, the thermosetting resin matrix and the modified filler can be quickly and uniformly mixed. In some embodiments, at least one of an initiator and a curing agent may be further added to the mixed raw material. Thus, the performance of the resin is further improved; the initiator and the curing agent are specifically selected according to different thermosetting resin matrixes; in the mixed raw materials, the mass ratio of the initiator to the curing agent is 0.1-2% based on the thermosetting resin matrix.
Step 3: vacuumizing the mixed raw materials, and pouring and filling a forming space; and then vacuumizing the molding space, and curing to obtain the composite resin.
The mixed raw materials are vacuumized, so that gas and water molecules in the mixed raw materials can be removed, and the raw materials are fully mixed.
According to an embodiment of the present invention, the vacuum degree of the vacuuming treatment is-0.09 MPa to-0.1 MPa. Thus, the gas and water molecules in the mixed raw material can be removed to the greatest extent.
According to the embodiment of the invention, the width of the molding space is 0.1 mm-10 mm, for example, the width of the molding space is 0.1mm, 0.5mm, 1.0mm, 2mm, 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm, 10mm, etc. for the convenience of experimental test. In practical application, the molding space can be set according to specific requirements.
According to an embodiment of the present invention, the curing treatment is performed at a temperature of 40 to 300 ℃, for example, a curing temperature of 40 ℃, 60 ℃,80 ℃, 100 ℃, 120 ℃, 140 ℃, 160 ℃, 180 ℃, 200 ℃, 300 ℃, etc. In some embodiments, the curing temperature may be 80 to 220 ℃. Thereby, the cured resin can be obtained quickly and efficiently in the above temperature range.
The composite resin prepared by the preparation method comprises a thermosetting resin matrix, modified filler and a heat conduction-lubrication dual-function microcapsule; the heat conduction-lubrication dual-function microcapsule is shown in fig. 1, and has a shell-core structure, wherein the core material of the inner core comprises nano metal particles, lubrication particles and fibers, and the shell material of the outer shell is resin.
The composite resin prepared by the preparation method has compact structure, no defects such as cracks and holes, and the like, and the heat conduction performance is greatly improved on the premise of not affecting the mechanical property and tribological property of the resin. The nano metal particles with electromagnetic properties such as nano iron powder, nano cobalt powder and nano nickel powder can be further optimized, the position of the microcapsule in the composite material can be directionally regulated and controlled in an electromagnetic field mode, and the heat dissipation rate of a high-temperature local area is improved.
The following further provides specific examples illustrating the technical scheme of the present invention:
example 1
The embodiment prepares the heat conduction-lubrication dual-function composite resin, which comprises the following steps:
1) Preparation of a thermally conductive-lubricating bifunctional microcapsule (containing 1g Ag nanoparticle, 3g PTFE nanoparticle):
1g of Ag nano particles, 3g of PTFE nano particles (lubricating particles), 2g of lubricating oil PAO6 and 4g of 901 unsaturated polyester resin monomer are weighed by an electronic balance and mixed to be used as a disperse phase (namely an oil phase);
dispersing 0.5g of surfactant SDS into 90mL of deionized water to form a continuous phase (namely an aqueous phase), and standing by after the SDS is completely dissolved;
the two solutions are added into a three-neck flask in a dropwise manner, magnetic stirring is kept, and the two solutions react for 4 hours at 80 ℃ to form a uniform solution. After the completion of the reaction, the mixture was washed by filtration with deionized water, followed by freeze-drying for 48 hours to obtain capsule powder.
2) 100g of 901 unsaturated polyester resin, 2.5g of carbon fiber and 2g of silicon dioxide are added into a 250mL beaker, 1g of curing agent methyl ethyl ketone peroxide, 0.5g of catalyst cobalt stearate and 20g of microcapsule (containing 2g of Ag nano particles and 6g of PTFE nano particles) are added, and the mixture is stirred uniformly to obtain a mixed raw material;
3) Vacuumizing the mixed raw materials to obtain a pretreated raw material mixture; pouring the pretreated raw material mixture into a forming space, and filling the forming space; wherein, the vacuum degree after the vacuuming treatment is-0.99 MPa; and vacuumizing the forming space filled with the pretreatment raw material mixture, and curing at a curing temperature of 100 ℃ to finally obtain the composite resin sample 1.
Example 2
The embodiment prepares the heat conduction-lubrication dual-function composite resin, which comprises the following steps:
1) Preparation of a thermally conductive-lubricating bifunctional microcapsule (containing 1g Cu nanoparticle, 3g PTFE nanoparticle):
referring to the preparation process of the microcapsule in example 1, the Ag nanoparticles replaced therein were Cu nanoparticles.
2) 100g of 901 unsaturated polyester resin, 2.5g of carbon fiber and 2g of silicon dioxide are added into a 250mL beaker, 1g of curing agent methyl ethyl ketone peroxide, 0.5g of catalyst cobalt stearate and 20g of microcapsule (containing 2g of Cu nano particles and 6g of PTFE nano particles) are added, and the mixture is stirred uniformly to obtain a mixed raw material; vacuumizing the mixed raw materials to obtain a pretreated raw material mixture; pouring the pretreatment raw material mixture into a forming space, and filling the forming space; wherein, the vacuum degree after the vacuuming treatment is-0.99 MPa; and vacuumizing the forming space filled with the pretreatment raw material mixture, and curing at a curing temperature of 100 ℃ to finally obtain a composite resin sample 2.
Example 3
The embodiment prepares the heat conduction-lubrication dual-function composite resin, which comprises the following steps:
1) Preparation of a thermally conductive-lubricating bifunctional microcapsule (containing 1g Mo nanoparticle, 3g PTFE nanoparticle):
referring to the preparation process of the microcapsule in example 1, ag nanoparticles replaced therein were Mo nanoparticles.
2) 50g of 901 unsaturated polyester resin, 2.5g of carbon fiber and 2g of silicon dioxide are added into a 250mL beaker, 1g of curing agent methyl ethyl ketone peroxide, 0.5g of catalyst cobalt stearate and 20g of microcapsule (containing 2g of Mo nano particles and 6g of PTFE nano particles) are added, and the mixture is stirred uniformly to obtain a mixed raw material; vacuumizing the mixed raw materials to obtain a pretreated raw material mixture; pouring the pretreatment raw material mixture into a forming space, and filling the forming space; wherein, the vacuum degree after the vacuuming treatment is-0.99 MPa; and vacuumizing the forming space filled with the pretreatment raw material mixture, and curing at a curing temperature of 100 ℃ to finally obtain a composite resin sample 3.
Example 4
The embodiment prepares the heat conduction-lubrication dual-function composite resin, which comprises the following steps:
1) Preparation of a thermally conductive-lubricating bifunctional microcapsule (containing 1g Fe nanoparticle, 6g PTFE nanoparticle):
referring to the preparation process of the microcapsule in example 1, the Ag nanoparticles replaced therein were Fe nanoparticles.
2) 50g of 901 unsaturated polyester resin, 2.5g of carbon fiber and 2g of silicon dioxide are added into a 250mL beaker, 1g of curing agent methyl ethyl ketone peroxide, 0.5g of catalyst cobalt stearate and 20g of microcapsule (containing 6g of Fe nano particles and 6g of PTFE nano particles) are added, and the mixture is stirred uniformly to obtain a mixed raw material; vacuumizing the mixed raw materials to obtain a pretreated raw material mixture; pouring the pretreatment raw material mixture into a forming space, and filling the forming space; wherein, the vacuum degree after the vacuuming treatment is-0.99 MPa; and vacuumizing the forming space filled with the pretreatment raw material mixture, and curing at a curing temperature of 100 ℃ to finally obtain a composite resin sample 4.
Comparative example 1
50g of 901 unsaturated polyester resin, 2.5g of carbon fiber, 6g of PTFE nano particles and 2g of silicon dioxide are added into a 250mL beaker, 1g of curing agent methyl ethyl ketone peroxide and 0.5g of catalyst cobalt stearate are added, and microcapsules are not added, and the mixture is stirred uniformly to obtain a mixed raw material; vacuumizing the mixed raw materials to obtain a pretreated raw material mixture; pouring the pretreatment raw material mixture into a forming space, and filling the forming space; wherein, the vacuum degree after the vacuuming treatment is-0.99 MPa; and vacuumizing the forming space filled with the pretreatment raw material mixture, and curing at a curing temperature of 100 ℃ to finally obtain the composite resin comparative sample 1.
Table 1 shows the respective raw materials and the proportions thereof used in the respective examples and comparative examples, and table 2 shows the thermal conductivity coefficients of the composite resin materials obtained in the examples and comparative examples.
Table 1 actual proportions of the composite resin materials (based on 100% of the thermosetting resin matrix)
Table 2 thermal conductivity of composite resin materials in examples and comparative examples
| Thermal conductivity W/(m.K) | |
| Example 1 | 2.346 |
| Example 2 | 2.105 |
| Example 3 | 1.965 |
| Example 4 | 2.431 |
| Comparative example 1 | 0.763 |
The thermal conductivity was measured using a thermal conductivity meter in table 2, and the results showed that the thermal conductivity of the microcapsule-added composite resin of the example was significantly better than that of the comparative example without addition.
Fig. 2 is a graph showing friction coefficients of the composite resin materials of example 1, example 3 and comparative example 1. The friction coefficient was measured using a PLINT frictional wear tester, and FIG. 2 shows that after the addition of metal particles, the friction coefficient was not significantly increased, whereas the thermal conductivity in Table 2 was significantly increased, and the thermal conductivity was enhanced without affecting other properties.
Example 5
This example differs from example 4 in that 2g basalt fiber was further added to the dispersed phase (i.e., oil phase) to further increase the strength when preparing microcapsules.
Basalt fibers are dispersed in an ethanol solution, the morphology of which is shown in fig. 3, and which shows crosslinked fine fibers, in which various mineral particles are entrained.
The coefficient of thermal conductivity of the composite resin obtained after basalt fiber is added is 2.425W/(m.K), and the coefficient of friction is 0.07-0.11.
It should be understood that the foregoing examples of the present invention are provided merely for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention, and that various other changes and modifications may be made therein by one skilled in the art without departing from the spirit and scope of the present invention as defined by the appended claims.
Claims (14)
1. The heat conduction-lubrication dual-function composite resin is characterized by comprising a thermosetting resin matrix, 0.1-50% of modified filler and 0.1-50% of heat conduction-lubrication dual-function microcapsule, wherein the mass of the thermosetting resin matrix is 100%;
the core material of the heat conduction-lubrication dual-function microcapsule comprises nano metal particles and lubricating oil, and the shell material is resin;
in the heat conduction-lubrication dual-function microcapsule, the mass ratio of the nano metal particles is 1-10%, the mass ratio of the lubricating oil is 10-20%, and the balance is a resin shell material.
2. The heat conductive-lubricating dual-function composite resin according to claim 1, wherein the mass ratio of the nano-metal particles is 0.001% to 5% based on 100% of the mass of the thermosetting resin matrix.
3. The heat conducting-lubricating dual function composite resin of claim 1, wherein the core material of the heat conducting-lubricating dual function microcapsule further comprises lubricating particles;
in the heat conduction-lubrication dual-function microcapsule, the mass ratio of the lubrication particles is 10% -30%.
4. A heat-conducting-lubricating dual-function composite resin according to claim 1 or 3, wherein the core material of the heat-conducting-lubricating dual-function microcapsule further comprises fibers;
in the heat conduction-lubrication dual-function microcapsule, the mass ratio of the fiber is 10% -20%.
5. The heat conductive-lubricating dual-function composite resin according to claim 1, wherein the shell material adopts at least one of epoxy resin, phenolic resin, unsaturated polyester resin, melamine-formaldehyde resin, urea-formaldehyde resin, polyurethane and polyimide.
6. The heat conduction-lubrication dual-function composite resin according to claim 1, wherein the nano metal particles are at least one selected from nano silver powder, nano copper powder, nano molybdenum powder, nano aluminum powder, nano iron powder, nano cobalt powder, and nano nickel powder;
preferably, the nano metal particles are at least one selected from nano iron powder, nano cobalt powder and nano nickel powder.
7. A thermally conductive-lubricious dual function composite resin as in claim 3 wherein the lubricious particles are selected from at least one of graphene, carbon nanotubes, polytetrafluoroethylene nanoparticles, graphite, molybdenum disulfide.
8. The heat conductive-lubricating dual-function composite resin of claim 4, wherein the fibers are selected from at least one of carbon fibers, glass fibers, basalt fibers.
9. The heat conductive-lubricating dual-function composite resin according to claim 1, wherein the thermosetting resin matrix is selected from at least one of epoxy resin, phenolic resin, unsaturated polyester resin, melamine-formaldehyde resin, urea-formaldehyde resin, polyurethane, polyimide.
10. The heat conducting-lubricating dual-function composite resin according to claim 1, wherein the modified filler is at least one selected from the group consisting of calcium carbonate, clay, kaolin, talc, asbestos, mica, carbon black, calcium sulfate, calcium sulfite, carbon fiber, glass fiber, silica, graphene, carbon nanotubes, polytetrafluoroethylene nanoparticles, graphite, molybdenum disulfide, boron nitride, and zirconia.
11. A method for preparing the heat conduction-lubrication dual-function composite resin according to any one of claims 1 to 10, characterized in that the method comprises the following steps:
synthesizing the heat conduction-lubrication dual-function microcapsule;
mixing the thermosetting resin matrix, the modified filler and the heat conduction-lubrication dual-function microcapsule to obtain a mixed raw material;
vacuumizing the mixed raw materials, and pouring and filling a forming space; and then vacuumizing the molding space, and curing to obtain the composite resin.
12. The production method according to claim 11, wherein the vacuum degree of the vacuuming treatment is-0.09 MPa to-0.1 MPa.
13. The method according to claim 11, wherein the temperature of the curing treatment is 40 to 300 ℃.
14. The method of claim 11, wherein the thermally conductive-lubricious dual function microcapsules are synthesized using a solvent evaporation process.
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