CN113105732A - Resin-based composite material with high thermal conductivity and preparation method thereof - Google Patents
Resin-based composite material with high thermal conductivity and preparation method thereof Download PDFInfo
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- CN113105732A CN113105732A CN202110396124.6A CN202110396124A CN113105732A CN 113105732 A CN113105732 A CN 113105732A CN 202110396124 A CN202110396124 A CN 202110396124A CN 113105732 A CN113105732 A CN 113105732A
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- antioxidant
- resin
- heat
- conducting
- composite material
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- 239000000463 material Substances 0.000 title claims abstract description 132
- 239000000805 composite resin Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 40
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 118
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 117
- 239000011347 resin Substances 0.000 claims abstract description 106
- 229920005989 resin Polymers 0.000 claims abstract description 106
- 239000000314 lubricant Substances 0.000 claims abstract description 91
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 70
- 239000000945 filler Substances 0.000 claims abstract description 63
- 239000012745 toughening agent Substances 0.000 claims abstract description 54
- 239000002994 raw material Substances 0.000 claims abstract description 27
- 239000012783 reinforcing fiber Substances 0.000 claims abstract description 25
- 238000002156 mixing Methods 0.000 claims description 57
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 26
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 24
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 claims description 24
- 239000000178 monomer Substances 0.000 claims description 23
- 239000000843 powder Substances 0.000 claims description 23
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical group CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 20
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical group CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 20
- 239000000835 fiber Substances 0.000 claims description 16
- TXQVDVNAKHFQPP-UHFFFAOYSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(CO)(CO)CO TXQVDVNAKHFQPP-UHFFFAOYSA-N 0.000 claims description 13
- 239000004593 Epoxy Substances 0.000 claims description 12
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 12
- 239000005639 Lauric acid Substances 0.000 claims description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 12
- 239000003365 glass fiber Substances 0.000 claims description 12
- 239000008187 granular material Substances 0.000 claims description 12
- 239000007795 chemical reaction product Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 11
- 239000000376 reactant Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 230000004580 weight loss Effects 0.000 claims description 11
- 239000002041 carbon nanotube Substances 0.000 claims description 10
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 10
- 229920001577 copolymer Polymers 0.000 claims description 10
- 239000011258 core-shell material Substances 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical group CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 claims description 8
- SYEWHONLFGZGLK-UHFFFAOYSA-N 2-[1,3-bis(oxiran-2-ylmethoxy)propan-2-yloxymethyl]oxirane Chemical compound C1OC1COCC(OCC1OC1)COCC1CO1 SYEWHONLFGZGLK-UHFFFAOYSA-N 0.000 claims description 8
- 229910021389 graphene Inorganic materials 0.000 claims description 6
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 5
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 5
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 claims description 5
- 239000004917 carbon fiber Substances 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 4
- 239000012188 paraffin wax Substances 0.000 claims description 4
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- DCXXMTOCNZCJGO-UHFFFAOYSA-N tristearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCCCCCCCCCC)COC(=O)CCCCCCCCCCCCCCCCC DCXXMTOCNZCJGO-UHFFFAOYSA-N 0.000 claims description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- QYMGIIIPAFAFRX-UHFFFAOYSA-N butyl prop-2-enoate;ethene Chemical compound C=C.CCCCOC(=O)C=C QYMGIIIPAFAFRX-UHFFFAOYSA-N 0.000 claims description 3
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 3
- YYXLGGIKSIZHSF-UHFFFAOYSA-N ethene;furan-2,5-dione Chemical compound C=C.O=C1OC(=O)C=C1 YYXLGGIKSIZHSF-UHFFFAOYSA-N 0.000 claims description 3
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- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 3
- 239000000347 magnesium hydroxide Substances 0.000 claims description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 3
- 239000000395 magnesium oxide Substances 0.000 claims description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 3
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 229920001897 terpolymer Polymers 0.000 claims description 3
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 3
- QMMJWQMCMRUYTG-UHFFFAOYSA-N 1,2,4,5-tetrachloro-3-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=C(Cl)C(Cl)=CC(Cl)=C1Cl QMMJWQMCMRUYTG-UHFFFAOYSA-N 0.000 claims description 2
- PZRWFKGUFWPFID-UHFFFAOYSA-N 3,9-dioctadecoxy-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane Chemical compound C1OP(OCCCCCCCCCCCCCCCCCC)OCC21COP(OCCCCCCCCCCCCCCCCCC)OC2 PZRWFKGUFWPFID-UHFFFAOYSA-N 0.000 claims description 2
- HCILJBJJZALOAL-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)-n'-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyl]propanehydrazide Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 HCILJBJJZALOAL-UHFFFAOYSA-N 0.000 claims description 2
- VSAWBBYYMBQKIK-UHFFFAOYSA-N 4-[[3,5-bis[(3,5-ditert-butyl-4-hydroxyphenyl)methyl]-2,4,6-trimethylphenyl]methyl]-2,6-ditert-butylphenol Chemical compound CC1=C(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)C(C)=C(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)C(C)=C1CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 VSAWBBYYMBQKIK-UHFFFAOYSA-N 0.000 claims description 2
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 2
- UAUDZVJPLUQNMU-UHFFFAOYSA-N Erucasaeureamid Natural products CCCCCCCCC=CCCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-UHFFFAOYSA-N 0.000 claims description 2
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 claims description 2
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 229920003182 Surlyn® Polymers 0.000 claims description 2
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 2
- BEIOEBMXPVYLRY-UHFFFAOYSA-N [4-[4-bis(2,4-ditert-butylphenoxy)phosphanylphenyl]phenyl]-bis(2,4-ditert-butylphenoxy)phosphane Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(C=1C=CC(=CC=1)C=1C=CC(=CC=1)P(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C BEIOEBMXPVYLRY-UHFFFAOYSA-N 0.000 claims description 2
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims description 2
- 229920001971 elastomer Polymers 0.000 claims description 2
- UAUDZVJPLUQNMU-KTKRTIGZSA-N erucamide Chemical compound CCCCCCCC\C=C/CCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-KTKRTIGZSA-N 0.000 claims description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 2
- 229920006244 ethylene-ethyl acrylate Polymers 0.000 claims description 2
- VOZRXNHHFUQHIL-UHFFFAOYSA-N glycidyl methacrylate Chemical compound CC(=C)C(=O)OCC1CO1 VOZRXNHHFUQHIL-UHFFFAOYSA-N 0.000 claims description 2
- 229940057995 liquid paraffin Drugs 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- 239000012170 montan wax Substances 0.000 claims description 2
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 2
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 claims description 2
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 claims description 2
- 239000004209 oxidized polyethylene wax Substances 0.000 claims description 2
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- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
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- 239000002131 composite material Substances 0.000 abstract description 16
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- 125000003700 epoxy group Chemical group 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- KUDUQBURMYMBIJ-UHFFFAOYSA-N 2-prop-2-enoyloxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC(=O)C=C KUDUQBURMYMBIJ-UHFFFAOYSA-N 0.000 description 1
- 241000227129 Aconitum Species 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910001369 Brass Inorganic materials 0.000 description 1
- 229910000906 Bronze Inorganic materials 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- DYAHQFWOVKZOOW-UHFFFAOYSA-N Sarin Chemical compound CC(C)OP(C)(F)=O DYAHQFWOVKZOOW-UHFFFAOYSA-N 0.000 description 1
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- 230000015556 catabolic process Effects 0.000 description 1
- 239000011231 conductive filler Substances 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
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Classifications
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- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
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- C08K3/04—Carbon
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Abstract
The invention relates to the technical field of heat-conducting high polymer materials, in particular to a resin-based composite material with high heat conductivity and a preparation method thereof, wherein the resin-based composite material with high heat conductivity comprises the following raw materials: the resin matrix is used as a main body, and the added heat-conducting master batch, the antioxidant, the lubricant A, the reinforcing fiber, the toughening agent and other auxiliary agents improve the overall processability, mechanical property and heat-conducting property of the resin matrix composite material. The special heat-conducting master batch is added to enable the resin base material to be firmly connected with the resin base material in an anchoring mode, the lubricating and dispersing effects in the system are better, the heat-conducting filler is prevented from agglomerating to form a heat-conducting network, and therefore the purpose that the heat-conducting filler with lower using amount is used for keeping higher heat conductivity and better mechanical property is achieved.
Description
Technical Field
The invention relates to the technical field of heat-conducting high polymer materials, in particular to a resin-based composite material with high heat conductivity and a preparation method thereof.
Background
The existing electronic components have certain internal resistance, heat can be generated as long as current passes through the components, and if the temperature is too high, the components are easily burnt out, so that a radiator can be added to a high-power device in many times. For example, MOS transistors of switching power supplies or power tools are equipped with heat dissipation devices; when the high-power LED for illumination works, a large amount of heat is also generated, if the heat is not dissipated timely, the LED lamp beads are burnt out, and a heat dissipation device is also required to be installed; the CPU of the computer has very high working frequency and high heat productivity, and a fan is also arranged for assisting heat dissipation besides a radiator is required to be arranged.
The radiating fin is a device for radiating heat of an easily-heating electronic element in an electric appliance, and is made of aluminum alloy, brass or bronze into a plate shape, a sheet shape, a plurality of sheet shapes and the like. However, the production process of the metal heat sink is complex, the production cost is high, and the weight of the heat sink is increased due to the excessively high specific gravity of the metal, which results in a high total weight of the components.
The resin-based heat-conducting composite material can overcome the defects of the heat dissipation part made of the metal material, can be formed at one time through injection molding, does not need complicated processing flows such as metal cutting and polishing, and is low in material cost. However, the heat dissipation element made of the existing resin-based heat conduction composite material has poor heat conduction effect, and if the addition amount of the heat conduction material is increased, the mechanical property is easily affected.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide a resin-based composite material with high thermal conductivity.
The invention also aims to provide a preparation method of the resin-based composite material with high thermal conductivity, which has the advantages of simple operation, convenient control, high production efficiency and low production cost and can be used for large-scale production.
The purpose of the invention is realized by the following technical scheme: a resin-based composite material with high thermal conductivity comprises the following raw materials in parts by weight:
the resin-based composite material disclosed by the invention takes a resin base material as a main body, and is added with auxiliary agents such as the heat-conducting master batch, the antioxidant, the lubricant A, the reinforcing fiber and the toughening agent, so that the overall processability, the mechanical property and the heat-conducting property of the resin-based composite material are improved. The special heat-conducting master batch is added to enable the resin base material to be firmly connected with the resin base material in an anchoring mode, the lubricating and dispersing effects in the system are better, the heat-conducting filler is prevented from agglomerating to form a heat-conducting network, and therefore the purpose that the heat-conducting filler with lower using amount is used for keeping higher heat conductivity and better mechanical property is achieved.
Preferably, the heat-conducting master batch comprises the following raw materials in parts by weight:
By adopting the technical scheme, the resin base material, the heat-conducting filler, the antioxidant and the lubricant B are used for preparing the heat-conducting master batch, and the heat-conducting master batch is added into the resin-based composite material with high heat conductivity for secondary processing, so that the uniform dispersion of the heat-conducting filler is promoted, and a stable heat-conducting network is formed.
Preferably, the resin substrate is at least one of PA6 resin, PA66 resin, PBT resin, PC resin, ABS resin, PP resin, and PS resin. Further, the intrinsic viscosity of the PA6 resin ranges from 1.8 to 2.4dl/g, the intrinsic viscosity of the PA66 resin ranges from 2.4 to 3.0dl/g, the intrinsic viscosity of the PBT resin ranges from 0.8 to 1.0dl/g, the PC resin melt index (260 ℃/2.16kg) ranges from 10 to 15g/10min, the ABS resin is selected from Qimei PA-757, PA-758 or PA-765A, the PP resin is selected from K8303, K7726, K8025, K9927, T30S or HP500N, and the PS resin is selected from Qimei PG-80N, GP5250 or Taiwan PG-383M.
Preferably, the heat conductive filler is at least one of magnesium hydroxide powder, aluminum hydroxide powder, magnesium oxide powder, aluminum oxide powder, zirconium oxide powder, silicon carbide powder, aluminum nitride micro powder, zinc oxide micro powder, hexagonal boron nitride micro powder, nano silver micro powder, graphite oxide, carbon nano tube, graphene oxide, nano aluminum powder and nano copper powder.
By adopting the technical scheme, the heat conduction and heat dissipation effects of the heat conduction and heat dissipation material are conveniently dispersed in the resin base material to form a heat conduction network. More preferably, the heat-conducting filler is a combination of at least two of magnesium hydroxide powder, aluminum hydroxide powder, magnesium oxide powder, aluminum oxide powder, zirconium oxide powder, silicon carbide powder, aluminum nitride powder, zinc oxide powder, hexagonal boron nitride powder, nano silver powder, graphite oxide, carbon nano tubes, graphene oxide, nano aluminum powder and nano copper powder, and the heat-conducting effect is better. The particle size of the heat-conducting filler is 50nm-10000 nm.
Preferably, the antioxidant A and the antioxidant B are both compounded by a main antioxidant and an auxiliary antioxidant according to the weight ratio of 1: 2-3; the primary antioxidant is antioxidant 1076, antioxidant 1010, antioxidant 1098, antioxidant 264, antioxidant 330 or antioxidant 1024, and the secondary antioxidant is antioxidant 168, antioxidant 618, antioxidant 626, antioxidant S9228, antioxidant PEPQ, antioxidant PEP36 or antioxidant 412S.
By adopting the technical scheme, the autoxidation reaction rate of the composite material can be effectively reduced, the aging and degradation of the composite material can be delayed, the antioxidant effect can be prevented from being not achieved due to the decomposition of the antioxidant caused by high temperature in the preparation process of the composite material, the thermal decomposition of the composite material in the extrusion process can be reduced, and the micromolecule precipitation of the material in the process can be reduced.
Preferably, the preparation method of the lubricant B comprises the following steps:
(R1), mixing lauric acid, ethylenediamine, active monomer and ammonium persulfate uniformly according to the weight ratio of 100:10-14:4-8: 1;
(R2), continuously stirring and keeping the temperature at the temperature of 180-230 ℃ for reaction for 11-15min to obtain a reactant;
(R3) and devolatilizing the reaction product to obtain lubricant B having an epoxy equivalent of 150-300.
By adopting the technical scheme, lauric acid, ethylenediamine, an active monomer and ammonium persulfate are mixed according to a specific proportion and then react to obtain the lubricant B with the epoxy equivalent of 150-300, and an epoxy group of the lubricant can simultaneously generate a physical and chemical reaction with an active group on the surface of the heat-conducting filler and a resin base material, so that the lubricating dispersion of the heat-conducting filler in master batches is promoted, and the processing performance of the material is improved; meanwhile, the heat-conducting filler which is firmly anchored with the resin base material is generated in the heat-conducting master batch, and can be dispersed more uniformly after secondary processing, so that a perfect heat-conducting network can be formed on the composite material under the condition of a lower adding proportion of the heat-conducting filler, and higher heat conductivity is kept.
Preferably, the reactive monomer is allyl glycidyl ether and/or glycerol triglycidyl ether.
By adopting the technical scheme, the reaction is promoted and the epoxy group is obtained. The composite material with good processing dispersion has the characteristics of small addition amount of the heat-conducting filler, heat conductivity coefficient of more than 2.0W/(m.K), good physical and mechanical properties, capability of meeting the use requirements in the field of heat dissipation and low production cost.
Preferably, the preparation method of the heat-conducting master batch comprises the following steps:
(B1) taking a resin base material, a heat-conducting filler, an antioxidant and a lubricant B according to parts by weight for later use;
(B2) adding the resin base material, the heat-conducting filler, the antioxidant and the lubricant B into a preheated internal mixer for mixing for 2-6min, cooling and crushing into granules to obtain the heat-conducting master batch.
By adopting the technical scheme, the resin base material, the heat-conducting filler, the antioxidant and the lubricant B are mixed and crushed into granules, and then are added into the process of preparing the resin-based composite material with high heat conductivity for secondary processing, so that the dispersion of the heat-conducting filler is promoted, and the heat-conducting filler with low addition amount still maintains the high heat conductivity and maintains better mechanical property. Further, the mixing temperature of the internal mixer is 200-300 ℃, and the particle size of the heat-conducting master batch is 0.1-10 mm.
Preferably, the lubricant A is at least one of pentaerythritol stearate, N' -ethylene bis-stearamide, oleamide, erucamide, butyl stearate, glycerol tristearate, microcrystalline paraffin, liquid paraffin, chlorinated paraffin, polyethylene wax, oxidized polyethylene wax, methyl silicone oil, benzyl silicone oil, ethyl silicone oil and montan wax; the reinforcing fiber is chopped glass fiber, chopped carbon fiber or stainless steel fiber; the toughening agent is at least one of MBS type toughening agent with a core-shell structure, ACR type toughening agent with a core-shell structure, ethylene-octene copolymer grafted glycidyl methacrylate, ethylene-acrylate-glycidyl methacrylate terpolymer, ethylene maleic anhydride binary copolymer, ethylene-octene copolymer, ethylene-butyl acrylate copolymer, ethylene-methyl acrylate copolymer, ethylene-ethyl acrylate copolymer, high rubber powder, ethylene-octene copolymer grafted maleic anhydride and surlyn resin.
By adopting the technical scheme, the lubricant A is adopted so as to improve the processing performance of the material and promote the fluidity of the material in equipment. The added reinforced fiber and the toughening agent have synergistic effect, so that the mechanical property of the material is improved. Furthermore, the diameter of the glass fiber monofilament is 7-12 μm, the length of the glass fiber monofilament is 3-6mm, the diameter of the carbon fiber monofilament is 6-9 μm, the length of the carbon fiber monofilament is 5-9mm, the stainless steel fiber is continuous fiber, and the diameter of the monofilament is 0.02-0.1 mm. The MBS or ACR type toughening agent with a core-shell structure is selected from a group consisting of a Brillouin M701, a M732, an MR502, a M521, a Dow EXL2620, an EXL2690, an EXL2691, a Mitsubishi S2501, an SX006 or an S2100, the ethylene-acrylate-glycidyl methacrylate terpolymer is selected from a group consisting of an Acoma AX8900, an AX8700, an AX8750, an AX8840, a DuPont PTW or 4170, the ethylene maleic anhydride bipolymer is selected from a group consisting of Dupont A560, an M603 or an M623, the ethylene-octene copolymer is selected from a group consisting of a Dow 8100, an 8150, an 8200 or an 8440, the ethylene-butyl acrylate copolymer is selected from an Acoma 35BA 1330, a 35BA40T, a 35BA320, a 28BA175, a Dupont 347, a Dupont 3427 or a 35, the ethylene-methyl acrylate copolymer is selected from an Acoma 24MA005, a group consisting of an ethylene-acrylate 08, a group consisting of an ethylene-acrylate copolymer, an ethylene-acrylate-grafted copolymer is selected from an Aconitum 181, a group consisting of an HR-3405, a group consisting of an ethylene, N493, N416 or mitsui chemical MA8150, sarin resin selected from dupont 8150, 8320, 9120 or AD 8545.
The other purpose of the invention is realized by the following technical scheme: the preparation method of the resin-based composite material with high thermal conductivity comprises the following steps:
(S1) taking the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A, the toughening agent and the reinforcing fiber according to the parts by weight for later use;
(S2) mixing the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A and the toughening agent for 10-30min to obtain a premix;
(S3) extruding and granulating the premix by a double-screw extruder, and adding the reinforced fibers by a weight loss scale through side feeding to obtain the resin-based composite material with high thermal conductivity.
Further, in the step (S3), the length-diameter ratio of the screw of the twin-screw extruder is 48:1, and the temperatures of the sections of the twin-screw extruder from the feeding section are 200-.
The invention has the beneficial effects that: the resin-based composite material with high thermal conductivity provided by the invention takes the resin base material as a main body, and the added heat-conducting master batches, the antioxidant, the lubricant A, the reinforcing fiber, the toughening agent and other auxiliaries are used for improving the overall processability, the mechanical property and the heat-conducting property of the resin-based composite material. The special heat-conducting master batch is added to enable the resin base material to be firmly connected with the resin base material in an anchoring mode, the lubricating and dispersing effects in the system are better, the heat-conducting filler is prevented from agglomerating to form a heat-conducting network, and therefore the purpose that the heat-conducting filler with lower using amount is used for keeping higher heat conductivity and better mechanical property is achieved.
The preparation method of the resin-based composite material with high thermal conductivity is simple to operate, convenient to control, high in production efficiency and low in production cost, and can be used for large-scale production.
Detailed Description
The present invention will be further described with reference to the following examples for facilitating understanding of those skilled in the art, and the description of the embodiments is not intended to limit the present invention.
Example 1
A resin-based composite material with high thermal conductivity comprises the following raw materials in parts by weight:
the heat-conducting master batch comprises the following raw materials in parts by weight:
the resin base material is PC resin with a melt index (260 ℃/2.16kg) of 13g/10 min.
The heat conducting filler is formed by mixing graphite with the particle size of 8 mu m and graphene with the particle size of 80nm according to the weight ratio of 2: 1.
The antioxidant A is prepared by compounding an antioxidant 1076 and an auxiliary antioxidant according to the weight ratio of 1:2.7, and the auxiliary antioxidant is prepared by mixing an antioxidant 168 and an antioxidant 412S according to the weight ratio of 3: 1; the antioxidant B is prepared by compounding an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:2.
The preparation method of the lubricant B comprises the following steps:
(R1), mixing lauric acid, ethylenediamine, active monomer and ammonium persulfate uniformly according to the weight ratio of 100:12:6: 1;
(R2), continuously stirring and keeping the temperature at 200 ℃ for reacting for 13min to obtain a reactant;
(R3) and devolatilization of the reaction product to obtain lubricant B having an epoxy equivalent of 180.
The reactive monomer is allyl glycidyl ether.
The preparation method of the heat-conducting master batch comprises the following steps:
(B1) taking a resin base material, a heat-conducting filler, an antioxidant and a lubricant B according to parts by weight for later use;
(B2) adding the resin base material, the heat-conducting filler, the antioxidant and the lubricant B into a preheated internal mixer, mixing for 5min at 240 ℃ and at 30/25 (front/rear) rotor speed, cooling and crushing into granules to obtain the heat-conducting master batch with the particle size of 5 mm.
The lubricant A is pentaerythritol stearate.
The reinforcing fiber is chopped glass fiber with monofilament diameter of 10 mu m and length of 4 mm.
The toughening agent is the Brillouin M701.
The preparation method of the resin-based composite material with high thermal conductivity comprises the following steps:
(S1) taking the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A, the toughening agent and the reinforcing fiber according to the parts by weight for later use;
(S2) mixing the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A and the toughening agent for 20min to obtain a premix;
(S3) extruding and granulating the premix by a double-screw extruder, and adding the reinforced fibers by a weight loss scale through side feeding to obtain the resin-based composite material with high thermal conductivity.
Wherein, in the step (S3), the length-diameter ratio of the screw of the double screw extruder is 48:1, the temperature of each section of the double screw extruder from the feeding section is 250 ℃, 260 ℃, 270 ℃, 260 ℃, the die temperature is 260 ℃, and the screw rotating speed is 450 rpm.
Example 2
A resin-based composite material with high thermal conductivity comprises the following raw materials in parts by weight:
the heat-conducting master batch comprises the following raw materials in parts by weight:
the resin base material is PC resin. The PC resin melt index (260 ℃/2.16kg) was 13g/10 min.
The heat-conducting filler is formed by mixing graphite with the particle size of 8 mu m and carbon nano tubes with the particle size of 100nm according to the weight ratio of 2: 1.
The antioxidant A is prepared by compounding an antioxidant 1076 and an auxiliary antioxidant according to the weight ratio of 1:2.7, and the auxiliary antioxidant is prepared by mixing an antioxidant 168 and an antioxidant 412S according to the weight ratio of 3: 1; the antioxidant B is prepared by compounding an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:2.
The preparation method of the lubricant B comprises the following steps:
(R1), mixing lauric acid, ethylenediamine, active monomer and ammonium persulfate uniformly according to the weight ratio of 100:12:6: 1;
(R2), continuously stirring and keeping the temperature at 200 ℃ for reacting for 13min to obtain a reactant;
(R3) and devolatilizing the reaction product to obtain lubricant B having an epoxy equivalent of 200.
The active monomer is glycerol triglycidyl ether.
The preparation method of the heat-conducting master batch comprises the following steps:
(B1) taking a resin base material, a heat-conducting filler, an antioxidant and a lubricant B according to parts by weight for later use;
(B2) adding the resin base material, the heat-conducting filler, the antioxidant and the lubricant B into a preheated internal mixer, mixing for 5min at 240 ℃ and at 30/25 (front/rear) rotor speed, cooling and crushing into granules to obtain the heat-conducting master batch with the particle size of 5 mm.
The lubricant A is pentaerythritol stearate.
The reinforcing fiber is chopped glass fiber with monofilament diameter of 10 μm and length of 4 mm.
The toughening agent is a core-shell structure toughening agent M701.
The preparation method of the resin-based composite material with high thermal conductivity comprises the following steps:
(S1) taking the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A, the toughening agent and the reinforcing fiber according to the parts by weight for later use;
(S2) mixing the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A and the toughening agent for 20min to obtain a premix;
(S3) extruding and granulating the premix by a double-screw extruder, and adding the reinforced fibers by a weight loss scale through side feeding to obtain the resin-based composite material with high thermal conductivity.
Wherein, in the step (S3), the length-diameter ratio of the screw of the double screw extruder is 48:1, the temperature of each section of the double screw extruder from the feeding section is 250 ℃, 260 ℃, 270 ℃, 260 ℃, the die temperature is 250 ℃, and the screw rotating speed is 450 rpm.
Example 3
A resin-based composite material with high thermal conductivity comprises the following raw materials in parts by weight:
the heat-conducting master batch comprises the following raw materials in parts by weight:
the resin base material is PC resin. The PC resin melt index (260 ℃/2.16kg) was 10g/10 min.
The heat conducting filler is formed by mixing carbon nano tubes with the particle size of 100nm and graphene with the particle size of 60nm according to the weight ratio of 1: 1.
The antioxidant A is prepared by compounding an antioxidant 1076 and an auxiliary antioxidant according to the weight ratio of 1:2.7, and the auxiliary antioxidant is prepared by mixing an antioxidant 168 and an antioxidant 412S according to the weight ratio of 3: 1; the antioxidant B is prepared by compounding an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:2.
The preparation method of the lubricant B comprises the following steps:
(R1), mixing lauric acid, ethylenediamine, active monomer and ammonium persulfate uniformly according to the weight ratio of 100:10:8: 1;
(R2), continuously stirring and keeping the temperature at 200 ℃ for reacting for 13min to obtain a reactant;
(R3) and devolatilizing the reaction product to obtain lubricant B having an epoxy equivalent of 250.
The active monomer is allyl glycidyl ether and/or glycerol triglycidyl ether.
The preparation method of the heat-conducting master batch comprises the following steps:
(B1) taking a resin base material, a heat-conducting filler, an antioxidant and a lubricant B according to parts by weight for later use;
(B2) adding the resin base material, the heat-conducting filler, the antioxidant and the lubricant B into a preheated internal mixer, cooling and crushing into granules under the conditions of 260 ℃ and 30/25 rotor speed (front/rear), thus obtaining the heat-conducting master batch with the particle size of 5 mm.
The lubricant A is pentaerythritol stearate.
The reinforcing fiber is chopped glass fiber with monofilament diameter of 10 μm and length of 4 mm.
The toughening agent is a core-shell structure toughening agent M701.
The preparation method of the resin-based composite material with high thermal conductivity comprises the following steps:
(S1) taking the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A, the toughening agent and the reinforcing fiber according to the parts by weight for later use;
(S2) mixing the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A and the toughening agent for 20min to obtain a premix;
(S3) extruding and granulating the premix by a double-screw extruder, and adding the reinforced fibers by a weight loss scale through side feeding to obtain the resin-based composite material with high thermal conductivity.
Wherein, in the step (S3), the length-diameter ratio of the screw of the double screw extruder is 48:1, the temperature of each section of the double screw extruder from the feeding section is 260 ℃, 260 ℃ and 260 ℃, the die temperature is 260 ℃, and the screw rotating speed is 450 rpm.
Example 4
A resin-based composite material with high thermal conductivity comprises the following raw materials in parts by weight:
the heat-conducting master batch comprises the following raw materials in parts by weight:
the resin base material is PC resin, and the melt index (260 ℃/2.16kg) of the PC resin is 14g/10 min.
The heat-conducting filler is formed by mixing nano silver micro powder with the particle size of 50nm and carbon nano tubes with the particle size of 50nm according to the weight ratio of 1: 1.
The antioxidant A is prepared by compounding an antioxidant 1076 and an auxiliary antioxidant according to the weight ratio of 1:2.7, and the auxiliary antioxidant is prepared by mixing an antioxidant 168 and an antioxidant 412S according to the weight ratio of 3: 1; the antioxidant B is prepared by compounding an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:2.
The preparation method of the lubricant B comprises the following steps:
(R1), mixing lauric acid, ethylenediamine, active monomer and ammonium persulfate uniformly according to the weight ratio of 100:13:7: 1;
(R2), continuously stirring and keeping the temperature at 200 ℃ for reacting for 13min to obtain a reactant;
(R3) and devolatilizing the reaction product to obtain lubricant B having an epoxy equivalent of 200.
The active monomer is formed by mixing allyl glycidyl ether and glycerol triglycidyl ether according to the weight ratio of 3: 1.
The preparation method of the heat-conducting master batch comprises the following steps:
(B1) taking a resin base material, a heat-conducting filler, an antioxidant and a lubricant B according to parts by weight for later use;
(B2) adding the resin base material, the heat-conducting filler, the antioxidant and the lubricant B into a preheated internal mixer, mixing for 5min at 240 ℃ and at 30/25 (front/rear) rotor speed, cooling and crushing into granules to obtain the heat-conducting master batch with the particle size of 5 mm.
The lubricant A is pentaerythritol stearate.
The reinforcing fiber is chopped glass fiber with monofilament diameter of 10 μm and length of 4 mm.
The toughening agent is a core-shell structure toughening agent M701.
The preparation method of the resin-based composite material with high thermal conductivity comprises the following steps:
(S1) taking the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A, the toughening agent and the reinforcing fiber according to the parts by weight for later use;
(S2) mixing the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A and the toughening agent for 20min to obtain a premix;
(S3) extruding and granulating the premix by a double-screw extruder, and adding the reinforced fibers by a weight loss scale through side feeding to obtain the resin-based composite material with high thermal conductivity.
Wherein, in the step (S3), the length-diameter ratio of the screw of the double screw extruder is 48:1, the temperature of each section of the double screw extruder from the feeding section is 260 ℃, 260 ℃ and 260 ℃, the die temperature is 260 ℃, and the screw rotating speed is 450 rpm.
Example 5
A resin-based composite material with high thermal conductivity comprises the following raw materials in parts by weight:
the heat-conducting master batch comprises the following raw materials in parts by weight:
wherein the PC resin has a melt index (260 ℃/2.16kg) of 13g/10min, and the ABS resin is selected from Qimei PA-757.
The heat conducting filler is formed by mixing graphite with the particle size of 80nm and carbon nano tubes with the particle size of 100nm according to the weight ratio of 2: 1.
The antioxidant A is prepared by compounding an antioxidant 1076 and an auxiliary antioxidant according to the weight ratio of 1:2.7, and the auxiliary antioxidant is prepared by mixing an antioxidant 168 and an antioxidant 412S according to the weight ratio of 3: 1; the antioxidant B is prepared by compounding an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:2.
The preparation method of the lubricant B comprises the following steps:
(R1), mixing lauric acid, ethylenediamine, active monomer and ammonium persulfate uniformly according to the weight ratio of 100:12:6: 1;
(R2), continuously stirring and keeping the temperature at 200 ℃ for reacting for 13min to obtain a reactant;
(R3) and devolatilization of the reaction product to obtain lubricant B having an epoxy equivalent of 180.
The reactive monomer is allyl glycidyl ether.
The preparation method of the heat-conducting master batch comprises the following steps:
(B1) taking a resin base material, a heat-conducting filler, an antioxidant and a lubricant B according to parts by weight for later use;
(B2) adding the resin base material, the heat-conducting filler, the antioxidant and the lubricant B into a preheated internal mixer, mixing for 5min at 240 ℃ and at 30/25 (front/rear) rotor speed, cooling and crushing into granules to obtain the heat-conducting master batch with the particle size of 5 mm.
The lubricant A is pentaerythritol stearate.
The reinforcing fiber is chopped glass fiber with monofilament diameter of 10 μm and length of 4 mm.
The toughening agent is formed by mixing a core-shell structure toughening agent M701 and AX8900 according to a weight ratio of 4: 1.
The preparation method of the resin-based composite material with high thermal conductivity comprises the following steps:
(S1) taking the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A, the toughening agent and the reinforcing fiber according to the parts by weight for later use;
(S2) mixing the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A and the toughening agent for 20min to obtain a premix;
(S3) extruding and granulating the premix by a double-screw extruder, and adding the reinforced fibers by a weight loss scale through side feeding to obtain the resin-based composite material with high thermal conductivity.
Wherein, in the step (S3), the length-diameter ratio of the screw of the twin-screw extruder is 48:1, the temperature of each section of the twin-screw extruder from the feeding section is 230 ℃, 240 ℃, 250 ℃, 240 ℃ and 240 ℃, the die temperature is 240 ℃, and the screw rotating speed is 450 rpm.
Example 6
A resin-based composite material with high thermal conductivity comprises the following raw materials in parts by weight:
the heat-conducting master batch comprises the following raw materials in parts by weight:
the intrinsic viscosity of the PBT resin is in the range of 0.9dl/g, and the melt index of the PC resin (260 ℃/2.16kg) is 13g/10 min.
The heat conducting filler is formed by mixing graphite with the particle size of 8 mu m and carbon nano tubes with the particle size of 100nm according to the weight ratio of 2: 1.
The antioxidant A is prepared by compounding an antioxidant 1076 and an auxiliary antioxidant according to the weight ratio of 1:2.7, and the auxiliary antioxidant is prepared by mixing an antioxidant 168 and an antioxidant 412S according to the weight ratio of 3: 1; the antioxidant B is prepared by compounding an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:2.
The preparation method of the lubricant B comprises the following steps:
(R1), mixing lauric acid, ethylenediamine, active monomer and ammonium persulfate uniformly according to the weight ratio of 100:12:5: 1;
(R2), continuously stirring and keeping the temperature at 200 ℃ for reacting for 13min to obtain a reactant;
(R3) and devolatilizing the reaction product to obtain lubricant B having an epoxy equivalent of 160.
The active monomer is glycerol triglycidyl ether.
The preparation method of the heat-conducting master batch comprises the following steps:
(B1) taking a resin base material, a heat-conducting filler, an antioxidant and a lubricant B according to parts by weight for later use;
(B2) adding the resin base material, the heat-conducting filler, the antioxidant and the lubricant B into a preheated internal mixer, mixing for 5min at 230 ℃ and at 30/25 (front/rear) rotor speed, cooling and crushing into granules to obtain the heat-conducting master batch with the particle size of 5 mm.
The lubricant A is pentaerythritol stearate.
The reinforcing fiber is chopped glass fiber with monofilament diameter of 10 μm and length of 4 mm.
The toughening agent is formed by compounding a toughening agent AX8900 and a toughening agent 8200 according to the weight ratio of 4: 2.
The preparation method of the resin-based composite material with high thermal conductivity comprises the following steps:
(S1) taking the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A, the toughening agent and the reinforcing fiber according to the parts by weight for later use;
(S2) mixing the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A and the toughening agent for 20min to obtain a premix;
(S3) extruding and granulating the premix by a double-screw extruder, and adding the reinforced fibers by a weight loss scale through side feeding to obtain the resin-based composite material with high thermal conductivity.
Wherein, in the step (S3), the length-diameter ratio of the screw of the twin-screw extruder is 48:1, the temperature of each section of the twin-screw extruder from the feeding section is 230 ℃, 240 ℃, 250 ℃ and 240 ℃, the die temperature is 240 ℃, and the screw rotating speed is 450 rpm.
Example 7
A resin-based composite material with high thermal conductivity comprises the following raw materials in parts by weight:
the heat-conducting master batch comprises the following raw materials in parts by weight:
the intrinsic viscosity of the PBT resin is in the range of 0.9dl/g, and the melt index of the PC resin (260 ℃/2.16kg) is 13g/10 min.
The heat conducting filler is formed by mixing graphite with the particle size of 8 mu m and carbon nano tubes with the particle size of 100nm according to the weight ratio of 2: 1.
The antioxidant A is prepared by compounding an antioxidant 1076 and an auxiliary antioxidant according to the weight ratio of 1:2.7, and the auxiliary antioxidant is prepared by mixing an antioxidant 168 and an antioxidant 412S according to the weight ratio of 3: 1; the antioxidant B is prepared by compounding an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:2.
The preparation method of the lubricant B comprises the following steps:
(R1), mixing lauric acid, ethylenediamine, active monomer and ammonium persulfate uniformly according to the weight ratio of 100:12:6: 1;
(R2), continuously stirring and keeping the temperature at 200 ℃ for reacting for 13min to obtain a reactant;
(R3) and devolatilizing the reaction product to obtain lubricant B having an epoxy equivalent of 200.
The reactive monomer is allyl glycidyl ether.
The preparation method of the heat-conducting master batch comprises the following steps:
(B1) taking a resin base material, a heat-conducting filler, an antioxidant and a lubricant B according to parts by weight for later use;
(B2) adding the resin base material, the heat-conducting filler, the antioxidant and the lubricant B into a preheated internal mixer, mixing for 5min at 230 ℃ and at 30/25 (front/rear) rotor speed, cooling and crushing into granules to obtain the heat-conducting master batch with the particle size of 5 mm.
The lubricant A is pentaerythritol stearate.
The reinforcing fiber is chopped glass fiber with monofilament diameter of 10 μm and length of 4 mm.
The toughening agent is formed by compounding a toughening agent AX8900 and a toughening agent 8200 according to the weight ratio of 4: 2.
The preparation method of the resin-based composite material with high thermal conductivity comprises the following steps:
(S1) taking the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A, the toughening agent and the reinforcing fiber according to the parts by weight for later use;
(S2) mixing the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A and the toughening agent for 20min to obtain a premix;
(S3) extruding and granulating the premix by a double-screw extruder, and adding the reinforced fibers by a weight loss scale through side feeding to obtain the resin-based composite material with high thermal conductivity.
Wherein, in the step (S3), the length-diameter ratio of the screw of the twin-screw extruder is 48:1, the temperature of each section of the twin-screw extruder from the feeding section is 240 ℃, 240 ℃ and 240 ℃, the die temperature is 240 ℃, and the screw rotating speed is 450 rpm.
Example 8
A resin-based composite material with high thermal conductivity comprises the following raw materials in parts by weight:
the heat-conducting master batch comprises the following raw materials in parts by weight:
the intrinsic viscosity of the PA6 resin is in the range of 2dl/g, and the intrinsic viscosity of the PA66 resin is in the range of 2.8 dl/g.
The heat conducting filler is formed by mixing graphite with the particle size of 8000nm and graphene with the particle size of 100nm according to the weight ratio of 2: 1.
The antioxidant A is prepared by compounding an antioxidant 1076 and an auxiliary antioxidant according to the weight ratio of 1:2.7, and the auxiliary antioxidant is prepared by mixing an antioxidant 168 and an antioxidant 412S according to the weight ratio of 3: 1; the antioxidant B is prepared by compounding an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:2.
The preparation method of the lubricant B comprises the following steps:
(R1), mixing lauric acid, ethylenediamine, active monomer and ammonium persulfate uniformly according to the weight ratio of 100:11:6: 1;
(R2), continuously stirring and keeping the temperature at 200 ℃ for reacting for 13min to obtain a reactant;
(R3) and devolatilizing the reaction product to obtain lubricant B having an epoxy equivalent of 190.
The active monomer is glycerol triglycidyl ether.
The preparation method of the heat-conducting master batch comprises the following steps:
(B1) taking a resin base material, a heat-conducting filler, an antioxidant and a lubricant B according to parts by weight for later use;
(B2) adding the resin base material, the heat-conducting filler, the antioxidant and the lubricant B into a preheated internal mixer, mixing for 5min at 240 ℃ and at 30/25 (front/rear) rotor speed, cooling and crushing into granules to obtain the heat-conducting master batch with the particle size of 5 mm.
The lubricant A is pentaerythritol stearate.
The reinforcing fiber is chopped glass fiber with monofilament diameter of 10 μm and length of 4 mm.
The toughening agent is formed by compounding a toughening agent N216 and a toughening agent AX8900 according to the weight ratio of 4: 1.
The preparation method of the resin-based composite material with high thermal conductivity comprises the following steps:
(S1) taking the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A, the toughening agent and the reinforcing fiber according to the parts by weight for later use;
(S2) mixing the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A and the toughening agent for 20min to obtain a premix;
(S3) extruding and granulating the premix by a double-screw extruder, and adding the reinforced fibers by a weight loss scale through side feeding to obtain the resin-based composite material with high thermal conductivity.
Wherein, in the step (S3), the length-diameter ratio of the screw of the double screw extruder is 48:1, the temperature of each section of the double screw extruder from the feeding section is 245 ℃, 255 ℃, 265 ℃ and 255 ℃, the die temperature is 255 ℃, and the screw rotating speed is 450 rpm.
Example 9
A resin-based composite material with high thermal conductivity comprises the following raw materials in parts by weight:
the heat-conducting master batch comprises the following raw materials in parts by weight:
the PC resin has a melt index (260 ℃/2.16kg) of 13g/10min, and the ABS resin is selected from PA-758.
The heat-conducting filler is formed by mixing graphite with the particle size of 9000nm and carbon nano tubes with the particle size of 200nm according to the weight ratio of 2: 1.
The antioxidant A is prepared by compounding an antioxidant 1076 and an auxiliary antioxidant according to the weight ratio of 1:2.7, and the auxiliary antioxidant is prepared by mixing an antioxidant 168 and an antioxidant 412S according to the weight ratio of 3: 1; the antioxidant B is prepared by compounding an antioxidant 1076 and an antioxidant 168 according to the weight ratio of 1:2.
The preparation method of the lubricant B comprises the following steps:
(R1), mixing lauric acid, ethylenediamine, active monomer and ammonium persulfate uniformly according to the weight ratio of 100:13:6: 1;
(R2), continuously stirring and keeping the temperature at 200 ℃ for reacting for 13min to obtain a reactant;
(R3) and devolatilizing the reaction product to obtain lubricant B having an epoxy equivalent of 200.
The active monomer is formed by mixing allyl glycidyl ether and glycerol triglycidyl ether according to the weight ratio of 1: 1.
The preparation method of the heat-conducting master batch comprises the following steps:
(B1) taking a resin base material, a heat-conducting filler, an antioxidant and a lubricant B according to parts by weight for later use;
(B2) adding the resin base material, the heat-conducting filler, the antioxidant and the lubricant B into a preheated internal mixer, mixing for 5min at 230 ℃ and at 30/25 (front/rear) rotor speed, cooling and crushing into granules to obtain the heat-conducting master batch with the particle size of 5 mm.
The lubricant A is pentaerythritol stearate.
The reinforcing fibers are chopped carbon fibers with monofilament diameter of 8 mu m and length of 7 mm.
The toughening agent is formed by mixing a core-shell structure toughening agent M701 and a toughening agent AX8900 according to a weight ratio of 4: 1.
The preparation method of the resin-based composite material with high thermal conductivity comprises the following steps:
(S1) taking the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A, the toughening agent and the reinforcing fiber according to the parts by weight for later use;
(S2) mixing the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A and the toughening agent for 20min to obtain a premix;
(S3) extruding and granulating the premix by a double-screw extruder, and adding the reinforced fibers by a weight loss scale through side feeding to obtain the resin-based composite material with high thermal conductivity.
Wherein, in the step (S3), the length-diameter ratio of the screw of the twin-screw extruder is 48:1, the temperature of each section of the twin-screw extruder from the feeding section is 240 ℃, 240 ℃ and 240 ℃, the die temperature is 240 ℃, and the screw rotating speed is 450 rpm.
Comparative example 1
This comparative example differs from example 1 in that:
and the lubricant B is pentaerythritol stearate.
Comparative example 2
This comparative example differs from example 1 in that:
the resin-based composite material is composed of the following raw materials in parts by weight:
comparative example 3
This comparative example differs from example 1 in that:
the resin-based composite material is composed of the following raw materials in parts by weight:
comparative example 4
This comparative example differs from example 6 in that:
The resin-based composite material with high thermal conductivity comprises the following raw materials in parts by weight:
comparative example 5
This comparative example differs from example 8 in that:
the resin-based composite material with high thermal conductivity comprises the following raw materials in parts by weight:
example 10
The composites of examples 1-9 and comparative examples 1-5 were tested for Izod notched impact strength, tensile strength, flexural modulus, and thermal conductivity. The measurement results are shown in the following table:
with the test performance of examples 1 to 9, we can see that the conductive composite material prepared by melt blending the conductive masterbatch prepared by using the special lubricant B and the resin has good comprehensive performance, and when the addition ratio of the nanoscale heat-conducting filler in the formula reaches 4%, the surface resistance can be more than 2.0W/m.k, because the lubricant B with an active end group is added in the preparation process of the heat-conducting masterbatch, the lubricant B can be simultaneously physically and chemically combined with the active group on the surface of the heat-conducting filler and the resin base material, so that an effect is formed between the resin base material and the heat-conducting filler, and the heat-conducting masterbatch is more favorable for uniform dispersion of the heat-conducting filler after secondary processing, so that the prepared composite material has two beneficial effects: the heat-conducting filler can form good uniform distribution, so that a perfect heat-conducting network can be formed under the condition of a lower adding proportion of the heat-conducting filler, and ii, two or more than two heat-conducting fillers are adopted, so that the formation of the heat-conducting network is facilitated, the adding amount of the heat-conducting filler is reduced, a composite material with good mechanical property can be prepared, and the performance requirement in the field of radiating fins is met.
In comparative example 1, the lubricant B is pentaerythritol stearate, the heat-conducting filler is seriously agglomerated in the manufacturing process of the heat-conducting master batch, and the heat-conducting filler is difficult to be uniformly dispersed even after secondary processing, so that the heat conductivity coefficient of the composite material is only 1.25W/(m.K). Compared example 2 and comparative example 3 do not prepare heat conducting master batches for secondary processing, even if lubricant B with active end groups is added in the comparative example 3, the nano-sized heat conducting filler is easy to agglomerate and difficult to uniformly disperse in the prepared conductive composite material through simple melt blending, so that an effective and complete heat conducting network cannot be formed, the heat conducting coefficient is low, and the use requirement cannot be met. Compared with the prior art, the heat-conducting master batch is added in a large amount in the comparative example 4, and the material of the heat-conducting filler is too large, so that the mechanical property of the composite material is poor, and the requirement of a workpiece on the mechanical property cannot be met. In the comparative example 5, only 10% of the heat-conducting master batch is added, the addition amount of the heat-conducting filler in the system is small, and a perfect heat-conducting network cannot be formed, so that the heat-conducting coefficient is low, and the requirement of the heat-radiating fin on high heat-conducting coefficient cannot be met.
The above-described embodiments are preferred implementations of the present invention, and the present invention may be implemented in other ways without departing from the spirit of the present invention.
Claims (10)
1. A resin-based composite material with high thermal conductivity is characterized in that: the feed comprises the following raw materials in parts by weight:
2. a high thermal conductivity resin-based composite material as claimed in claim 1, wherein: the heat-conducting master batch comprises the following raw materials in parts by weight:
3. a high thermal conductivity resin-based composite material as claimed in claim 2, wherein: the resin base material is at least one of PA6 resin, PA66 resin, PBT resin, PC resin, ABS resin, PP resin and PS resin.
4. A high thermal conductivity resin-based composite material as claimed in claim 2, wherein: the heat-conducting filler is at least one of magnesium hydroxide powder, aluminum hydroxide powder, magnesium oxide powder, aluminum oxide powder, zirconium oxide powder, silicon carbide powder, aluminum nitride micro powder, zinc oxide micro powder, hexagonal boron nitride micro powder, nano silver micro powder, graphite oxide, carbon nano tube, graphene oxide, nano aluminum powder and nano copper powder.
5. A high thermal conductivity resin-based composite material as claimed in claim 2, wherein: the antioxidant A and the antioxidant B are both compounded by a main antioxidant and an auxiliary antioxidant according to the weight ratio of 1: 2-3; the primary antioxidant is antioxidant 1076, antioxidant 1010, antioxidant 1098, antioxidant 264, antioxidant 330 or antioxidant 1024, and the secondary antioxidant is antioxidant 168, antioxidant 618, antioxidant 626, antioxidant S9228, antioxidant PEPQ, antioxidant PEP36 or antioxidant 412S.
6. The resin-based composite material with high thermal conductivity as claimed in claim 2, wherein the preparation method of the lubricant B comprises the following steps:
(R1), mixing lauric acid, ethylenediamine, active monomer and ammonium persulfate uniformly according to the weight ratio of 100:10-14:4-8: 1;
(R2), continuously stirring and keeping the temperature at the temperature of 180-230 ℃ for reaction for 11-15min to obtain a reactant;
(R3) and devolatilizing the reaction product to obtain lubricant B having an epoxy equivalent of 150-300.
7. A high thermal conductivity resin-based composite material as claimed in claim 6, wherein: the active monomer is allyl glycidyl ether and/or glycerol triglycidyl ether.
8. The resin-based composite material with high thermal conductivity as claimed in any one of claims 2-7, wherein the preparation method of the heat-conducting master batch comprises the following steps:
(B1) taking a resin base material, a heat-conducting filler, an antioxidant and a lubricant B according to parts by weight for later use;
(B2) adding the resin base material, the heat-conducting filler, the antioxidant and the lubricant B into a preheated internal mixer for mixing for 2-6min, cooling and crushing into granules to obtain the heat-conducting master batch.
9. A high thermal conductivity resin-based composite material as claimed in claim 1, wherein: the lubricant A is at least one of pentaerythritol stearate, N' -ethylene bis-stearamide, oleamide, erucamide, butyl stearate, glycerol tristearate, microcrystalline paraffin, liquid paraffin, chlorinated paraffin, polyethylene wax, oxidized polyethylene wax, methyl silicone oil, benzyl silicone oil, ethyl silicone oil and montan wax; the reinforcing fiber is chopped glass fiber, chopped carbon fiber or stainless steel fiber; the toughening agent is at least one of MBS type toughening agent with a core-shell structure, ACR type toughening agent with a core-shell structure, ethylene-octene copolymer grafted glycidyl methacrylate, ethylene-acrylate-glycidyl methacrylate terpolymer, ethylene maleic anhydride binary copolymer, ethylene-octene copolymer, ethylene-butyl acrylate copolymer, ethylene-methyl acrylate copolymer, ethylene-ethyl acrylate copolymer, high rubber powder, ethylene-octene copolymer grafted maleic anhydride and surlyn resin.
10. A method for preparing a resin-based composite material of high thermal conductivity according to any one of claims 1 to 9, comprising the steps of:
(S1) taking the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A, the toughening agent and the reinforcing fiber according to the parts by weight for later use;
(S2) mixing the resin base material, the heat-conducting master batch, the antioxidant, the lubricant A and the toughening agent for 10-30min to obtain a premix;
(S3) extruding and granulating the premix by a double-screw extruder, and adding the reinforced fibers by a weight loss scale through side feeding to obtain the resin-based composite material with high thermal conductivity.
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