CN113717534A - Heat conduction material and preparation process - Google Patents
Heat conduction material and preparation process Download PDFInfo
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- CN113717534A CN113717534A CN202111083836.9A CN202111083836A CN113717534A CN 113717534 A CN113717534 A CN 113717534A CN 202111083836 A CN202111083836 A CN 202111083836A CN 113717534 A CN113717534 A CN 113717534A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 title claims description 23
- 239000000835 fiber Substances 0.000 claims abstract description 68
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 67
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 67
- 239000002245 particle Substances 0.000 claims abstract description 64
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 63
- 229920002545 silicone oil Polymers 0.000 claims abstract description 53
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 41
- 239000001257 hydrogen Substances 0.000 claims abstract description 41
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000007822 coupling agent Substances 0.000 claims abstract description 33
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000000843 powder Substances 0.000 claims abstract description 27
- 239000003054 catalyst Substances 0.000 claims abstract description 26
- 239000003112 inhibitor Substances 0.000 claims abstract description 26
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 22
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 20
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 20
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003063 flame retardant Substances 0.000 claims abstract description 20
- 239000004020 conductor Substances 0.000 claims abstract description 14
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 4
- 239000004945 silicone rubber Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims description 56
- 238000003756 stirring Methods 0.000 claims description 51
- 238000004898 kneading Methods 0.000 claims description 42
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 30
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 27
- 239000000243 solution Substances 0.000 claims description 26
- 238000002156 mixing Methods 0.000 claims description 24
- 238000004073 vulcanization Methods 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 12
- 238000000465 moulding Methods 0.000 claims description 9
- 238000003490 calendering Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000004132 cross linking Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- -1 methyl hydrogen Chemical compound 0.000 claims description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 4
- 229920002554 vinyl polymer Polymers 0.000 claims description 4
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical group C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 3
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- 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 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 3
- 230000001680 brushing effect Effects 0.000 claims description 3
- 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
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 26
- 239000000741 silica gel Substances 0.000 abstract description 26
- 229910002027 silica gel Inorganic materials 0.000 abstract description 26
- 238000005303 weighing Methods 0.000 description 6
- 229920000049 Carbon (fiber) Polymers 0.000 description 3
- 239000004917 carbon fiber Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
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- C09K5/14—Solid materials, e.g. powdery or granular
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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Abstract
The invention relates to the technical field of heat-conducting silica gel, in particular to a heat-conducting material and a preparation process thereof, wherein the heat-conducting material comprises methyl vinyl silicone oil, hydrogen-containing silicone oil, modified alumina particles, graphene fiber powder, a propanol solution, a coupling agent, a catalyst, an inhibitor, a cross-linking agent, an antioxidant and a flame retardant, and the components are as follows by weight: the heat-conducting silicone rubber pad comprises, by weight, 100-150 parts of methyl vinyl silicone oil, 15-30 parts of hydrogen-containing silicone oil, 300-500 parts of modified alumina particles, 50-100 parts of graphene fiber powder, 80-100 parts of a propanol solution, 1-5 parts of a coupling agent, 2-8 parts of a catalyst, 5-9 parts of an inhibitor, 10-15 parts of a cross-linking agent, 15-20 parts of an antioxidant and 10-15 parts of a flame retardant.
Description
Technical Field
The invention relates to the technical field of heat-conducting silica gel, in particular to a heat-conducting material and a preparation process thereof.
Background
The heat-conducting silica gel sheet is a heat-conducting medium composite material taking silica gel as a base material, also called as a heat-conducting silica gel pad, a heat-conducting silica gel sheet, a soft heat-conducting pad and the like, the silica gel sheet is used as a heat-conducting material and has been widely applied in the field of electronic equipment, the silica gel sheet has certain flexibility, excellent insulativity, compressibility and surface natural viscosity, and the manufacturing and production processes of the heat-conducting silica gel sheet of different manufacturers have certain differences: the heat conducting material is prepared with common solid organic silica gel as material.
At present, the main heat conduction mechanism of the heat conduction silica gel is carried out through heat conduction, and the heat conduction channels inside and outside the currently adopted heat conduction silica gel are insufficient, so that the heat conduction performance of the silica gel pad is poor, and the application range of the silica gel pad is limited.
In summary, the present invention solves the existing problems by designing a heat conductive material and a preparation process thereof.
Disclosure of Invention
The invention aims to provide a heat conduction material and a preparation process thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a heat conduction material and a preparation process thereof comprise methyl vinyl silicone oil, hydrogen-containing silicone oil, modified alumina particles, graphene fiber powder, propanol solution, a coupling agent, a catalyst, an inhibitor, a cross-linking agent, an antioxidant and a flame retardant, wherein the components are as follows according to the weight ratio: 100-150 parts of methyl vinyl silicone oil, 15-30 parts of hydrogen-containing silicone oil, 300-500 parts of modified alumina particles, 50-100 parts of graphene fiber powder, 80-100 parts of propanol solution, 1-5 parts of coupling agent, 2-8 parts of catalyst, 5-9 parts of inhibitor, 10-15 parts of cross-linking agent, 15-20 parts of antioxidant and 10-15 parts of flame retardant.
As a preferable scheme of the invention, the method comprises the following steps:
s1, feeding the modified alumina particles into a drying oven, sealing, replacing for 7-8 times with nitrogen, and then heating and drying at the pressure of 1.5-2 MPa and the temperature of 150-175 ℃ to remove excessive moisture to obtain dried modified alumina particles;
s2, feeding the dried modified alumina particles, methyl vinyl silicone oil and hydrogen-containing silicone oil into a stirring machine to be uniformly mixed, feeding the mixture into a vacuum kneading machine to be primarily kneaded after stirring and mixing, feeding the coupling agent, the catalyst, the inhibitor, the crosslinking agent, the antioxidant and the flame retardant into the vacuum kneading machine to be secondarily kneaded after primary kneading is finished, placing the mixture obtained after secondary kneading into a vacuum machine to be vacuumized for 0.5-1.5 h, completely pumping out bubbles in the mixture to obtain a mixed base material, feeding the mixed base material into a calender to be calendered and molded, and then carrying out high-temperature vulcanization molding to obtain a base gasket;
s3, feeding the graphene fiber powder, hydrogen-containing silicone oil, a propanol solution, a catalyst, an inhibitor and a coupling agent into a planetary stirrer to be stirred at a low speed of 1050-1250 r/min for 90-100 min at a stirring temperature of 30-35 ℃ until the graphene fiber powder is completely and uniformly dispersed to obtain a graphene fiber dispersion liquid;
s4, brushing the graphene fiber dispersion liquid on the outer wall of the basic gasket, heating until the propanol solution is completely volatilized, enabling the graphene fibers to be regularly and directionally arranged on the surface of the basic gasket, enabling a coupling agent adsorbed on the surface of the graphene fibers to be subjected to a cross-linking reaction with unsaturated groups and hydrogen-containing silicone oil in the basic gasket, enabling the graphene fiber layer to be firmly attached to the surface of the basic gasket, repeating the operation for 10-15 times, and cooling the basic gasket attached with the graphene fiber layer after hot air vulcanization to obtain the heat-conducting silicone rubber pad.
In a preferred embodiment of the present invention, the coupling agent is a silane coupling agent containing a vinyl group, the catalyst is a platinum-vinylsiloxane complex and has a concentration of 1800ppm, the inhibitor is ethynylcyclohexanol, the crosslinking agent is linear methylhydrogenpolysiloxane and has a viscosity of 50mpa · s to 250mpa · s, the hydrogen content is 6.1 wt% to 6.5 wt%, the antioxidant is prepared by mixing an antioxidant 1010 and an antioxidant 1076 in a mass ratio of 1: 1, and the flame retardant is prepared by mixing aluminum hydroxide and magnesium hydroxide in a mass ratio of 1: 2.
In a preferred embodiment of the present invention, the viscosity of the methyl vinyl silicone oil is 2550 to 2600mPa · s, the mass fraction of hydrogen contained in the hydrogen-containing silicone oil is 0.35 to 0.4%, the diameter of the monofilament in the graphene fiber powder is 22 to 23 μm, the length of the monofilament is 1100 to 1200 μm, the particle size of the modified alumina particle is 20 to 35 μm, and the concentration of the propanol solution is 10 to 15%.
In a preferred embodiment of the present invention, the modified alumina particles are prepared by mixing hexamethyldisilazane, methanol, and spherical alumina particles, and the components are, by weight: 30-45 parts of hexamethyldisilazane, 80-100 parts of methanol and 700-1000 parts of alumina particles.
As a preferred embodiment of the present invention, the method for preparing the modified alumina particles comprises the following steps:
s21, adding hexamethyldisilazane into propanol, and stirring and mixing by using an electromagnetic stirrer, wherein the stirring speed is 300-450 r/min, and the stirring time is 30min to prepare a mixed solution;
and S22, adding the spherical alumina particles into the mixed solution, and stirring and drying to obtain the modified spherical alumina particles.
As a preferable scheme of the invention, the rotation speed of the stirrer in S2 is 3500 r/min-4000 r/min, the stirring time is 15 min-30 min, the high-temperature vulcanization molding temperature is 155-175 ℃, and the vulcanization time is 60 min-80 min.
In a preferable embodiment of the present invention, in S2, the first kneading temperature of the vacuum kneader is 95 to 100 ℃, the first kneading time is 100 to 120min, the second kneading temperature of the vacuum kneader is 120 to 130 ℃, and the second kneading time is 50 to 60 min.
In a preferred embodiment of the present invention, the temperature of the hot air vulcanization in S4 is 185 to 190 ℃, and the vulcanization time is 25 to 35 min.
As a preferable scheme of the invention, the stirring time in the S22 is 0.5-1 h, the drying is carried out in two times, the drying temperature is 120 ℃ for the first time, the drying time is 1.5h, and the drying temperature is 160 ℃ for the second time, the drying time is 0.5 h.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the modified alumina particles are added into the heat-conducting silica gel, so that the heat-conducting performance of the modified alumina is higher, the modified alumina can be uniformly distributed in the heat-conducting silica gel pad, the heat-conducting channel in the heat-conducting silica gel pad is increased, the graphene fiber dispersion liquid is coated on the outer wall of the basic gasket in a brush mode, the graphene fibers can be arranged in a manner of being parallel to the plane of the basic gasket along with the volatilization of the propanol solution, the high heat-conducting performance of the carbon fiber material along the axial direction of the fibers is exerted, the heat-conducting silica gel pad has a good soaking function in the plane direction, and under the combined action of the modified alumina particles and the graphene fibers, the manufactured heat-conducting silica gel pad has the advantage of high heat-conducting performance, and the application range of the heat-conducting silica gel pad can be effectively improved.
2. According to the invention, the graphene fiber dispersion liquid is coated on the outer wall of the basic gasket, so that the graphene fiber powder directionally distributed on the surface of the basic gasket can play a role similar to skeleton reinforcement, the mechanical properties of the heat-conducting silica gel pad such as stretching and tearing are greatly improved, and meanwhile, in the high-temperature vulcanization process, the coupling agent containing unsaturated groups and chemically bonded on the surface of carbon fibers can generate a cross-linking reaction with hydrogen-containing silicone oil and vinyl on the surface of the basic gasket, so that the firm connection between the carbon fiber material layer and the basic gasket is realized, and the subsequent calendering processing is facilitated.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and the terms used herein in the specification of the present invention are for the purpose of describing particular embodiments only and are not intended to limit the present invention, and the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
The invention provides a technical scheme that:
a heat conduction material and a preparation process thereof comprise methyl vinyl silicone oil, hydrogen-containing silicone oil, modified alumina particles, graphene fiber powder, propanol solution, a coupling agent, a catalyst, an inhibitor, a cross-linking agent, an antioxidant and a flame retardant, wherein the components are as follows according to the weight ratio: 100-150 parts of methyl vinyl silicone oil, 15-30 parts of hydrogen-containing silicone oil, 300-500 parts of modified alumina particles, 50-100 parts of graphene fiber powder, 80-100 parts of propanol solution, 1-5 parts of coupling agent, 2-8 parts of catalyst, 5-9 parts of inhibitor, 10-15 parts of cross-linking agent, 15-20 parts of antioxidant and 10-15 parts of flame retardant.
Further, the method comprises the following steps:
s1, feeding the modified alumina particles into a drying oven, sealing, replacing for 7-8 times with nitrogen, and then heating and drying at the pressure of 1.5-2 MPa and the temperature of 150-175 ℃ to remove excessive moisture to obtain dried modified alumina particles;
s2, feeding the dried modified alumina particles, methyl vinyl silicone oil and hydrogen-containing silicone oil into a stirring machine to be uniformly mixed, feeding the mixture into a vacuum kneading machine to be primarily kneaded after stirring and mixing, feeding the coupling agent, the catalyst, the inhibitor, the crosslinking agent, the antioxidant and the flame retardant into the vacuum kneading machine to be secondarily kneaded after primary kneading is finished, placing the mixture obtained after secondary kneading into a vacuum machine to be vacuumized for 0.5-1.5 h, completely pumping out bubbles in the mixture to obtain a mixed base material, feeding the mixed base material into a calender to be calendered and molded, and then carrying out high-temperature vulcanization molding to obtain a base gasket;
s3, feeding the graphene fiber powder, hydrogen-containing silicone oil, a propanol solution, a catalyst, an inhibitor and a coupling agent into a planetary stirrer to be stirred at a low speed of 1050-1250 r/min for 90-100 min at a stirring temperature of 30-35 ℃ until the graphene fiber powder is completely and uniformly dispersed to obtain a graphene fiber dispersion liquid;
s4, brushing the graphene fiber dispersion liquid on the outer wall of the basic gasket, heating until the propanol solution is completely volatilized, enabling the graphene fibers to be regularly and directionally arranged on the surface of the basic gasket, enabling a coupling agent adsorbed on the surface of the graphene fibers to be subjected to a cross-linking reaction with unsaturated groups and hydrogen-containing silicone oil in the basic gasket, enabling the graphene fiber layer to be firmly attached to the surface of the basic gasket, repeating the operation for 10-15 times, and cooling the basic gasket attached with the graphene fiber layer after hot air vulcanization to obtain the heat-conducting silicone rubber pad.
Further, the coupling agent is a silane coupling agent containing vinyl groups, the catalyst is a platinum-vinyl siloxane complex, the concentration of the platinum-vinyl siloxane complex is 1800ppm, the inhibitor is ethynylcyclohexanol, the cross-linking agent is linear methyl hydrogen polysiloxane, the viscosity of the cross-linking agent is 50 mpa-s-250 mpa-s, the hydrogen content of the cross-linking agent is 6.1 wt% -6.5 wt%, the antioxidant is prepared by mixing an antioxidant 1010 and an antioxidant 1076 according to the mass ratio of 1: 1, and the flame retardant is prepared by mixing aluminum hydroxide and magnesium hydroxide according to the mass ratio of 1: 2.
Furthermore, the viscosity range of the methyl vinyl silicone oil is 2550-2600 mPa.s, the mass fraction range of hydrogen contained in the hydrogen-containing silicone oil is 0.35-0.4%, the monofilament diameter in the graphene fiber powder is 22-23 μm, the length is 1100-1200 μm, the particle diameter of the modified alumina particle is 20-35 μm, and the concentration of the propanol solution is 10-15%.
Further, the modified alumina particles are prepared by mixing hexamethyldisilazane, methanol and spherical alumina particles, and the components are as follows according to the weight ratio: 30-45 parts of hexamethyldisilazane, 80-100 parts of methanol and 700-1000 parts of alumina particles.
Further, the preparation method of the modified alumina particles comprises the following steps:
s21, adding hexamethyldisilazane into propanol, and stirring and mixing by using an electromagnetic stirrer, wherein the stirring speed is 300-450 r/min, and the stirring time is 30min to prepare a mixed solution;
and S22, adding the spherical alumina particles into the mixed solution, and stirring and drying to obtain the modified spherical alumina particles.
Further, in the S2, the rotating speed of the stirrer is 3500 r/min-4000 r/min, the stirring time is 15 min-30 min, the high-temperature vulcanization molding temperature is 155-175 ℃, and the vulcanization time is 60 min-80 min.
Further, in the S2, the primary kneading temperature of the vacuum kneader is 95-100 ℃, the primary kneading time is 100-120 min, the secondary kneading temperature of the vacuum kneader is 120-130 ℃, and the secondary kneading time is 50-60 min.
Further, the temperature of hot air vulcanization in the S4 is 185-190 ℃, and the vulcanization time is 25-35 min.
Further, the stirring time in the step S22 is 0.5 h-1 h, the drying is carried out in two times, the drying temperature is 120 ℃ for the first time, the drying time is 1.5h, and the drying temperature is 160 ℃ for the second time, and the drying time is 0.5 h.
Detailed description of the preferred embodiments
Example 1:
weighing 45 parts of hexamethyldisilazane, 100 parts of methanol and 700 parts of alumina particles, putting hexamethyldisilazane into propanol, stirring and mixing by using an electromagnetic stirrer, wherein the stirring speed is 450r/min, the stirring time is 30min, preparing a mixed solution, adding spherical alumina particles into the mixed solution, stirring and drying for 1h, drying for two times, and obtaining modified spherical alumina particles, wherein the drying temperature is 120 ℃ during primary drying, the drying time is 1.5h, and the drying temperature is 160 ℃ during secondary drying, and the drying time is 0.5 h;
weighing 100 parts of methyl vinyl silicone oil, 15 parts of hydrogen-containing silicone oil, 300 parts of modified alumina particles, 50 parts of graphene fiber powder, 90 parts of propanol solution, 5 parts of coupling agent, 8 parts of catalyst, 9 parts of inhibitor, 15 parts of cross-linking agent, 20 parts of antioxidant and 15 parts of flame retardant, feeding the modified alumina particles into a drying oven, sealing, replacing 8 times with nitrogen, heating and drying at the pressure of 2MPa and the temperature of 175 ℃ to remove redundant moisture to obtain dried modified alumina particles;
feeding the dried modified alumina particles, methyl vinyl silicone oil and hydrogen-containing silicone oil into a stirrer, uniformly mixing at the rotation speed of 4000r/min for 30min, stirring and mixing, then feeding into a vacuum kneader for primary kneading at the primary kneading temperature of 100 ℃ for 120min, after the primary kneading is finished, feeding a coupling agent, a catalyst, an inhibitor, a cross-linking agent, an antioxidant and a flame retardant into the vacuum kneader for secondary kneading at the secondary kneading temperature of 130 ℃ for 60min, placing the mixture obtained after the secondary kneading into a vacuum machine, vacuumizing for 1.5h to completely extract bubbles in the mixture to obtain a mixed base material, feeding the mixed base material into a calender for calendering and then carrying out high-temperature vulcanization molding, vulcanizing at 175 deg.C for 80min to obtain base gasket;
feeding graphene fiber powder, hydrogen-containing silicone oil, a propanol solution, a catalyst, an inhibitor and a coupling agent into a planetary mixer for low-speed stirring at a stirring speed of 1250r/min for 100min at a stirring temperature of 35 ℃ to obtain a graphene fiber dispersion liquid after the graphene fiber powder is completely dispersed, coating the graphene fiber dispersion liquid on the outer wall of a basic gasket, heating until the propanol solution is completely volatilized, so that the graphene fibers are regularly and directionally arranged on the surface of the basic gasket, simultaneously carrying out a cross-linking reaction on the coupling agent adsorbed on the surface of the graphene fibers, unsaturated groups in the basic gasket and the hydrogen-containing silicone oil to firmly attach the graphene fiber layer on the surface of the basic gasket, repeating the operation for 10 times, vulcanizing the basic gasket attached with the graphene fiber layer by hot air, and then cooling the basic gasket at the temperature of 190 ℃ and vulcanizing the temperature of 190 ℃, And vulcanizing for 35min to obtain the heat-conducting silica gel pad.
Example 2:
weighing 45 parts of hexamethyldisilazane, 100 parts of methanol and 700 parts of alumina particles, putting hexamethyldisilazane into propanol, stirring and mixing by using an electromagnetic stirrer, wherein the stirring speed is 450r/min, the stirring time is 30min, preparing a mixed solution, adding spherical alumina particles into the mixed solution, stirring and drying for 1h, drying for two times, and obtaining modified spherical alumina particles, wherein the drying temperature is 120 ℃ during primary drying, the drying time is 1.5h, and the drying temperature is 160 ℃ during secondary drying, and the drying time is 0.5 h;
weighing 130 parts of methyl vinyl silicone oil, 25 parts of hydrogen-containing silicone oil, 400 parts of modified alumina particles, 75 parts of graphene fiber powder, 90 parts of propanol solution, 5 parts of coupling agent, 8 parts of catalyst, 9 parts of inhibitor, 15 parts of cross-linking agent, 20 parts of antioxidant and 15 parts of flame retardant, feeding the modified alumina particles into a drying oven, sealing, replacing 8 times with nitrogen, heating and drying at the pressure of 2MPa and the temperature of 175 ℃ to remove redundant moisture to obtain dried modified alumina particles;
feeding the dried modified alumina particles, methyl vinyl silicone oil and hydrogen-containing silicone oil into a stirrer, uniformly mixing at the rotation speed of 4000r/min for 30min, stirring and mixing, then feeding into a vacuum kneader for primary kneading at the primary kneading temperature of 100 ℃ for 120min, after the primary kneading is finished, feeding a coupling agent, a catalyst, an inhibitor, a cross-linking agent, an antioxidant and a flame retardant into the vacuum kneader for secondary kneading at the secondary kneading temperature of 130 ℃ for 60min, placing the mixture obtained after the secondary kneading into a vacuum machine, vacuumizing for 1.5h to completely extract bubbles in the mixture to obtain a mixed base material, feeding the mixed base material into a calender for calendering and then carrying out high-temperature vulcanization molding, vulcanizing at 175 deg.C for 80min to obtain base gasket;
feeding graphene fiber powder, hydrogen-containing silicone oil, a propanol solution, a catalyst, an inhibitor and a coupling agent into a planetary mixer for low-speed stirring at a stirring speed of 1250r/min for 100min at a stirring temperature of 35 ℃ to obtain a graphene fiber dispersion liquid after the graphene fiber powder is completely dispersed, coating the graphene fiber dispersion liquid on the outer wall of a basic gasket, heating until the propanol solution is completely volatilized, so that the graphene fibers are regularly and directionally arranged on the surface of the basic gasket, simultaneously carrying out a cross-linking reaction on the coupling agent adsorbed on the surface of the graphene fibers, unsaturated groups in the basic gasket and the hydrogen-containing silicone oil to firmly attach the graphene fiber layer on the surface of the basic gasket, repeating the operation for 10 times, vulcanizing the basic gasket attached with the graphene fiber layer by hot air, and then cooling the basic gasket at the temperature of 190 ℃ and vulcanizing the temperature of 190 ℃, And vulcanizing for 35min to obtain the heat-conducting silica gel pad.
Example 3:
weighing 45 parts of hexamethyldisilazane, 100 parts of methanol and 700 parts of alumina particles, putting hexamethyldisilazane into propanol, stirring and mixing by using an electromagnetic stirrer, wherein the stirring speed is 450r/min, the stirring time is 30min, preparing a mixed solution, adding spherical alumina particles into the mixed solution, stirring and drying for 1h, drying for two times, and obtaining modified spherical alumina particles, wherein the drying temperature is 120 ℃ during primary drying, the drying time is 1.5h, and the drying temperature is 160 ℃ during secondary drying, and the drying time is 0.5 h;
weighing 150 parts of methyl vinyl silicone oil, 30 parts of hydrogen-containing silicone oil, 500 parts of modified alumina particles, 100 parts of graphene fiber powder, 90 parts of propanol solution, 5 parts of coupling agent, 8 parts of catalyst, 9 parts of inhibitor, 15 parts of cross-linking agent, 20 parts of antioxidant and 15 parts of flame retardant, feeding the modified alumina particles into a drying oven, sealing, replacing 8 times with nitrogen, heating and drying at the pressure of 2MPa and the temperature of 175 ℃ to remove redundant moisture to obtain dried modified alumina particles;
feeding the dried modified alumina particles, methyl vinyl silicone oil and hydrogen-containing silicone oil into a stirrer, uniformly mixing at the rotation speed of 4000r/min for 30min, stirring and mixing, then feeding into a vacuum kneader for primary kneading at the primary kneading temperature of 100 ℃ for 120min, after the primary kneading is finished, feeding a coupling agent, a catalyst, an inhibitor, a cross-linking agent, an antioxidant and a flame retardant into the vacuum kneader for secondary kneading at the secondary kneading temperature of 130 ℃ for 60min, placing the mixture obtained after the secondary kneading into a vacuum machine, vacuumizing for 1.5h to completely extract bubbles in the mixture to obtain a mixed base material, feeding the mixed base material into a calender for calendering and then carrying out high-temperature vulcanization molding, vulcanizing at 175 deg.C for 80min to obtain base gasket;
feeding graphene fiber powder, hydrogen-containing silicone oil, a propanol solution, a catalyst, an inhibitor and a coupling agent into a planetary mixer for low-speed stirring at a stirring speed of 1250r/min for 100min at a stirring temperature of 35 ℃ to obtain a graphene fiber dispersion liquid after the graphene fiber powder is completely dispersed, coating the graphene fiber dispersion liquid on the outer wall of a basic gasket, heating until the propanol solution is completely volatilized, so that the graphene fibers are regularly and directionally arranged on the surface of the basic gasket, simultaneously carrying out a cross-linking reaction on the coupling agent adsorbed on the surface of the graphene fibers, unsaturated groups in the basic gasket and the hydrogen-containing silicone oil to firmly attach the graphene fiber layer on the surface of the basic gasket, repeating the operation for 10 times, vulcanizing the basic gasket attached with the graphene fiber layer by hot air, and then cooling the basic gasket at the temperature of 190 ℃ and vulcanizing the temperature of 190 ℃, And vulcanizing for 35min to obtain the heat-conducting silica gel pad.
The heat conductive silica gel pads in embodiment examples 1 to 3 were subjected to performance tests, and the test results are shown in table 1.
Table 1 heat-conducting silica gel pad performance test results
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A heat conduction material comprises methyl vinyl silicone oil, hydrogen-containing silicone oil, modified alumina particles, graphene fiber powder, propanol solution, a coupling agent, a catalyst, an inhibitor, a cross-linking agent, an antioxidant and a flame retardant, and the components are as follows according to the weight ratio: 100-150 parts of methyl vinyl silicone oil, 15-30 parts of hydrogen-containing silicone oil, 300-500 parts of modified alumina particles, 50-100 parts of graphene fiber powder, 80-100 parts of propanol solution, 1-5 parts of coupling agent, 2-8 parts of catalyst, 5-9 parts of inhibitor, 10-15 parts of cross-linking agent, 15-20 parts of antioxidant and 10-15 parts of flame retardant.
2. A preparation process of a heat conduction material comprises the following steps:
s1, feeding the modified alumina particles into a drying oven, sealing, replacing for 7-8 times with nitrogen, and then heating and drying at the pressure of 1.5-2 MPa and the temperature of 150-175 ℃ to remove excessive moisture to obtain dried modified alumina particles;
s2, feeding the dried modified alumina particles, methyl vinyl silicone oil and hydrogen-containing silicone oil into a stirring machine to be uniformly mixed, feeding the mixture into a vacuum kneading machine to be primarily kneaded after stirring and mixing, feeding the coupling agent, the catalyst, the inhibitor, the crosslinking agent, the antioxidant and the flame retardant into the vacuum kneading machine to be secondarily kneaded after primary kneading is finished, placing the mixture obtained after secondary kneading into a vacuum machine to be vacuumized for 0.5-1.5 h, completely pumping out bubbles in the mixture to obtain a mixed base material, feeding the mixed base material into a calender to be calendered and molded, and then carrying out high-temperature vulcanization molding to obtain a base gasket;
s3, feeding the graphene fiber powder, hydrogen-containing silicone oil, a propanol solution, a catalyst, an inhibitor and a coupling agent into a planetary stirrer to be stirred at a low speed of 1050-1250 r/min for 90-100 min at a stirring temperature of 30-35 ℃ until the graphene fiber powder is completely and uniformly dispersed to obtain a graphene fiber dispersion liquid;
s4, brushing the graphene fiber dispersion liquid on the outer wall of the basic gasket, heating until the propanol solution is completely volatilized, enabling the graphene fibers to be regularly and directionally arranged on the surface of the basic gasket, enabling a coupling agent adsorbed on the surface of the graphene fibers to be subjected to a cross-linking reaction with unsaturated groups and hydrogen-containing silicone oil in the basic gasket, enabling the graphene fiber layer to be firmly attached to the surface of the basic gasket, repeating the operation for 10-15 times, and cooling the basic gasket attached with the graphene fiber layer after hot air vulcanization to obtain the heat-conducting silicone rubber pad.
3. A thermally conductive material according to claim 1, wherein: the coupling agent is a silane coupling agent containing vinyl groups, the catalyst is a platinum-vinyl siloxane complex with the concentration of 1800ppm, the inhibitor is ethynylcyclohexanol, the cross-linking agent is linear methyl hydrogen polysiloxane with the viscosity of 50-250 mpa · s, the hydrogen content is 6.1-6.5 wt%, the antioxidant is prepared by mixing an antioxidant 1010 and an antioxidant 1076 according to the mass ratio of 1: 1, and the flame retardant is prepared by mixing aluminum hydroxide and magnesium hydroxide according to the mass ratio of 1: 2.
4. A thermally conductive material according to claim 1, wherein: the viscosity range of the methyl vinyl silicone oil is 2550-2600 mPa.s, the mass fraction range of hydrogen contained in the hydrogen-containing silicone oil is 0.35-0.4%, the monofilament diameter in the graphene fiber powder is 22-23 μm, the length is 1100-1200 μm, the particle size of the modified alumina particles is 20-35 μm, and the concentration of the propanol solution is 10-15%.
5. A thermally conductive material according to claim 1, wherein: the modified alumina particles are prepared by mixing hexamethyldisilazane, methanol and spherical alumina particles, and the components are as follows according to the weight ratio: 30-45 parts of hexamethyldisilazane, 80-100 parts of methanol and 700-1000 parts of alumina particles.
6. A thermally conductive material according to claim 5, wherein: the preparation method of the modified alumina particles comprises the following steps:
s21, adding hexamethyldisilazane into propanol, and stirring and mixing by using an electromagnetic stirrer, wherein the stirring speed is 300-450 r/min, and the stirring time is 30min to prepare a mixed solution;
and S22, adding the spherical alumina particles into the mixed solution, and stirring and drying to obtain the modified spherical alumina particles.
7. The process of claim 2, wherein the step of preparing a thermally conductive material comprises: in the S2, the rotating speed of the stirrer is 3500 r/min-4000 r/min, the stirring time is 15 min-30 min, the high-temperature vulcanization molding temperature is 155-175 ℃, and the vulcanization time is 60 min-80 min.
8. The process of claim 2, wherein the step of preparing a thermally conductive material comprises: in the S2, the primary kneading temperature of the vacuum kneader is 95-100 ℃, the primary kneading time is 100-120 min, the secondary kneading temperature of the vacuum kneader is 120-130 ℃, and the secondary kneading time is 50-60 min.
9. The process of claim 2, wherein the step of preparing a thermally conductive material comprises: the temperature of hot air vulcanization in the S4 is 185-190 ℃, and the vulcanization time is 25-35 min.
10. A thermally conductive material according to claim 6, wherein: and the stirring time in the S22 is 0.5 h-1 h, the drying is carried out in two times, the drying temperature is 120 ℃ in the primary drying, the drying time is 1.5h, and the drying temperature is 160 ℃ in the secondary drying, and the drying time is 0.5 h.
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