CN114874442A - Si-H polymer, heat-conducting silica gel composition, and preparation method and application thereof - Google Patents
Si-H polymer, heat-conducting silica gel composition, and preparation method and application thereof Download PDFInfo
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- CN114874442A CN114874442A CN202210725097.7A CN202210725097A CN114874442A CN 114874442 A CN114874442 A CN 114874442A CN 202210725097 A CN202210725097 A CN 202210725097A CN 114874442 A CN114874442 A CN 114874442A
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- silicone gel
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- 239000000203 mixture Substances 0.000 title claims abstract description 47
- 229920000642 polymer Polymers 0.000 title claims abstract description 42
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910002027 silica gel Inorganic materials 0.000 title abstract description 18
- 239000000741 silica gel Substances 0.000 title abstract description 18
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 88
- -1 methoxyl groups Chemical group 0.000 claims abstract description 44
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 32
- MNFGEHQPOWJJBH-UHFFFAOYSA-N diethoxy-methyl-phenylsilane Chemical compound CCO[Si](C)(OCC)C1=CC=CC=C1 MNFGEHQPOWJJBH-UHFFFAOYSA-N 0.000 claims abstract description 19
- OLLFKUHHDPMQFR-UHFFFAOYSA-N dihydroxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](O)(O)C1=CC=CC=C1 OLLFKUHHDPMQFR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 7
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 39
- 239000000463 material Substances 0.000 claims description 31
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 28
- 229920002554 vinyl polymer Polymers 0.000 claims description 26
- 239000003054 catalyst Substances 0.000 claims description 18
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 18
- 229920002545 silicone oil Polymers 0.000 claims description 16
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 239000001257 hydrogen Substances 0.000 claims description 15
- 239000006229 carbon black Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 10
- 229910052697 platinum Inorganic materials 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000003112 inhibitor Substances 0.000 claims description 8
- 239000000945 filler Substances 0.000 claims description 7
- 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 description 6
- 239000003086 colorant Substances 0.000 claims description 6
- 239000003063 flame retardant Substances 0.000 claims description 6
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 3
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 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
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000011231 conductive filler Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 229910000077 silane Inorganic materials 0.000 claims description 3
- 239000011667 zinc carbonate Substances 0.000 claims description 3
- 235000004416 zinc carbonate Nutrition 0.000 claims description 3
- 229910000010 zinc carbonate Inorganic materials 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 2
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 claims description 2
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 claims description 2
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 229910052684 Cerium Inorganic materials 0.000 claims 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 238000001556 precipitation Methods 0.000 claims 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 claims 1
- 239000000499 gel Substances 0.000 abstract description 56
- 230000000740 bleeding effect Effects 0.000 abstract description 8
- 230000006872 improvement Effects 0.000 abstract description 6
- 239000003921 oil Substances 0.000 description 23
- 238000006243 chemical reaction Methods 0.000 description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 15
- 239000007788 liquid Substances 0.000 description 15
- 238000000034 method Methods 0.000 description 13
- 238000001816 cooling Methods 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 10
- 239000002904 solvent Substances 0.000 description 10
- 229960000583 acetic acid Drugs 0.000 description 8
- 239000012153 distilled water Substances 0.000 description 8
- 239000012362 glacial acetic acid Substances 0.000 description 8
- 230000008569 process Effects 0.000 description 8
- 238000004132 cross linking Methods 0.000 description 7
- PKTOVQRKCNPVKY-UHFFFAOYSA-N dimethoxy(methyl)silicon Chemical compound CO[Si](C)OC PKTOVQRKCNPVKY-UHFFFAOYSA-N 0.000 description 7
- 238000009472 formulation Methods 0.000 description 7
- XHFLOLLMZOTPSM-UHFFFAOYSA-M sodium;hydrogen carbonate;hydrate Chemical class [OH-].[Na+].OC(O)=O XHFLOLLMZOTPSM-UHFFFAOYSA-M 0.000 description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 6
- 239000008096 xylene Substances 0.000 description 6
- 239000004971 Cross linker Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 238000005336 cracking Methods 0.000 description 4
- 239000011541 reaction mixture Substances 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010703 silicon Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 2
- 229920001276 ammonium polyphosphate Polymers 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- CVQVSVBUMVSJES-UHFFFAOYSA-N dimethoxy-methyl-phenylsilane Chemical group CO[Si](C)(OC)C1=CC=CC=C1 CVQVSVBUMVSJES-UHFFFAOYSA-N 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 230000003335 steric effect Effects 0.000 description 2
- 239000004114 Ammonium polyphosphate Substances 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- HEFNNWSXXWATRW-UHFFFAOYSA-N Ibuprofen Chemical compound CC(C)CC1=CC=C(C(C)C(O)=O)C=C1 HEFNNWSXXWATRW-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical class [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 1
- 229920004482 WACKER® Polymers 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- NZAWGKXMYAMFTA-UHFFFAOYSA-N [Ce].[SiH3]O Chemical compound [Ce].[SiH3]O NZAWGKXMYAMFTA-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 1
- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 108010025899 gelatin film Proteins 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 150000004687 hexahydrates Chemical class 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229960004838 phosphoric acid Drugs 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000004804 winding 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
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/80—Siloxanes having aromatic substituents, e.g. phenyl side groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Materials Engineering (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a Si-H polymer, a heat-conducting silica gel composition, and a preparation method and application thereof. The Si-H polymer is obtained by performing polycondensation reaction on hydrosilane containing 2-3 methoxyl groups, methyl phenyl diethoxysilane and diphenyl silanediol; the molar ratio of methoxyl in the hydrosilane, diethoxyl in the methyl phenyl diethoxysilane and hydroxyl in the diphenyl silanediol is 1 (0.5-1.5) to (0.25-1). The Si-H polymer is added into the components of the heat-conducting silicone gel as a cross-linking agent, so that the oil leakage problem of the cured heat-conducting silicone gel can be effectively improved, and meanwhile, no obvious negative influence is brought to the flexibility of the heat-conducting silicone gel. In addition, the heat conductive property of the heat conductive silicone gel remains stable for a long period of time due to effective improvement of the oil bleeding problem.
Description
Technical Field
The invention relates to the field of heat-conducting silicone gel, in particular to a Si-H polymer, a heat-conducting silicone gel composition, and a preparation method and application thereof.
Background
With the proposal of strategic objectives of national 'carbon peak reaching' and 'carbon neutralization', the demand of the whole society on energy saving and emission reduction is more and more urgent, the energy storage material plays an important role in the redistribution of energy resources of the whole society through 'peak clipping and valley filling', and the power battery of the new energy automobile can store the energy resources at the time of electricity utilization valley, which is beneficial to the redistribution of the energy resources, so that the new energy automobile is vigorously supported and developed in recent years. New energy automobile power battery can produce the heat at the in-process of work, if these heats can not give off in time to the environment, will cause fatal injury to electronic components around the battery, also can shorten the life of battery simultaneously, so in new energy automobile power battery's equipment process, the heat conduction material can be used to the indispensable meeting to realize the heat dissipation of battery. The traditional heat conduction material has the phenomenon of internal hardening caused by continuous heating and temperature change, and has short service life. In recent years, thermally conductive silicone gels have become increasingly popular. The heat-conducting silicone gel is a heat-conducting material which can be deformed and cured, is soft and elastic and does not release any small molecules in the curing process. The heat-conducting silica gel not only has the functions of heat conduction, flame retardance, filling and shock absorption, but also has excellent performances of high and low temperature resistance, weather aging resistance, ozone resistance, electrical insulation, hydrophobicity, flame retardance, no toxicity, no corrosion, physiological inertia and the like. For the connection combination of exposed electronic elements, the reliability and the stability of the electronic elements and the whole machine can be improved through the sealing filling of the heat-conducting silicone gel, and the normal work of the electronic elements under the conditions of vibration, high temperature, high humidity, air pollution and the like is ensured.
However, the use of thermally conductive silicone gels has a problem of oil bleeding. Oil leakage can cause cracking of the heat-conducting silica gel, separation of the heat-conducting filler and pulverization, thereby causing reduction of the heat-conducting performance of the heat-conducting silica gel.
Chinese patent entitled a method for preparing stable high thermal conductive silicone gel provides a silicone gel having high stability and thermal conductivity, but it does not investigate the problem of oil bleeding of the thermal conductive silicone gel.
Therefore, there is a need to research and solve the problem that the thermally conductive silicone gel is easily oil-permeable.
Disclosure of Invention
The primary object of the present invention is to overcome the above-mentioned problem of the prior art that the thermally conductive silicone gel is prone to oil leakage, and to provide a Si — H polymer. The Si-H polymer is added into the components of the heat-conducting silicone gel as a cross-linking agent, so that the oil leakage problem of the cured heat-conducting silicone gel can be effectively improved, and meanwhile, no obvious negative influence is brought to the flexibility of the heat-conducting silicone gel. In addition, the heat conductive property of the heat conductive silicone gel remains stable for a long period of time due to effective improvement of the oil bleeding problem.
It is a further object of the present invention to provide the use of the above-described Si-H polymer as a crosslinking agent in the preparation of a thermally conductive silicone gel composition.
It is a further object of the present invention to provide a thermally conductive silicone gel composition.
It is a further object of the present invention to provide a method for preparing the above thermally conductive silicone gel composition.
The above object of the present invention is achieved by the following technical solutions:
the Si-H polymer is obtained by performing polycondensation reaction on hydrosilane containing 2-3 methoxyl groups, methyl phenyl diethoxysilane and diphenyl silanediol; the molar ratio of methoxyl in the hydrosilane, diethoxyl in the methyl phenyl diethoxysilane and hydroxyl in the diphenyl silanediol is 1 (0.5-1.5) to (0.25-1).
The heat-conducting silicone gel composition is cured by adding the cross-linking agent, and the oil leakage of the heat-conducting silicone gel can be improved to a certain extent by increasing the dosage of the conventional cross-linking agent, but the flexibility of the heat-conducting silicone gel is reduced by increasing the cross-linking degree. Therefore, it is difficult to balance the problems of oil bleeding and decreased flexibility of the thermally conductive silicone gel by adding the conventional crosslinking agent.
Through multiple experiments, the inventor of the invention finds that the polycondensation reaction is carried out by taking specific amounts of 2-3 methoxyl-containing hydrosilanes, methylphenyldiethoxysilane and diphenylsilanediol as raw materials, wherein the reactivity of methoxyl in the 2-3 methoxyl-containing hydrosilanes is slightly higher than that of ethoxyl in the methylphenyldiethoxysilane, so that the Si-H polymer obtained contains an appropriate amount of Si-H structures on the-Si-O-Si-O-Si-main chain and is introduced by the methylphenyldiethoxysilane
And diphenyl silanediol
The two sides of the main chain structure are distributed more uniformly, thereby bringing high steric hindrance to the Si-H structure. The Si-H polymer is added into the components of the heat-conducting silicone gel as a cross-linking agent, and can bring a proper cross-linking degree during curing, and simultaneously, the Si-H polymer can effectively improve the oil leakage problem of the cured heat-conducting silicone gel by matching with a high steric effect, and does not bring obvious negative influence on the flexibility of the heat-conducting silicone gel. And the oil leakage problem is effectively improved, so that the heat-conducting silica gel keeps good shape for a long time, and the phenomena of cracking and pulverization are avoided, so that the heat-conducting performance of the heat-conducting silica gel is kept stable for a long time.
If the hydrosilane containing 2-3 methoxyl groups or the silane containing 4 methoxyl groups is not added, the obtained polymer does not have Si-H bonds and cannot be used as a cross-linking agent; if the hydrosilane containing only one methoxyl group is added, the hydrosilane cannot generate polycondensation reaction; if no methylphenyldiethoxysilane is added, the main chain of the resulting Si-H polymer is absent
The content of Si-H is higher, and the silicon gel is used as a cross-linking agent, so that the cross-linking density of the heat-conducting silicon gel is increased, the flexibility of a glue film is reduced, and the hardness is higher; if no diphenylsilanediol is added, the main chain of the resulting Si-H polymer is absent
The steric effect is low, the polymer can not effectively bind polysiloxane molecules or silicone oil molecules and is used as a cross-linking agent, and the oil leakage problem improvement effect of the heat-conducting silicone gel is poor; if methylphenyldiethoxysilane is replaced with methylphenyldimethoxysilane, since the competitive reaction is not appropriate,
if the Si-H polymer is not uniformly distributed, the steric hindrance of the Si-H structure is low on both sides of the main chain structure of the obtained Si-H polymer, and the oil leakage problem of the heat-conducting silica gel is not well improved when the obtained Si-H polymer is used as a cross-linking agent.
Preferably, the hydrosilane is at least one of methyldimethoxysilane or trimethoxysilane.
Preferably, the number average molecular weight of the Si-H polymer is 1000-3000.
More preferably, the number average molecular weight of the Si-H polymer is 1500-2600.
Preferably, the polycondensation reaction comprises the steps of:
s1, mixing hydrogen-containing silane, methyl phenyl diethoxy silane and diphenyl silanediol, and stirring;
s2, adding a catalyst, and stirring and reacting for 1-2 hours at 80-90 ℃ to obtain the Si-H polymer.
More preferably, the process of mixing in step S1 is: adding hydrosilane, methyl phenyl diethoxysilane and diphenyl silanediol into the solvent, and mixing.
Further preferably, the solvent is one or more of toluene, cyclohexane, tetrahydrofuran or dichloromethane.
More preferably, the stirring in step S1 is followed by a cooling process, wherein the cooling temperature is 5 ℃ or lower.
More preferably, the catalyst in step S2 is one or more of glacial acetic acid, benzenesulfonic acid or phosphoric acid.
More preferably, after the stirring reaction in step S2 is finished, the method further includes a reaction termination process and a separation and purification process; the specific process of the termination reaction treatment is as follows: adding a pH regulator until the reaction system is alkaline, and continuously stirring for 20-60 min; the specific process of the separation and purification treatment comprises the following steps: adding water, stirring for 20-60 min, standing, separating, washing with distilled water for 1-3 times, heating to 120-125 ℃, distilling at-0.08-0.10 MPa for 1-3 h, and distilling off the solvent to obtain colorless transparent liquid.
Further preferably, the pH adjuster is at least one of a sodium hydroxide solution or a saturated sodium bicarbonate solution.
The use of the above-described Si-H polymer as a cross-linking agent in the preparation of a thermally conductive silicone gel composition is also within the scope of the present invention.
A thermally conductive silicone gel composition comprising component A and component B; wherein:
the component A comprises the following components in parts by weight: 35-50 parts of base material, 45-55 parts of heat-conducting filler, 1.5-5.5 parts of heat-resistant agent, 0.5-2.5 parts of coloring agent and 0.0015-0.003 part of catalyst;
the component B comprises the following components in parts by weight: 35 to 50 parts of a base material, 45 to 55 parts of a heat-conducting filler, 1.5 to 5.5 parts of the Si-H polymer described in any one of claims 1 to 3, 1 to 8 parts of hydrogen-containing silicone oil, 1.5 to 5.5 parts of a heat-resistant agent, and 0.0005 to 0.0015 part of an inhibitor;
the mass ratio of the component A to the component B is 1 (0.95-1.05);
the base material comprises the following components in parts by weight: 10-20 parts of first vinyl terminated polysiloxane, 10-20 parts of second vinyl terminated polysiloxane, 30-60 parts of a flame retardant, 1-10 parts of white carbon black and 5-10 parts of dimethyl silicone oil;
the viscosity of the first vinyl terminated polysiloxane is more than or equal to 200 and less than or equal to 1000mPa.s, and the viscosity of the second vinyl terminated polysiloxane is more than or equal to 1000 and less than or equal to 5000 mPa.s.
The present invention adds the above-described Si-H polymer as a crosslinking agent to the components of the thermally conductive silicone gel composition. In the process of curing the heat-conducting silicone gel composition, the vinyl-terminated polysiloxane and hydrogen-containing silicone oil are subjected to hydrosilylation to enable the molecular chain of the vinyl-terminated polysiloxane to be chain extended, and a framework is formed; simultaneously, vinyl-terminated polysiloxane and Si-H polymer are crosslinked, so that the crosslinking degree of the vinyl-terminated polysiloxane is properly improved on one hand, and the crosslinking degree of the vinyl-terminated polysiloxane is properly improved on the other hand
The vinyl terminated polysiloxane is uniformly distributed on two sides of a main chain structure of the cross-linking agent, high steric hindrance is brought to a Si-H structure, winding and wrapping of vinyl terminated polysiloxane molecules are achieved through combined action of proper cross-linking degree and high steric hindrance effect, and therefore the oil leakage problem of the cured heat-conducting silicone gel is effectively solved, and the heat-conducting silicone gel keeps good flexibility due to the fact that the cross-linking degree is properly improved. And the oil leakage problem is effectively improved, so that the heat-conducting silica gel keeps good shape for a long time, and the phenomena of cracking and pulverization are avoided, so that the heat-conducting performance of the heat-conducting silica gel is kept stable for a long time.
Two vinyl-terminated polysiloxanes with different viscosities are selected from the base materials of the heat-conducting silicone gel composition, so that the hardness and flexibility of the heat-conducting silicone gel composition can be regulated and controlled.
Namely, the oil leakage problem of the heat-conducting silica gel formed after the heat-conducting silica gel composition is cured is effectively improved, and the heat-conducting silica gel composition keeps better; in addition, the heat conductivity is stable for a long period of time due to effective improvement of the oil problem.
The thermally conductive filler is added to the components in a conventional form, for example, a powder form.
Preferably, the heat conducting filler is one or more of aluminum oxide, zinc oxide, boron nitride, aluminum nitride, ceramic powder or aluminum.
Preferably, the heat-resistant agent is one or more of zinc carbonate, calcined titanium dioxide or cerium silanol.
Preferably, the colorant is one or more of carbon black, black paste, phthalocyanine blue, phthalocyanine green and iron red.
Preferably, the catalyst is a platinum catalyst.
More preferably, the platinum catalyst is one or more of chloroplatinic acid hexahydrate, a complex of platinum and vinyl silicone oil or a complex of platinum and ethynyl
Further preferably, the platinum catalyst is a complex of platinum and ethynyl, and the catalyst is selected to facilitate control of the operating time and overall cure time.
Preferably, the inhibitor is one or more of alkyl maleate, alkyl fumarate, vinyl ring or alkynol.
Further preferably, the inhibitor is an alkynol, and the inhibitor is selected to be more favorable for controlling the operation time and the curing time during curing.
Preferably, the flame retardant is one or more of triethyl phosphate, APP, MCA or aluminium hydroxide;
preferably, the white carbon black is one or two of gas-phase white carbon black or precipitated white carbon black.
Preferably, the specific surface area of the white carbon black is 120-400 m 2 /g。
Preferably, the viscosity of the dimethyl silicone oil is 50-2000 mPas.
More preferably, the viscosity of the dimethylsilicone fluid is 1000 mpa.s.
Preferably, the hydrogen-containing silicone oil is straight-chain type hydrogen-containing polydimethylsiloxane or branched-chain type hydrogen-containing polydimethylsiloxane.
Preferably, the viscosity of the hydrogen-containing silicone oil is 50-500 mPa.s.
Preferably, the hydrogen content of the hydrogen-containing silicone oil is 0.12-0.18%.
Preferably, the viscosity of the first vinyl-terminated polysiloxane is 250 ≦ η ≦ 300mPa.s, and the viscosity of the second vinyl-terminated polysiloxane is 1000 ≦ η ≦ 3000 mPa.s.
Preferably, the first vinyl-terminated polysiloxane has the structure shown in formula (i):
wherein n is an integer of 60-120;
the second vinyl-terminated polysiloxane has a structure shown as a formula (II)
Wherein m is an integer of 150 to 300.
Preferably, the vinyl content of the first vinyl-terminated polysiloxane is 1.5% to 4.5%.
Preferably, the vinyl content of the second vinyl-terminated polysiloxane is from 0.5% to 1.2%.
The preparation method of the heat-conducting silica gel composition comprises the following steps: mixing the components of the base material to obtain the base material for later use; mixing the components of the component A to obtain a component A; and mixing the components of the component B to obtain the component B.
Preferably, after the components of the component A are mixed, the operation of stirring and dispersing is also included; after the components of the component B are mixed, the operation of stirring and dispersing is also included.
Compared with the prior art, the invention has the beneficial effects that:
(1) the Si-H polymer is added into the components of the heat-conducting silicone gel as a cross-linking agent, so that the oil leakage problem of the cured heat-conducting silicone gel can be effectively solved, and no obvious negative influence is brought to the mechanical property of the heat-conducting silicone gel.
(2) The heat-conducting silica gel composition disclosed by the invention has the advantages that the oil leakage problem of the heat-conducting silica gel formed after curing is effectively improved, and the heat-conducting silica gel composition also has good mechanical property and heat-conducting property.
Detailed Description
In order to more clearly and completely describe the technical scheme of the invention, the invention is further described in detail by the specific embodiments, and it should be understood that the specific embodiments described herein are only used for explaining the invention, and are not used for limiting the invention, and various changes can be made within the scope defined by the claims of the invention.
Some of the reagents selected in the examples and comparative examples of the present invention are described below:
first vinyl terminated polysiloxane 1 #: v-250, vinyl content 0.55%, viscosity: 250mPa.s, Jiangsu family, Happy New materials Co., Ltd;
first vinyl terminated polysiloxane # 2: c-1 (300), vinyl content 0.54%, viscosity: 300mPa.s, Guangzhou Jitai chemical Co., Ltd;
second vinyl terminated polysiloxane 1 #: v-2000, vinyl content 0.20%, viscosity: 1000mpa.s, york family, new materials, ltd;
second vinyl terminated polysiloxane # 2: c-1 (2000), vinyl content 0.21%, viscosity: 3000mpa.s, guangzhou Jitai chemical corporation;
flame retardant: A8D16, a compound of aluminum hydroxide and ammonium polyphosphate, Shenzhen Jinhao Hui exhibition industry Co., Ltd;
white carbon black: h30, fumed silica, wacker chemistry;
dimethyl silicone oil: PMX-200 and 1000mPa.s, Dow Corning;
crosslinker # 1 (Si-H polymer # 1): self-made, the preparation process is as follows: dissolving methyldimethoxysilane, methylphenyldiethoxysilane and diphenylsilanediol in a molar ratio of 1:1:0.5 in xylene, putting into a reaction kettle, stirring and cooling to 3 ℃, then adding glacial acetic acid, heating to 82 ℃, and stirring and reacting for 3 hours; then dropwise adding saturated sodium bicarbonate water solution to make the reaction solution alkaline, continuously stirring for 0.5h, adding water and stirring for 0.5h, standing, and draining the lower layer liquid after layering; the reaction mixture was washed with distilled water 2 times and then dried, and the solvent was distilled off to obtain a colorless transparent liquid, whose number average molecular weight was 1500.
Crosslinker # 2 (Si-H polymer # 2): the preparation method comprises the following steps: dissolving methyltrimethoxysilane, methylphenyldiethoxysilane and diphenylsilanediol in a molar ratio of 1:1.5:0.75 in XX, adding into a reaction kettle, stirring and cooling to 45 ℃, adding glacial acetic acid, heating to 82 ℃, and stirring and reacting for 3 hours; then dropwise adding saturated sodium bicarbonate water solution to make the reaction solution alkaline, continuously stirring for 0.5h, adding water and stirring for 0.5h, standing, and draining the lower layer liquid after layering; the reaction product was washed with distilled water and dried, and the solvent was distilled off to obtain a colorless transparent liquid, the number average molecular weight of which was 2600.
Crosslinker # 3 (Si-H polymer # 3): self-made, the preparation process is as follows: dissolving methyldimethoxysilane, methylphenyldiethoxysilane and diphenylsilanediol in a molar ratio of 1:0.5:1 in xylene, putting into a reaction kettle, stirring and cooling to 3 ℃, then adding glacial acetic acid, heating to 82 ℃, and stirring and reacting for 3 hours; then dropwise adding saturated sodium bicarbonate water solution to make the reaction solution alkaline, continuously stirring for 0.5h, adding water and stirring for 0.5h, standing, and draining the lower layer liquid after layering; the reaction mixture was washed with distilled water 2 times and then dried, and the solvent was distilled off to obtain a colorless transparent liquid, the number average molecular weight of which was determined to be 1900.
Crosslinker # 4 (Si-H polymer # 4): self-made, the preparation process is as follows: dissolving methyldimethoxysilane, methylphenyldiethoxysilane and diphenylsilanediol in a molar ratio of 1:1.5:0.25 in xylene, putting into a reaction kettle, stirring and cooling to 3 ℃, adding glacial acetic acid, heating to 82 ℃, and stirring and reacting for 3 hours; then dropwise adding saturated sodium bicarbonate water solution to make the reaction solution alkaline, continuously stirring for 0.5h, adding water and stirring for 0.5h, standing, and draining the lower layer liquid after layering; the reaction product was washed with distilled water 2 times and then dried, and the solvent was distilled off to obtain a colorless transparent liquid whose number average molecular weight was 2300.
Crosslinking agent # 5 (Si — H polymer # 5): self-made, the preparation process is as follows: dissolving methyldimethoxysilane and diphenylsilanediol in a molar ratio of 1:0.5 in xylene, putting into a reaction kettle, stirring and cooling to 3 ℃, then adding glacial acetic acid, heating to 82 ℃, and stirring and reacting for 3 hours; then dropwise adding saturated sodium bicarbonate water solution to make the reaction solution alkaline, continuously stirring for 0.5h, adding water and stirring for 0.5h, standing, and draining the lower layer liquid after layering; the reaction was washed with distilled water 2 times and dried, and the solvent was distilled off to obtain a colorless transparent liquid whose molecular weight was measured to be 900.
Crosslinking agent # 6 (Si — H polymer # 6): self-made, the preparation process is as follows: dissolving methyldimethoxysilane and methylphenyldiethoxysilane in a molar ratio of 1:1 in xylene, putting into a reaction kettle, stirring and cooling to 3 ℃, adding glacial acetic acid, heating to 82 ℃, and stirring and reacting for 3 hours; then dropwise adding saturated sodium bicarbonate water solution to make the reaction solution alkaline, continuously stirring for 0.5h, adding water and stirring for 0.5h, standing, and draining the lower layer liquid after layering; the reaction mixture was washed with distilled water 2 times and then dried, and the solvent was distilled off to obtain a colorless transparent liquid whose number average molecular weight was measured to be 1600.
Crosslinking agent # 7 (Si — H polymer # 7): self-made, the preparation process is as follows: dissolving methyldimethoxysilane, methylphenyldimethoxysilane and diphenylsilanediol in a molar ratio of 1:1:0.5 in xylene, putting into a reaction kettle, stirring and cooling to 3 ℃, then adding glacial acetic acid, heating to 82 ℃, and stirring and reacting for 3 hours; then dropwise adding saturated sodium bicarbonate water solution to make the reaction solution alkaline, continuously stirring for 0.5h, adding water and stirring for 0.5h, standing, and draining the lower layer liquid after layering; the reaction mixture was washed with distilled water 2 times and dried, and the solvent was distilled off to obtain a colorless transparent liquid whose number average molecular weight was measured to be 2100.
Crosslinking agent 8#: commercially available, RH-LHC-3, 300mPa.s, Ningbo Runzhe high New materials, Ltd;
heat-conducting filler: GD-S151C, a complex of spherical alumina and angular alumina, foshanggo new materials gmbh;
heat-resistant agent: zinc carbonate, Shandong Xinya New materials GmbH;
colorant: black paste, new materials of john carol limited;
catalyst # 1: PT-2500DZ, platinum catalyst, Guangzhou silicon friend New materials science and technology Co., Ltd;
catalyst # 2: PT-5000, platinum catalyst, Guangzhou silicon friend New materials science and technology Co., Ltd;
hydrogen-containing silicone oil 1 #: SH-18, H group content 0.18%, Jiangsu family Happy New Material Co., Ltd;
hydrogen-containing silicone oil 2#: d-15, H group content 0.12%, Jiangsu family Happy New Material Co., Ltd;
inhibitor # 1: VM-18, vinyl double-end, Zhejiang Jiahui New materials Co.
Inhibitor # 2: VM-20, alkynol, Zhejiang Jiahui New materials, Inc.
Examples 1 to 6
Examples 1-16 provide a series of thermally conductive silicone gel compositions having formulations with the amounts of each component listed in tables 1-5.
Base material 1# -base material 5 #: self-made, and the composition is shown in table 1; the preparation process comprises the following steps: adding the components into a power mixer, stirring and dispersing uniformly, heating to 125 ℃, dehydrating for 120 minutes under-0.09 MPa, testing the water content to be lower than 300ppm, and cooling to obtain the water-based paint.
TABLE 1 composition of the base materials
The component A1# to the component A8# are self-made, and the composition is shown in Table 2: the preparation process comprises the following steps: the following components are added into a power mixer to be uniformly stirred and dispersed, and the high-performance high-efficiency energy-saving material is obtained.
TABLE 2 compositions of Components A1# -A8 #
| Components | Component A1# | Component A2# | Component A3# | Component A4# | Component A5# | Component A6# | Component A7# | Component A8# |
| Base material 1# | 43 | 50 | 35 | / | / | / | / | 43 |
| Base material No. 2 | / | / | / | 43 | / | / | / | / |
| Base material No. 3 | / | / | / | / | 43 | / | / | / |
| Base material 4# | / | / | / | / | / | 43 | / | / |
| Base material 5# | / | / | / | / | / | / | 43 | / |
| Heat conductive filler | 50 | 45 | 55 | 50 | 50 | 50 | 50 | 50 |
| Heat-resistant agent | 5 | 1.5 | 5.5 | 5 | 5 | 5 | 5 | 5 |
| Coloring agent | 2 | 0.5 | 2.5 | 2 | 2 | 2 | 2 | 2 |
| Catalyst 1# | 0.002 | 0.0015 | 0.003 | 0.002 | 0.002 | 0.002 | 0.002 | / |
| Catalyst No. 2 | / | / | / | / | / | / | / | 0.002 |
The component B1# -the component B12#, which is prepared by self and has the composition shown in Table 3: the preparation process comprises the following steps: the following components are added into a power mixer to be uniformly stirred and dispersed, and the high-performance high-efficiency energy-saving material is obtained.
TABLE 3 composition of Components B1# -B12 #
TABLE 4 formulations of examples 1-10
TABLE 5 formulations of examples 11-16
Comparative example 1
This comparative example provides a thermally conductive silicone gel composition, which is different from example 1 in the following formulation: the crosslinking agent 1# in component B1# was replaced with crosslinking agent 5 #.
Comparative example 2
This comparative example provides a thermally conductive silicone gel composition, which differs from example 1 in the formulation: the crosslinking agent 1# in component B1# was replaced with crosslinking agent 6 #.
Comparative example 3
This comparative example provides a thermally conductive silicone gel composition, which differs from example 1 in the formulation: the crosslinking agent 1# in component B1# was replaced with crosslinking agent 7 #.
Comparative example 4
This comparative example provides a thermally conductive silicone gel composition, which differs from example 1 in the formulation: the crosslinking agent 1# in component B1# was replaced with crosslinking agent 8 #.
Performance testing
The thermally conductive silicone gel compositions of the examples and comparative examples were taken, the component a and the component B of the examples and comparative examples were mixed, cured, and the cured gels were subjected to a performance test. The test standards or methods are as follows:
appearance: and observing whether the solidified gel is a uniform elastomer or not and whether an oily matter is separated out from the surface or not.
Tensile strength: GB/T528-2009.
Elongation at break: GB/T528-2009.
Hardness (Shore-00): GB/T531.1-2008.
Coefficient of thermal conductivity: GB/T10297-2015.
Flame retardant property: ANSI UL 94-2018.
Volume resistivity: GB/T31838.2-2019.
Dielectric strength: GB/T1408.1-2016.
Thermal conductivity after high and low temperature cycling: reference ISO 22007-2; completely curing for 7 days at 25 ℃; low temperature: -40 ℃, time: 30 min; high temperature: 85 ℃, time: 30 min; temperature conversion time: 5 min; cycle number: 1000 times.
Thermal conductivity after double 85 aging: reference ISO 22007-2; completely curing for 7 days at 25 ℃; ② 85 ℃ and 85% humidity for 1000 h.
Sealing after high-low temperature circulation: GBT15905-1995, the gel film was solidified and cut into a cake having a diameter of 5mm and a thickness of 2mm, placed on 3 layers of qualitative filter paper, placed in an environment of 23 ℃ and RH 50% for 7 days, and observed whether there was an oily mark on the filter paper and whether there was shrinkage, cracking and falling off of the gel.
The test results are shown in table 5.
TABLE 5 results of Performance test
As can be seen from table 5, the heat-conductive silicone gel compositions of examples 1 to 16 have appropriate toughness (tensile strength 41 to 48MPa, elongation at break 50% to 56%) and low hardness (40 to 45%) after curing, and the oil bleeding problem is significantly improved, which indicates that the oil bleeding problem of the heat-conductive silicone gel formed after curing the heat-conductive silicone gel composition of the present invention is effectively improved, and good flexibility is maintained; in addition, the heat conductivity is stable for a long period of time due to effective improvement of the oil problem.
Comparative example 1 added cross-linking agent # 5, the oil bleeding problem was improved, but the cured gel had a greater hardness, which affected its use; the cross-linking agent No. 6 is added in the comparative example 2, the cross-linking agent No. 7 is added in the comparative example 3, and the cross-linking agent No. 8 is added in the comparative example 4, the oil leakage problem of the three is not effectively improved, and the heat conducting property can not be kept stable for a long time.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. The Si-H polymer is characterized by being obtained by carrying out polycondensation reaction on hydrosilane containing 2-3 methoxyl groups, methyl phenyl diethoxy silane and diphenyl silanediol; the molar ratio of methoxyl in the hydrosilane, diethoxyl in the methyl phenyl diethoxysilane and hydroxyl in the diphenyl silanediol is 1 (0.5-1.5) to (0.25-1).
2. The Si-H polymer according to claim 1, wherein the number average molecular weight of the Si-H polymer is 1000 to 3000.
3. The Si-H polymer of claim 1, wherein said polycondensation reaction comprises the steps of:
s1, mixing hydrogen-containing silane, methyl phenyl diethoxy silane and diphenyl silanediol, and stirring;
s2, adding a catalyst, and stirring and reacting for 1-2 hours at 80-90 ℃ to obtain the Si-H polymer.
4. Use of the Si-H polymer of any one of claims 1 to 3 as a cross-linking agent in the preparation of a thermally conductive silicone gel composition.
5. A thermally conductive silicone gel composition comprising component a and component B; wherein:
the component A comprises the following components in parts by weight: 35-50 parts of base material, 45-55 parts of heat-conducting filler, 1.5-5.5 parts of heat-resistant agent, 0.5-2.5 parts of coloring agent and 0.0015-0.003 part of catalyst;
the component B comprises the following components in parts by weight: 35 to 50 parts of a base material, 45 to 55 parts of a heat-conducting filler, 1.5 to 5.5 parts of the Si-H polymer described in any one of claims 1 to 3, 1 to 8 parts of hydrogen-containing silicone oil, 1.5 to 5.5 parts of a heat-resistant agent, and 0.0005 to 0.0015 part of an inhibitor;
the mass ratio of the component A to the component B is 1 (0.95-1.05);
the base material comprises the following components in parts by weight: 10-20 parts of first vinyl terminated polysiloxane, 10-20 parts of second vinyl terminated polysiloxane, 30-60 parts of a flame retardant, 1-10 parts of white carbon black and 5-10 parts of dimethyl silicone oil;
the viscosity of the first vinyl terminated polysiloxane is more than or equal to 200 and less than or equal to 1000mPa.s, and the viscosity of the second vinyl terminated polysiloxane is more than or equal to 1000 and less than or equal to 5000 mPa.s.
6. The thermally conductive silicone gel composition of claim 5, wherein the thermally conductive filler is one or more of alumina, zinc oxide, boron nitride, aluminum nitride, ceramic powder, or aluminum;
the heat-resistant agent is one or more of zinc carbonate, calcined titanium dioxide or silanol cerium;
the colorant is one or more of carbon black, black paste, phthalocyanine blue, phthalocyanine green and iron red;
the catalyst is a platinum catalyst;
the inhibitor is one or more of alkyl maleate, alkyl fumarate, vinyl ring body or alkynol;
the flame retardant is one or more of triethyl phosphate, APP, MCA or aluminum hydroxide;
the white carbon black is one or two of gas-phase white carbon black or precipitation white carbon black;
the viscosity of the dimethyl silicone oil is 50-2000 mPa.s.
7. A thermally conductive silicone gel composition according to claim 5, wherein said hydrogen-containing silicone oil has a hydrogen content of 0.12% to 0.18%.
8. The thermally conductive silicone gel composition of claim 5, wherein the first vinyl terminated polysiloxane has a structure according to formula (I):
wherein n is an integer of 60-120;
the second vinyl-terminated polysiloxane has a structure shown as a formula (II)
Wherein m is an integer of 150 to 300.
9. The thermally conductive silicone gel composition of claim 5, wherein said first vinyl terminated polysiloxane has a vinyl content of 1.5% to 4.5%; the vinyl content of the second vinyl-terminated polysiloxane is 0.5-1.2%.
10. A method of making a thermally conductive silicone gel composition as claimed in any one of claims 5 to 9, comprising the steps of: mixing the components of the base material to obtain the base material for later use; mixing the components of the component A to obtain a component A; and mixing the components of the component B to obtain the component B.
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|---|---|---|---|---|
| CN115304920A (en) * | 2022-08-31 | 2022-11-08 | 惠州普赛达新材料有限公司 | Organic silicon foaming material and preparation method and application thereof |
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