CN114507506A - Single-component addition type heat-conducting adhesive and preparation method and application thereof - Google Patents
Single-component addition type heat-conducting adhesive and preparation method and application thereof Download PDFInfo
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- CN114507506A CN114507506A CN202210164713.6A CN202210164713A CN114507506A CN 114507506 A CN114507506 A CN 114507506A CN 202210164713 A CN202210164713 A CN 202210164713A CN 114507506 A CN114507506 A CN 114507506A
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- 239000000853 adhesive Substances 0.000 title claims abstract description 63
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title abstract description 9
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 29
- 239000000945 filler Substances 0.000 claims abstract description 26
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 25
- 239000001257 hydrogen Substances 0.000 claims abstract description 24
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 24
- -1 polysiloxane Polymers 0.000 claims abstract description 24
- 229920002545 silicone oil Polymers 0.000 claims abstract description 23
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003054 catalyst Substances 0.000 claims abstract description 18
- 239000003112 inhibitor Substances 0.000 claims abstract description 13
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 6
- 238000009835 boiling Methods 0.000 claims description 25
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 18
- 229910000077 silane Inorganic materials 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 17
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 16
- 239000012756 surface treatment agent Substances 0.000 claims description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 13
- 239000007822 coupling agent Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 229910052697 platinum Inorganic materials 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 7
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000011231 conductive filler Substances 0.000 claims description 5
- JMXKSZRRTHPKDL-UHFFFAOYSA-N titanium ethoxide Chemical compound [Ti+4].CC[O-].CC[O-].CC[O-].CC[O-] JMXKSZRRTHPKDL-UHFFFAOYSA-N 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 125000000217 alkyl group Chemical group 0.000 claims description 4
- INASARODRJUTTN-UHFFFAOYSA-N 3-methyldodec-1-yn-3-ol Chemical compound CCCCCCCCCC(C)(O)C#C INASARODRJUTTN-UHFFFAOYSA-N 0.000 claims description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 3
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 claims description 3
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 3
- MOIJCDGIMUADRQ-UHFFFAOYSA-N 3,3-diphenylprop-1-yn-1-ol Chemical compound C=1C=CC=CC=1C(C#CO)C1=CC=CC=C1 MOIJCDGIMUADRQ-UHFFFAOYSA-N 0.000 claims description 2
- OWRXWSVBJIIORE-UHFFFAOYSA-N 3,7,11-trimethyldodec-1-yn-3-ol Chemical compound CC(C)CCCC(C)CCCC(C)(O)C#C OWRXWSVBJIIORE-UHFFFAOYSA-N 0.000 claims description 2
- 229910052580 B4C Inorganic materials 0.000 claims description 2
- 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
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002318 adhesion promoter Substances 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 claims description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000004917 carbon fiber Substances 0.000 claims description 2
- 239000013522 chelant 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
- 229910003460 diamond Inorganic materials 0.000 claims description 2
- 239000010432 diamond Substances 0.000 claims description 2
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 239000003292 glue Substances 0.000 abstract description 4
- 239000000919 ceramic Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 15
- 229920002379 silicone rubber Polymers 0.000 description 10
- 239000000203 mixture Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 239000004945 silicone rubber Substances 0.000 description 6
- 238000010438 heat treatment Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- 239000004944 Liquid Silicone Rubber Substances 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 3
- SCPWMSBAGXEGPW-UHFFFAOYSA-N dodecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCC[Si](OC)(OC)OC SCPWMSBAGXEGPW-UHFFFAOYSA-N 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- JTSZXOTUXGOAJS-UHFFFAOYSA-N ethenyl-[ethenyl(dimethyl)silyl]oxy-dimethylsilane;platinum Chemical group [Pt].C=C[Si](C)(C)O[Si](C)(C)C=C.C=C[Si](C)(C)O[Si](C)(C)C=C JTSZXOTUXGOAJS-UHFFFAOYSA-N 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000012763 reinforcing filler Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003002 pH adjusting agent Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives 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; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention belongs to the technical field of heat-conducting adhesive glue, and discloses a single-component addition type heat-conducting adhesive glue, and a preparation method and application thereof. The single-component addition type heat-conducting adhesive comprises the following components in parts by weight: 20-150 parts of vinyl silicone oil, 10-750 parts of heat-conducting filler, 0.5-10 parts of surface treating agent, 0.1-2 parts of tackifier, 0.01-0.5 part of pH value regulator, 0.1-10 parts of hydrogen-containing polysiloxane, 0.1-1 part of catalyst and 0.1-1 part of inhibitor; the single-component addition type heat-conducting adhesive provided by the invention has high stability, heat conductivity and adhesiveness. The single-component addition type heat-conducting adhesive can be used for bonding and sealing in the fields of electromagnetic ovens, microwave ovens, PTC ceramic heaters, other electric control boxes and the like.
Description
Technical Field
The invention relates to the technical field of heat-conducting adhesive, in particular to single-component addition type heat-conducting adhesive and a preparation method and application thereof.
Background
Compared with adhesive systems such as polyurethane, epoxy and the like, the silicone rubber has good electrical property, heat resistance, aging resistance, chemical inertness and the like, and can be used for a long time at the temperature of-60-200 ℃. With the rapid development of the electronic industry, the addition type liquid silicone rubber has excellent properties, so that the addition type liquid silicone rubber has wide application in the field of electronic element packaging. Compared with a two-component system, the single-component addition type liquid silicone rubber has the advantages of simple construction process, convenience in operation and the like, and in addition, rapid curing can be realized through heating, so that the construction efficiency is improved, and therefore, the single-component addition type liquid silicone rubber has wide application prospects in the field of electronic packaging in recent years.
As the density and integration of electronic components increase, it is required to use a heat conductive silicone rubber composition having effective heat radiation characteristics. At present, in order to improve the heat conductivity of the heat conductive silicone rubber composition, a large amount of heat conductive filler needs to be filled, but this increases the viscosity of the heat conductive silicone rubber composition, deteriorates workability, workability and physical properties, and affects the adhesion of the heat conductive silicone rubber composition to a substrate.
Therefore, it is necessary to develop a one-component addition type silicone rubber having good thermal conductivity, low viscosity, high strength and good adhesion.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a single-component addition type heat-conducting adhesive and a preparation method and application thereof.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
in a first aspect, the invention provides a single-component addition type heat-conducting adhesive which comprises the following components in parts by weight:
20-150 parts of vinyl silicone oil, 10-750 parts of heat-conducting filler, 0.5-10 parts of surface treating agent, 0.1-2 parts of tackifier, 0.01-0.5 part of pH value regulator, 0.1-10 parts of hydrogen-containing polysiloxane, 0.1-1 part of catalyst and 0.1-1 part of inhibitor;
the surface treatment agent comprises silane with a boiling point higher than 210 ℃ and silane with a boiling point lower than 160 ℃;
the adhesion promoter includes a titanate coupling agent. In the single-component addition type heat-conducting adhesive, the heat-conducting filler is treated by a multi-component surface treatment system: (1) the silane with the boiling point higher than 210 ℃ has larger molecular weight, so that more surface coating can be carried out on the heat-conducting filler; (2) the silane with a lower molecular weight and a boiling point lower than 160 ℃ is subjected to synergistic treatment, so that the surface of the heat-conducting filler can be better silanized, the surface wettability of the heat-conducting filler is greatly improved, and the problem that the silane with a boiling point higher than 210 ℃ is difficult to completely react with hydroxyl on the surface of the heat-conducting filler due to steric hindrance of the silane with a boiling point higher than 210 ℃ is avoided, so that heat-conducting filler particles can be better dispersed in a base material, the compatibility with the base material is improved, and good operability can be shown even in the presence of a large amount of heat-conducting filler; (3) when the single-component addition type heat-conducting adhesive is cured, the adhesive has good tensile strength and elongation even if no reinforcing filler is added.
Preferably, the single-component addition type heat-conducting adhesive comprises the following components in parts by weight:
80-150 parts of vinyl silicone oil, 50-750 parts of heat-conducting filler, 0.8-5.5 parts of surface treating agent, 0.2-2 parts of tackifier, 0.1-0.5 part of pH value regulator, 0.5-6.5 parts of hydrogen-containing polysiloxane, 0.1-0.5 part of catalyst and 0.1-0.5 part of inhibitor.
As a preferred embodiment of the single-component addition type heat-conducting adhesive, the silane with the boiling point higher than 210 ℃ has a structure shown in a formula (I) or a formula (II);
wherein n is more than or equal to 6, R is alkyl with more than 6 carbons, and X, Y, Z is a hydrolyzable group.
In a preferred embodiment of the one-component addition type heat-conductive adhesive according to the present invention, the silane having a boiling point of less than 160 ℃ is at least one selected from the group consisting of vinyltrimethoxysilane, methyltrimethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, and methyltriethoxysilane.
In a preferred embodiment of the one-component addition type heat-conducting adhesive according to the present invention, the mass of the silane having a boiling point higher than 210 ℃ or the silane having a boiling point lower than 160 ℃ is 0.01 to 1% of the mass of the heat-conducting filler.
As a preferred embodiment of the one-component addition-type thermal conductive adhesive according to the present invention, the titanate coupling agent is at least one of ethyl titanate, butyl titanate, isopropyl titanate, tetra-t-butyl titanate, tetra-t-amyl titanate, and a chelate of titanate.
As a preferred embodiment of the single-component addition type heat-conducting adhesive glue, the tackifier also comprises a structure R1Si(R2)3A compound of (1);
wherein, R is1Is at least one of methoxy, epoxypropyl, vinyl and acetoxymethyl or alkyl substituted by the group; r2Is at least one group of methoxyl, ethoxyl and propoxyl.
According to the single-component addition type heat-conducting adhesive disclosed by the invention, different tackifiers are matched, so that the prepared single-component addition type heat-conducting adhesive has universality for bonding of base materials, and no additional tackifier is required to be synthesized.
As a preferred embodiment of the one-component addition type heat-conducting adhesive according to the present invention, the vinyl silicone oil is at least one of silicone oils containing terminal vinyl groups or side vinyl groups; the viscosity of the vinyl silicone oil is 500-5000 mPa.s, and the content of vinyl is 0.1-1%.
As a preferred embodiment of the single-component addition type heat-conducting adhesive according to the present invention, the hydrogen-containing polysiloxane is at least one of terminal hydrogen-containing silicone oil or side hydrogen-containing silicone oil; the hydrogenpolysiloxane has a viscosity of 10 mPas-500 mPas (preferably 50 mPas-100 mPas) and a hydrogen content of 0.01-1.6% (preferably 0.07-0.75%).
Preferably, the ratio of the hydrogen content in the hydrogenpolysiloxane to the vinyl content in the vinyl silicone oil is 1 (1-5).
As a preferred embodiment of the one-component addition type heat-conducting adhesive according to the present invention, the heat-conducting filler is at least one of silver powder, aluminum powder, copper powder, nickel powder, carbon powder, aluminum oxide, zinc oxide, magnesium oxide, titanium oxide, boron nitride, aluminum nitride, carbon fiber, boron carbide, silicon carbide, graphene, diamond, and silicon micropowder.
Preferably, the average particle size of the heat conductive filler is 0.5 μm to 20 μm; the morphology of the thermally conductive filler is preferably spherical or spheroidal.
As a preferred embodiment of the one-component addition type thermal conductive adhesive according to the present invention, the pH adjusting agent is a weak acid, preferably glacial acetic acid or hydrochloric acid, and is used for adjusting the pH of the one-component addition type thermal conductive adhesive to 3 to 5.
As a preferred embodiment of the single-component addition type heat-conducting adhesive according to the present invention, the catalyst is a platinum catalyst, and the platinum content of the platinum catalyst is 500ppm to 5000ppm, preferably 2000 ppm; preferably, the platinum catalyst is bis (1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane) platinum.
As a preferred embodiment of the single-component addition type heat-conducting adhesive glue of the present invention, the inhibitor is an alkynol compound; the alkynol compound is alpha-alkynol with a boiling point higher than 200 ℃.
Preferably, the inhibitor is at least one of 1, 1-diphenyl-2-propyn-3-ol, 3-methyl-1-dodecyn-3-ol and 3,7, 11-trimethyldodecyn-3-ol.
In a second aspect, the invention provides a preparation method of the single-component addition type heat-conducting adhesive, which comprises the following steps:
(1) adding the heat-conducting filler into the vinyl silicone oil, and uniformly stirring; dripping the surface treating agent at 80-150 ℃, and uniformly stirring;
(2) cooling and then adding the tackifier; stirring evenly at 60-65 ℃; wherein the titanate coupling agent is added in one part;
(3) and cooling, adding the rest of the titanate coupling agent, hydrogen-containing polysiloxane, pH value regulator, catalyst and inhibitor, and uniformly stirring to obtain the catalyst.
The preparation method has the advantages of simple production process, no pollution, no byproduct generation, low cost and the like.
Preferably, the preparation method comprises the following steps:
(1) adding the heat-conducting filler into the vinyl silicone oil, and uniformly stirring; heating to 80-150 ℃, dropwise adding the silane with the boiling point higher than 210 ℃, and stirring for 10-30 min under the protection of inert gas; then, the silane with the boiling point lower than 160 ℃ is dripped, and the mixture is stirred for 10 to 30min under the protection of inert gas;
(2) cooling to room temperature, adding the compound of the structure R1Si(R2)3And 0.5-1.5 wt% of titanate coupling agent, heating to 60-65 ℃, and stirring in vacuum for 30-60 min to remove the bound water in the filler, eliminate the hydroxyl on the filler and synthesize to obtain a prepolymer;
(3) cooling to room temperature, adding the rest of titanate coupling agent, hydrogen-containing polysiloxane, pH regulator (regulating pH of the system to 3-5), catalyst and inhibitor, and vacuum stirring for 30-60 min.
And in the third aspect, the single-component addition type heat conduction adhesive is applied to the bonding and sealing of the electric control box body. Such as the bonding and sealing in the fields of electromagnetic ovens, microwave ovens, PTC ceramic heaters, other electric control boxes and the like.
Compared with the prior art, the invention has the beneficial effects that:
the single-component addition type heat-conducting adhesive provided by the invention has high stability, heat conductivity and adhesiveness. When a large amount of heat-conducting filler is added, the viscosity of the heat-conducting filler is slightly increased, and the heat-conducting filler has good filling, coating and sealing performances and is suitable for being used in a packaging form. In addition, the single-component addition type heat-conducting adhesive provided by the invention has higher tensile strength, elongation and bonding strength even if no reinforcing filler is used. The single-component addition type heat-conducting adhesive can be used for bonding and sealing in the fields of electromagnetic ovens, microwave ovens, PTC ceramic heaters, other electric control boxes and the like.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples. It will be understood by those skilled in the art that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The test methods used in the examples are all conventional methods unless otherwise specified; the materials, reagents and the like used are commercially available unless otherwise specified.
The following examples and comparative examples illustrate the raw materials but are not limited to these materials:
vinyl silicone oil:
a1: vinyl terminated polydimethylsiloxanes; viscosity is 500mPa · s; vinyl content 0.43 wt%;
a2: vinyl terminated polydimethylsiloxanes; viscosity 1000mPa · s; vinyl content 0.32 wt%;
a3: vinyl terminated polydimethylsiloxanes; viscosity is 5000mPa · s; the vinyl content was 0.16 wt%.
Heat-conducting filler:
b1: spherical alumina with an average particle size of 20 μm;
b2: spherical alumina with an average particle size of 5 μm;
b3: spheroidal alumina with an average particle size of 1 μm.
Surface treatment agent 1:
c1: dodecyl trimethoxy silane with a boiling point of 234.9 deg.C (760 mmHg);
c2: decaalkyltrimethoxysilane, boiling at 213.6 deg.C (760 mmHg).
Surface treatment agent 2:
d1: methyltrimethoxysilane having a boiling point of 102 ℃ (760 mmHg);
d2: ethyltrimethoxysilane, boiling point 124 ℃ (760 mmHg).
Tackifier 1:
e1: gamma- (2, 3-glycidoxy) propyltrimethoxysilane;
e2: vinyl trimethoxy silane.
Tackifier 2:
f1: ethyl titanate;
f2: titanium acid isopropyl ester.
pH value regulator:
g: glacial acetic acid.
Hydrogen-containing polysiloxane:
h1: hydrogen-containing silicone oil with viscosity of 80mPa s; hydrogen content is 0.75 wt%;
h2: hydrogen-containing silicone oil with viscosity of 100mPa s; hydrogen content is 0.29 wt%;
h3: hydrogen-terminated silicone oil with the viscosity of 50mPa & s; the hydrogen content was 0.07 wt%.
Catalyst:
i: bis (1, 3-divinyl-1, 1,3, 3-tetramethyldisiloxane) platinum, the platinum content being 2000 ppm.
Inhibitor (B):
j: 3-methyl-1-dodecyn-3-ol with a boiling point of 229 ℃ (760 mmHg).
The compositions of the one-component addition type thermally conductive adhesive pastes of examples 1 to 4 and comparative examples 1 to 8 are shown in table 1.
The preparation method of the single-component addition type heat-conducting adhesive of examples 1 to 4 and comparative examples 1 to 8 is as follows:
(1) firstly, adding vinyl silicone oil into a planetary stirrer, then adding heat-conducting filler in batches, and uniformly stirring; heating to 80-150 ℃, then dripping the surface treating agent 1, and filling nitrogen to protect and stir for 10-30 min; dripping the surface treating agent 2, charging nitrogen gas for protection, vacuumizing and stirring for 10-30 min.
(2) Cooling to room temperature, adding tackifier 1 and part of tackifier 2, wherein the tackifier 2 added in the step accounts for 1 wt% of the total tackifier 2, heating to 60-65 ℃, vacuumizing and stirring for 30-60 min, removing bound water in the filler, eliminating hydroxyl on the filler and synthesizing to obtain a prepolymer;
(3) cooling to room temperature, adding the rest tackifier 2, hydrogen-containing polysiloxane, pH regulator (regulating system pH to about 4), catalyst and inhibitor, and stirring under vacuum for 30 min.
TABLE 1 Components (parts by weight) of examples and comparative examples
The one-component addition type thermally conductive adhesive pastes of examples and comparative examples were tested for their relevant properties, and the results are shown in table 2. The performance detection method comprises the following steps:
(1) coefficient of thermal conductivity
The samples were tested for thermal conductivity according to ASTM-D5470.
(2) Viscosity of the oil
The samples were tested for viscosity according to GB/T2794-2013.
(3) Tensile strength
The samples were tested for tensile strength according to GB/T528-2009.
(4) Elongation at break
The samples were tested for elongation at break according to GB/T528-2009.
(5) Tensile shear strength
The tensile shear strength of the samples was tested according to GB/T7124-.
(6) Hardness of
The hardness of the samples was tested according to GB/T531.1-2008.
Table 2 table comparing test results of examples and comparative examples
As can be seen from the comparison of the examples and comparative examples in Table 2, the one-component addition type thermally conductive adhesive compositions of examples 1 to 5 are excellent in thermal conductivity, viscosity, tensile strength, elongation at break, tensile shear strength, and the like. Example 5 compared to example 1, the viscosity increase was small when a large amount of thermally conductive filler was added.
Compared with the example 1, the single-component addition type heat-conducting adhesive of the comparative example 5 only contains the surface treatment agent 1 dodecyl trimethoxy silane, does not contain the surface treatment agent 2, and has higher viscosity, lower tensile strength and lower elongation at break; in the one-component addition type thermally conductive adhesive paste of comparative example 1, even though dodecyltrimethoxysilane was contained in an amount equal to the sum of the parts by weight of the surface treatment agent 1 and the parts by weight of the surface treatment agent 2 in example 1, the viscosity of the prepared product was high and the tensile strength and elongation at break were low without the surface treatment agent 2.
Compared with the example 1, the single-component addition type heat-conducting adhesive of the comparative example 6 only contains the surface treatment agent of methyltrimethoxysilane, and does not contain the surface treatment agent 1, so that the prepared product has higher viscosity and lower tensile strength and elongation at break; in the one-component addition type thermally conductive adhesive paste of comparative example 2, even though methyltrimethoxysilane was contained in an amount equal to the sum of the parts by weight of surface treatment agent 1 and surface treatment agent 2 in example 1, the viscosity of the prepared product was high and the tensile strength and elongation at break were low without surface treatment agent 1.
Compared with the example 1, in the single-component addition type heat-conducting adhesive of the comparative example 7, only the tackifier 1 methyltrimethoxysilane is contained, and the tackifier 2 is not contained, so that the tensile shear strength of the prepared product is lower; in the one-component addition type thermally conductive adhesive paste of comparative example 3, even though methyltrimethoxysilane was included in an amount equal to the sum of the parts by weight of the tackifier 1 and the tackifier 2 of example 1, the tensile shear strength of the prepared product was low without the tackifier 2.
Compared with the example 1, in the single-component addition type heat-conducting adhesive of the comparative example 8, only the tackifier 2 ethyl titanate is contained, and the tackifier 1 is not contained, so that the tensile shear strength of the prepared product is lower; in the one-component addition type thermally conductive adhesive of comparative example 4, even though the same amount of ethyl titanate as that of the sum of the parts by weight of tackifier 1 and tackifier 2 of example 1 was contained, no tackifier 1 was present, and the tensile shear strength of the prepared product was low.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (15)
1. The single-component addition type heat-conducting adhesive is characterized by comprising the following components in parts by weight:
20-150 parts of vinyl silicone oil, 10-750 parts of heat-conducting filler, 0.5-10 parts of surface treating agent, 0.1-2 parts of tackifier, 0.01-0.5 part of pH value regulator, 0.1-10 parts of hydrogen-containing polysiloxane, 0.1-1 part of catalyst and 0.1-1 part of inhibitor;
the surface treatment agent comprises silane with a boiling point higher than 210 ℃ and silane with a boiling point lower than 160 ℃;
the adhesion promoter includes a titanate coupling agent.
2. The single-component addition type heat-conducting adhesive according to claim 1, wherein the silane with the boiling point higher than 210 ℃ has the structure shown in formula (I) or formula (II);
wherein n is more than or equal to 6, R is alkyl with more than 6 carbons, and X, Y, Z is a hydrolyzable group.
3. The one-component addition-type thermally conductive adhesive according to claim 1, wherein the silane having a boiling point of less than 160 ℃ is at least one of vinyltrimethoxysilane, methyltrimethoxysilane, ethyltrimethoxysilane, propyltrimethoxysilane, and methyltriethoxysilane.
4. The one-component addition-type heat-conductive adhesive according to claim 1, wherein the mass of the silane with the boiling point higher than 210 ℃ or the silane with the boiling point lower than 160 ℃ is 0.01-1% of the mass of the heat-conductive filler.
5. The single component addition type thermal conductive adhesive according to claim 1, wherein the titanate coupling agent is at least one of ethyl titanate, butyl titanate, isopropyl titanate, tetra-t-butyl titanate, tetra-t-amyl titanate, and a chelate of titanate.
6. The one-component addition-type thermally conductive adhesive of claim 1, wherein the tackifier further comprises the structure R1Si(R2)3A compound of (1);
wherein, R is1Is at least one of methoxy, epoxypropyl, vinyl and acetoxymethyl or alkyl substituted by the group; r2Is at least one group of methoxyl, ethoxyl and propoxyl.
7. The one-component addition-type thermally conductive adhesive according to any one of claims 1 to 6, wherein the vinyl silicone oil is at least one of a silicone oil containing terminal vinyl groups or side vinyl groups; the viscosity of the vinyl silicone oil is 500-5000 mPa.s, and the content of vinyl is 0.1-1%.
8. The one-component addition-type thermally conductive adhesive according to any one of claims 1 to 6, wherein the hydrogen-containing polysiloxane is at least one of terminal hydrogen-containing silicone oil or lateral hydrogen-containing silicone oil; the hydrogen-containing polysiloxane has the viscosity of 10-500 mPa.s and the hydrogen content of 0.01-1.6%.
9. The one-component addition-type heat-conducting adhesive according to any one of claims 1 to 6, wherein the heat-conducting filler is at least one of silver powder, aluminum powder, copper powder, nickel powder, carbon powder, aluminum oxide, zinc oxide, magnesium oxide, titanium oxide, boron nitride, aluminum nitride, carbon fiber, boron carbide, silicon carbide, graphene, diamond and silicon micropowder.
10. The one-component addition-type thermally conductive adhesive paste according to any one of claims 1 to 6, wherein the pH of the one-component addition-type thermally conductive adhesive paste is 3 to 5.
11. The one-component addition-type thermally conductive adhesive according to any one of claims 1 to 6, wherein the catalyst is a platinum catalyst, and the platinum content of the platinum catalyst is 500ppm to 5000 ppm.
12. The one-component addition-type thermally conductive adhesive according to any one of claims 1 to 6, wherein the inhibitor is an alkynol compound; the alkynol compound is alpha-alkynol with a boiling point higher than 200 ℃.
13. The one-part addition-type thermally conductive adhesive according to claim 12, wherein the inhibitor is at least one of 1, 1-diphenyl-2-propyn-3-ol, 3-methyl-1-dodecyn-3-ol, and 3,7, 11-trimethyldodecyn-3-ol.
14. The method for preparing the one-component addition type thermal adhesive according to any one of claims 1 to 13, comprising the steps of:
(1) adding the heat-conducting filler into the vinyl silicone oil, and uniformly stirring; dripping the surface treating agent at 80-150 ℃, and uniformly stirring;
(2) cooling and then adding the tackifier; stirring evenly at 60-65 ℃; wherein the titanate coupling agent is added in one part;
(3) and cooling, adding the rest of the titanate coupling agent, hydrogen-containing polysiloxane, pH value regulator, catalyst and inhibitor, and uniformly stirring to obtain the catalyst.
15. Use of a one-component addition-type thermally conductive adhesive according to any one of claims 1 to 13 for adhesively sealing an electrical cabinet.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115505368A (en) * | 2022-10-10 | 2022-12-23 | 杭州之江新材料有限公司 | Single-component dealcoholized organosilicon sealant and preparation method thereof |
| CN115612446A (en) * | 2022-10-27 | 2023-01-17 | 江西蓝星星火有机硅有限公司 | Heat-conducting addition type organic silicon composition for encapsulation |
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| CN111051433A (en) * | 2017-07-24 | 2020-04-21 | 陶氏东丽株式会社 | Thermally conductive silicone gel composition, thermally conductive member, and heat dissipation structure |
| CN113801626A (en) * | 2021-09-24 | 2021-12-17 | 广州集泰化工股份有限公司 | Single-component addition type adhesive and preparation method thereof |
| CN113881250A (en) * | 2021-10-20 | 2022-01-04 | 广州集泰化工股份有限公司 | Heat-conducting filler and surface treatment method thereof |
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| CN111051433A (en) * | 2017-07-24 | 2020-04-21 | 陶氏东丽株式会社 | Thermally conductive silicone gel composition, thermally conductive member, and heat dissipation structure |
| CN113801626A (en) * | 2021-09-24 | 2021-12-17 | 广州集泰化工股份有限公司 | Single-component addition type adhesive and preparation method thereof |
| CN113881250A (en) * | 2021-10-20 | 2022-01-04 | 广州集泰化工股份有限公司 | Heat-conducting filler and surface treatment method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115505368A (en) * | 2022-10-10 | 2022-12-23 | 杭州之江新材料有限公司 | Single-component dealcoholized organosilicon sealant and preparation method thereof |
| CN115505368B (en) * | 2022-10-10 | 2023-11-28 | 杭州之江新材料有限公司 | Single-component dealcoholized organosilicon sealant and preparation method thereof |
| CN115612446A (en) * | 2022-10-27 | 2023-01-17 | 江西蓝星星火有机硅有限公司 | Heat-conducting addition type organic silicon composition for encapsulation |
| CN115612446B (en) * | 2022-10-27 | 2024-01-26 | 江西蓝星星火有机硅有限公司 | Heat-conducting addition type organic silicon composition for encapsulation |
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