CN114907804A - High-temperature-resistant high-thermal-conductivity high-reflection flame-retardant structural adhesive and application thereof - Google Patents
High-temperature-resistant high-thermal-conductivity high-reflection flame-retardant structural adhesive and application thereof Download PDFInfo
- Publication number
- CN114907804A CN114907804A CN202210753747.9A CN202210753747A CN114907804A CN 114907804 A CN114907804 A CN 114907804A CN 202210753747 A CN202210753747 A CN 202210753747A CN 114907804 A CN114907804 A CN 114907804A
- Authority
- CN
- China
- Prior art keywords
- parts
- flame
- retardant
- structural adhesive
- epoxy resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003063 flame retardant Substances 0.000 title claims abstract description 92
- 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 title claims abstract description 88
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 75
- 239000000853 adhesive Substances 0.000 title claims abstract description 74
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 57
- 239000000945 filler Substances 0.000 claims abstract description 36
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 32
- 239000011521 glass Substances 0.000 claims abstract description 28
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 28
- 239000000440 bentonite Substances 0.000 claims abstract description 25
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 25
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 25
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000011889 copper foil Substances 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 18
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920005989 resin Polymers 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 13
- -1 boron trifluoride amine Chemical class 0.000 claims abstract description 12
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims abstract description 10
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 229910015900 BF3 Inorganic materials 0.000 claims abstract description 8
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Substances FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229920002857 polybutadiene Polymers 0.000 claims abstract description 8
- 239000005062 Polybutadiene Substances 0.000 claims abstract description 6
- 239000003822 epoxy resin Substances 0.000 claims description 76
- 229920000647 polyepoxide Polymers 0.000 claims description 76
- 239000000843 powder Substances 0.000 claims description 68
- 125000002723 alicyclic group Chemical group 0.000 claims description 66
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 claims description 42
- 239000002994 raw material Substances 0.000 claims description 40
- 239000003795 chemical substances by application Substances 0.000 claims description 26
- 239000002518 antifoaming agent Substances 0.000 claims description 24
- 239000002270 dispersing agent Substances 0.000 claims description 24
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 23
- YRZFHTRSHNGOSR-UHFFFAOYSA-N phenylmethanamine;trifluoroborane Chemical compound FB(F)F.NCC1=CC=CC=C1 YRZFHTRSHNGOSR-UHFFFAOYSA-N 0.000 claims description 23
- 229910003460 diamond Inorganic materials 0.000 claims description 22
- 239000010432 diamond Substances 0.000 claims description 22
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 claims description 21
- 239000011353 cycloaliphatic epoxy resin Substances 0.000 claims description 14
- 239000003292 glue Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- LTVUCOSIZFEASK-MPXCPUAZSA-N (3ar,4s,7r,7as)-3a-methyl-3a,4,7,7a-tetrahydro-4,7-methano-2-benzofuran-1,3-dione Chemical compound C([C@H]1C=C2)[C@H]2[C@H]2[C@]1(C)C(=O)OC2=O LTVUCOSIZFEASK-MPXCPUAZSA-N 0.000 claims description 3
- WIOWSZFVJSZSCX-UHFFFAOYSA-N 2,4-dimethylaniline;trifluoroborane Chemical compound FB(F)F.CC1=CC=C(N)C(C)=C1 WIOWSZFVJSZSCX-UHFFFAOYSA-N 0.000 claims description 3
- MWSKJDNQKGCKPA-UHFFFAOYSA-N 6-methyl-3a,4,5,7a-tetrahydro-2-benzofuran-1,3-dione Chemical compound C1CC(C)=CC2C(=O)OC(=O)C12 MWSKJDNQKGCKPA-UHFFFAOYSA-N 0.000 claims description 3
- OXQXGKNECHBVMO-UHFFFAOYSA-N 7-oxabicyclo[4.1.0]heptane-4-carboxylic acid Chemical compound C1C(C(=O)O)CCC2OC21 OXQXGKNECHBVMO-UHFFFAOYSA-N 0.000 claims description 3
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 230000018044 dehydration Effects 0.000 claims description 3
- 238000006297 dehydration reaction Methods 0.000 claims description 3
- 238000004383 yellowing Methods 0.000 abstract description 7
- 239000004593 Epoxy Substances 0.000 abstract 1
- NZNMSOFKMUBTKW-UHFFFAOYSA-N cyclohexanecarboxylic acid Chemical compound OC(=O)C1CCCCC1 NZNMSOFKMUBTKW-UHFFFAOYSA-N 0.000 abstract 1
- 239000007822 coupling agent Substances 0.000 description 19
- 238000002310 reflectometry Methods 0.000 description 17
- 238000012360 testing method Methods 0.000 description 17
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 15
- 238000001723 curing Methods 0.000 description 13
- 239000004744 fabric Substances 0.000 description 13
- 239000003365 glass fiber Substances 0.000 description 11
- 239000007788 liquid Substances 0.000 description 10
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 9
- 238000007761 roller coating Methods 0.000 description 9
- 238000007650 screen-printing Methods 0.000 description 9
- 238000003618 dip coating Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000012074 organic phase Substances 0.000 description 5
- 238000010998 test method Methods 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 238000005476 soldering Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000002161 passivation Methods 0.000 description 3
- 238000011056 performance test Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- DCQBZYNUSLHVJC-UHFFFAOYSA-N 3-triethoxysilylpropane-1-thiol Chemical compound CCO[Si](OCC)(OCC)CCCS DCQBZYNUSLHVJC-UHFFFAOYSA-N 0.000 description 2
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- KSZDKSNRUYOJHR-UHFFFAOYSA-M dodecyl(trimethyl)azanium;hydrogen sulfate Chemical compound OS([O-])(=O)=O.CCCCCCCCCCCC[N+](C)(C)C KSZDKSNRUYOJHR-UHFFFAOYSA-M 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 230000017525 heat dissipation Effects 0.000 description 2
- 238000007731 hot pressing Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 238000002390 rotary evaporation Methods 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 1
- UUEWCQRISZBELL-UHFFFAOYSA-N 3-trimethoxysilylpropane-1-thiol Chemical compound CO[Si](OC)(OC)CCCS UUEWCQRISZBELL-UHFFFAOYSA-N 0.000 description 1
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- FZOIBNKTZLVZPG-UHFFFAOYSA-N C=O.C1CCCC=C1 Chemical compound C=O.C1CCCC=C1 FZOIBNKTZLVZPG-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- VDRSDNINOSAWIV-UHFFFAOYSA-N [F].[Si] Chemical compound [F].[Si] VDRSDNINOSAWIV-UHFFFAOYSA-N 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 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
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000007323 disproportionation reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000006735 epoxidation reaction Methods 0.000 description 1
- 229920006335 epoxy glue Polymers 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012757 flame retardant agent Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical group 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
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- 230000001590 oxidative effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000007719 peel strength test Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
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- 239000004014 plasticizer Substances 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
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- 230000001105 regulatory effect Effects 0.000 description 1
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- 238000011160 research Methods 0.000 description 1
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- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
- B32B15/017—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of aluminium or an aluminium alloy, another layer being formed of an alloy based on a non ferrous metal other than aluminium
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/20—Layered products comprising a layer of metal comprising aluminium or copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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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
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4223—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof aromatic
-
- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices with at least one potential-jump barrier or surface barrier specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/62—Arrangements for conducting electric current to or from the semiconductor body, e.g. lead-frames, wire-bonds or solder balls
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- 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
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- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- 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
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- C08K2201/011—Nanostructured additives
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- 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
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K3/22—Oxides; Hydroxides of metals
- C08K3/2279—Oxides; Hydroxides of metals of antimony
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
-
- 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
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L2933/00—Details relating to devices covered by the group H01L33/00 but not provided for in its subgroups
- H01L2933/0008—Processes
- H01L2933/0033—Processes relating to semiconductor body packages
- H01L2933/0066—Processes relating to semiconductor body packages relating to arrangements for conducting electric current to or from the semiconductor body
Abstract
The invention discloses a high-temperature-resistant high-heat-conduction high-reflection flame-retardant structural adhesive and application thereof, wherein the high-temperature-resistant high-heat-conduction high-reflection flame-retardant structural adhesive is prepared by mixing 3, 4-epoxy group cyclohexane carboxylic acid-3 ', 4' -epoxy group cyclohexane methyl ester and epoxy polybutadiene resin with silicon rubber, and adding heat-conducting filler, flame retardant, titanium dioxide, organic bentonite, phthalic anhydride, boron trifluoride amine complex accelerator and some auxiliaries. The flame-retardant structural adhesive can be used for glass-based miniLED substrates, aluminum substrates and PCB boards, can firmly adhere copper foils and glass, copper foils and aluminum plates and PCB boards, and has the advantages of high heat conductivity and emissivity, good flame retardance, high-temperature yellowing resistance, adjustable viscosity and wide applicability.
Description
Technical Field
The invention relates to the field of electronic structure adhesives, in particular to a high-temperature-resistant high-heat-conduction high-reflection flame-retardant structural adhesive.
Background
The structural adhesive is widely applied in the electronic field, can be used for adhering glass, copper foil, metal and copper foil, and then etching a required circuit on the copper for manufacturing a circuit board of a glass substrate or an aluminum substrate.
The existing structural adhesives are usually cured by bisphenol a epoxy resins and amines, and have the following problems: the paint contains a large number of benzene ring double bonds and chlorides, has poor aging resistance and high temperature resistance, is seriously yellowed after contacting with air for 10 minutes at the temperature of more than 200 ℃, has low adhesive force and is inflammable, and cannot meet the application requirements of the display field of high-end electronic industry; the epoxy resin and the amine have quick curing reaction and short operable time; high viscosity, the need for diluent, a great loss in production efficiency and environmental pollution.
In addition, the conventional structural adhesive has low thermal conductivity, poor heat dissipation in the use process and low reflectivity, and has great defects when applied to the display field.
Therefore, the research on the high-temperature-resistant high-thermal-conductivity high-reflection structural adhesive which can be used in the display field is of great significance.
Disclosure of Invention
Based on the problems in the prior art, the invention provides the flame-retardant structural adhesive, and the structural adhesive has excellent high-temperature resistance, high heat conduction and high reflection performance by regulating and controlling a formula system, so that the structural adhesive can be applied to the display field of high-end electronic industries such as miniLEDs, PCB boards and the like.
The invention adopts the following technical scheme for realizing the purpose:
the utility model provides a fire-retardant structure of high temperature resistant high heat conduction high reflection glues which characterized in that: the structural adhesive is composed of a component A and a component B:
the component A comprises the following raw materials in parts by mass:
10-30 parts of alicyclic epoxy resin,
10-30 parts of a second alicyclic epoxy resin,
5-10 parts of silicon rubber,
20-40 parts of heat-conducting filler,
10-20 parts of a flame retardant agent,
8-16 parts of titanium dioxide powder,
0.1 to 1 portion of flatting agent,
0.1 to 0.3 portion of defoaming agent,
2-10 parts of a silane coupling agent,
1-3 parts of a dispersing agent,
1-3 parts of organic bentonite;
the component B comprises the following raw materials in parts by mass:
99.5 to 99.9 portions of phthalic anhydride,
0.1-0.5 part of boron trifluoride amine complex accelerator;
the cycloaliphatic epoxy resin I is 3, 4-epoxy cyclohexane carboxylic acid-3 ', 4' -epoxy cyclohexane methyl ester, and the cycloaliphatic epoxy resin II is epoxidized polybutadiene resin.
Further, the heat conducting filler is composed of diamond and modified spherical alumina according to the mass ratio of 1-1.5: 1. The spherical alumina treated by the coupling agent can improve the wettability of resin to powder and improve the anti-settling property. The heat-conducting filler commonly used in the existing adhesive has the influence on the adhesive force when the addition amount is small and the heat conductivity is low and the addition amount is large. Therefore, the powder diamond and the modified spherical alumina are matched with the rutile type titanium dioxide filler, the synergistic effect can be achieved, the high thermal conductivity of 2W/(m.K) can be achieved, the high reflectivity can also be achieved, the bonding force is not seriously reduced and can reach 2kg/25mm under the condition of proper addition amount, and the pain points of poor thermal conductivity and low reflectivity of the adhesive in the high-end field are solved.
Further, the flame retardant comprises aluminum hydroxide and nano antimony trioxide in a mass ratio of 1.5-2.5: 1. The commonly used flame retardant in the existing binder is halogen-containing resin, particularly bromine-containing resin, the color of the flame retardant is yellow, the yellowing is more serious after high temperature, and phosphorus-containing resin and a plasticizer can volatilize at 290 ℃. The invention uses titanium dioxide with certain flame retardance, modified spherical alumina, flame retardant aluminum hydroxide which resists high temperature and does not change color and nano antimony trioxide to compound to generate synergistic action. Meanwhile, the silicon rubber resin generates silicon dioxide after being burnt, and is non-combustible. The invention utilizes silicon rubber to toughen and improve flame retardance, and the silicon rubber is matched with heat-conducting powder and a flame retardant to achieve the effects of high heat conduction, high reflection and flame retardance.
Further, the phthalic anhydride is at least one of methyl tetrahydrophthalic anhydride MeTHPA, methyl hexahydrophthalic anhydride MeHHPA and methyl nadic anhydride MNA.
Further, the boron trifluoride amine complex accelerator is at least one of boron trifluoride-benzylamine complex and boron trifluoride-2, 4-dimethylaniline complex.
The preparation method of the flame-retardant structural adhesive comprises the following steps:
under the stirring state, firstly mixing the alicyclic epoxy resin I and the alicyclic epoxy resin II, heating at 80 ℃ until the alicyclic epoxy resin I and the alicyclic epoxy resin II are dissolved, then adding the silicon rubber, heating at 120 ℃ for dehydration condensation for 2 hours, then adding the silane coupling agent, the dispersing agent, the organic bentonite, the flatting agent, the antifoaming agent, the titanium dioxide, the heat-conducting filler and the flame retardant, stirring uniformly, and filtering to obtain a component A;
mixing phthalic anhydride and boron trifluoride amine complex, heating at 80 ℃ to dissolve, and filtering to obtain a component B;
when in use, the component A and the component B are mixed according to the mass ratio of 1: 0.3, mixing uniformly to obtain the flame-retardant structural adhesive with high temperature resistance, high heat conductivity and high reflection.
The flame-retardant structural adhesive can be used for bonding a copper foil and a glass substrate, a copper foil and an aluminum substrate or used as an adhesive of a PCB (printed circuit board).
Based on the flame-retardant structural adhesive, the invention also provides a glass-based miniLED substrate, and the glass and the copper foil of the glass-based miniLED substrate are bonded through the flame-retardant structural adhesive.
The invention has the beneficial effects that:
1. in the formulation system of the present invention: the cycloaliphatic epoxy resin I and the cycloaliphatic epoxy resin II are obtained by oxidizing and modifying butadiene resin, both contain epoxy groups, and after the epoxy groups are crosslinked with phthalic anhydride curing agents, the prepared polymer does not contain yellowing groups and does not yellow after being heated for 10 minutes at 290 ℃. Because the flexible structure of the silicon rubber is incombustible, after the silicon rubber is introduced into a molecular structure, the high-Tg-point high-temperature-resistant resin is formed, so that the polymer has the strong rigid structure of the epoxy resin and the toughness and incombustibility of the silicon rubber, the impact resistance after construction is improved, and the heat resistance and the flame retardant property of the epoxy resin are improved. Meanwhile, the titanium dioxide and the heat-conducting filler have an interaction reinforcing effect and a flame-retardant effect, and the heat-conducting performance and the reflection performance of the system are improved to a great extent by matching with aluminum hydroxide and nano antimony trioxide, so that the system has flame retardance. The structural adhesive solves the problem of serious yellowing of the existing adhesive due to high-temperature heating, and solves the problems of poor bonding performance after a large amount of heat-conducting reflective filler is added or low heat conductivity and reflectivity due to the fact that the heat-conducting reflective filler is added.
2. The structural adhesive has good adhesion to copper, glass, copper and aluminum plates, has thermal conductivity of 2W/(m.K), has reflectivity higher than 80%, and does not yellow after reflow soldering for 10 minutes at 290 ℃.
3. The solid content of the structural adhesive reaches more than 99 percent, and almost no VOC is discharged.
4. The structural adhesive A, B has long service life after being mixed and can be used within 24 hours.
5. The structural adhesive has adjustable viscosity, is suitable for different construction processes such as roller coating, screen printing and the like, and has wide applicability. The adhesive can be made into low viscosity, the glass fiber cloth is immersed in the adhesive in a dip-coating mode, the glass fiber cloth is cured for 10 minutes at 100 ℃ and is in a solid state but not completely cured state, then the impregnated glass fiber cloth can be placed among a glass substrate, an aluminum substrate and a copper foil or replace the structural adhesive used by the existing PCB when the adhesion is needed, and then the adhesion effect can be achieved by hot pressing at 180 ℃ for 10 minutes, so that the tensile strength after copper cladding can be improved. Or the adhesive can be made into a low-viscosity copper foil, a glass substrate and an aluminum substrate which are constructed and bonded in a roller coating mode, glue is transferred to the glass and the aluminum plate by a roller, the copper foil is covered on the glass and the aluminum plate, the vacuumizing and the bubble removing are carried out, and the adhesive can be cured after being baked for 10 minutes at 180 ℃ to generate excellent bonding. The adhesive can also be constructed by adjusting higher viscosity through a screen printing mode, is printed on glass and an aluminum plate, is covered with copper foil, is vacuumized, removes bubbles, and can be cured after being baked for 10 minutes at 180 ℃ to generate excellent adhesion.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
The reagents and instruments used in the following examples are commercially available.
In the following examples:
the silicone rubber can be selected from 107 silicone rubbers with a hydroxyl terminated viscosity of 5000cps of Shenzhen Jipeng silicon fluorine materials Limited.
The heat-conducting filler is 3000-mesh powder diamond W5 of original super-hard abrasive grinding tool Limited and modified spherical alumina BED-011 of Suzhou Belde new material science and technology Limited.
The flame retardant is selected from aluminum hydroxide of Asahi New Material Co., Ltd, and nanometer antimony trioxide of Asahi New Material Co., Ltd.
The phthalic anhydride is at least one of methyl tetrahydrophthalic anhydride MeTHPA (Zhejiang Shuima Fine chemical Co., Ltd.), methyl hexahydrophthalic anhydride MeHHPA (Jiaxing Ninghuan chemical New Material Co., Ltd.) and methyl nadic anhydride MNA (Jingjiang Yongtaifeng chemical Co., Ltd.).
The titanium dioxide is selected from DuPont R-902 +.
The leveling agent is at least one selected from Digao 450 and ByK-333.
The defoaming agent is at least one selected from ByK-066N, BYK-057 and BYK-368N.
The silane coupling agent is at least one selected from KH-550 (3-aminopropyltriethoxysilane), KH-560 (3-glycidoxypropyltrimethoxysilane), KH-570 (gamma- (methacryloyloxy) propyltrimethoxysilane), KH-580 (3-mercaptopropyltrimethoxysilane), and KH-590 (3-mercaptopropyltriethoxysilane).
The dispersant is at least one selected from deep bamboo SN-2011, SN-2311 and SN-2041A.
The organic bentonite is at least one selected from Haimines SD-2 and Claiminton 62.
The boron trifluoride-amine complex accelerator is selected from boron trifluoride-benzylamine complex (Chuzhou Huishen materials company H600), boron trifluoride-2, 4-dimethylaniline complex (Chuzhou Huishen materials company H602)
The alicyclic epoxy resin I is prepared by synthesizing cyclohexene formaldehyde from butadiene and acrolein through heating and pressurizing reaction, and then performing disproportionation esterification and epoxidation reaction, and the synthesis steps are as follows: 2.18g H were put into a 1000mL beaker in this order 3 PO 4 、1.48g NaH 2 PO 4 ·2H 2 O、12.0gNa 2 WO 4 ·2H 2 O、360mL H 2 O 2 (35%) and stirred at room temperature for 10min, and after complete dissolution, transferred to a constant pressure dropping funnel. 200.0g of 3, 4-cyclohexenylformic acid-3 ', 4' -cyclohexenylmethyl ester, 680mL of toluene and 9.10g of dodecyl trimethyl ammonium hydrogen sulfate are sequentially put into a 2000mL three-neck flask, the stirring rate is 1200 r/min, the temperature is raised to 90 ℃, the mixed liquid in a dropping funnel begins to be dropped for 2h, and the reaction continues for 3h after the dropping is finished. After the reaction, the mixture is transferred to 2L of liquid separation and leakage, an organic phase is separated out, 200mL of water is used for washing for 15min, the organic phase is separated out, rotary evaporation and desolventization (6mmHg, 50 ℃) are carried out, a mechanical pump is used for carrying out reduced pressure distillation at the temperature of 175 ℃ and 185 ℃ to obtain about 182g of colorless liquid, namely 3, 4-epoxy cyclohexane carboxylic acid-3 ', 4' -epoxy cyclohexane methyl ester, which is marked as alicyclic epoxy resin I.
The alicyclic epoxy resin II is obtained by epoxidizing double bonds in 3000-5000 relative molecular mass liquid polybutadiene resin molecules, and the synthesis steps are as follows: 300.0g of low-average relative molecular mass liquid polybutadiene resin, 860mL of toluene and 10.90g of dodecyl trimethyl ammonium hydrogen sulfate are sequentially put into a 2000mL three-neck flask, the stirring speed is 1200 r/min, the temperature is raised to 100 ℃, and 2.18g H is started to be dripped 3 PO 4 、1.48g NaH 2 PO 4 ·2H 2 O、12.0g Na 2 WO 4 ·2H 2 O、360mLH 2 O 2 (35%) the mixed liquid is dripped for 2h, and the reaction is continued for 3h after dripping. After the reaction is finished, transferring the mixture to 2L of liquid separation and leakage, separating an organic phase, washing the organic phase with 300mL of water for 20min, separating the organic phase, performing rotary evaporation and desolventizing (6mmHg, 50 ℃), performing reduced pressure distillation at the temperature of 185 ℃ by a mechanical pump to obtain 272g of colorless liquid, filling the alicyclic resin into a 500mL beaker, and cooling to obtain solid alicyclic epoxy resin epoxidized polybutadiene resin, which is marked as alicyclic epoxy resin II. The epoxy group, the hydroxyl group and the ester group side chain in the molecular structure are linear macromolecules, and the polybutadiene rubber structure and the epoxy resin structure are simultaneously adopted, so that the high-strength high-toughness high-strength epoxy resin has good impact toughness and adhesive property, is small in viscosity after being mixed and dissolved with a curing agent, convenient to operate and good in manufacturability, and a cured product has good heat resistance, the heat deformation temperature can reach more than 200 ℃, and has a very outstanding strength retention rate at high temperature.
The preparation method of the flame-retardant structural adhesive of the following embodiment is as follows:
in a three-neck flask, firstly, mixing the alicyclic epoxy resin I and the alicyclic epoxy resin II, heating the mixture to the temperature of 80 ℃ until the alicyclic epoxy resin I and the alicyclic epoxy resin II are dissolved (stirring at a high speed in the process), then adding the silicon rubber, heating the mixture at the temperature of 120 ℃ for dehydration condensation for 2 hours (stirring at a high speed in the process), and obtaining transparent liquid. And (3) filling the obtained transparent liquid into a corrosion-resistant tank, placing the tank below a dispersion machine, rotating the dispersion machine at the speed of 1000 r/min, and then adding a silane coupling agent, a dispersing agent, organic bentonite, a leveling agent, a defoaming agent, titanium dioxide, a heat-conducting filler and a flame retardant. After the feeding is finished, the rotating speed of the dispersion machine is increased to 2000 r/min, the dispersion is carried out for 30 min, and then the component A is obtained by filtering through 100-mesh filter cloth.
Phthalic anhydride and boron trifluoride amine complex were mixed and heated to dissolution at 80 ℃ and filtered through 200 mesh filter cloth to obtain component B.
When in use, the component A and the component B are mixed according to the mass ratio of 1: 0.3, and evenly mixing to obtain the flame-retardant structural adhesive with high temperature resistance, high heat conduction and high reflection.
Example 1
The embodiment provides a flame-retardant structural adhesive suitable for manufacturing a prepreg by dip-coating glass fiber cloth, which comprises the following formula:
the component A comprises the following raw materials in parts by mass:
30 parts of alicyclic epoxy resin, namely 30 parts of alicyclic epoxy resin,
two 10 parts of alicyclic epoxy resin and 10 parts of epoxy resin,
5 parts of hydroxyl-terminated silicon rubber,
22 parts of heat-conducting filler (11 parts of powdered diamond and 11 parts of modified spherical alumina powder),
16 parts of fire retardant (11 parts of aluminum hydroxide powder and 5 parts of nano antimony trioxide powder),
11 parts of R-902+ titanium dioxide powder,
0.3 part of BYK-333 leveling agent,
0.1 part of BYK-057 defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite.
The component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 2
The embodiment provides a flame-retardant structural adhesive with high thermal conductivity, which is suitable for manufacturing a prepreg by dip-coating glass fiber cloth, and the formula of the flame-retardant structural adhesive is as follows:
the component A comprises the following raw materials in parts by mass:
30 parts of alicyclic epoxy resin, namely, 30 parts of alicyclic epoxy resin,
two 10 parts of alicyclic epoxy resin and 10 parts of epoxy resin,
5 parts of hydroxyl-terminated silicon rubber,
25 parts of heat-conducting filler (14 parts of powdered diamond, 11 parts of modified spherical alumina powder),
15 parts of flame retardant (10 parts of aluminum hydroxide powder and 5 parts of nano antimony trioxide powder),
9 parts of R-902+ titanium dioxide powder,
0.3 part of BYK-333 leveling agent,
0.1 part of BYK-057 defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite.
The component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 3
The embodiment provides a high-reflectivity flame-retardant structural adhesive suitable for dip-coating glass fiber cloth to manufacture a prepreg, and the formula of the high-reflectivity flame-retardant structural adhesive is as follows:
the component A comprises the following raw materials in parts by mass:
30 parts of alicyclic epoxy resin, namely 30 parts of alicyclic epoxy resin,
10 parts of two alicyclic epoxy resins, namely alicyclic epoxy resin,
5 parts of hydroxyl-terminated silicon rubber,
20 parts of heat-conducting filler (10 parts of powdered diamond and 10 parts of modified spherical alumina powder),
15 parts of flame retardant (10 parts of aluminum hydroxide powder and 5 parts of nano antimony trioxide powder),
14 parts of R-902+ titanium dioxide powder,
0.3 part of BYK-333 leveling agent,
0.1 part of BYK-057 defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite.
The component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 4
The embodiment provides a flame-retardant structural adhesive with a good flame-retardant effect, which is suitable for dip-coating glass fiber cloth to manufacture a prepreg, and the formula of the flame-retardant structural adhesive is as follows:
the component A comprises the following raw materials in parts by mass:
30 parts of alicyclic epoxy resin, namely 30 parts of alicyclic epoxy resin,
two 10 parts of alicyclic epoxy resin and 10 parts of epoxy resin,
5 parts of hydroxyl-terminated silicon rubber,
20 parts of heat-conducting filler (10 parts of powdered diamond and 10 parts of modified spherical alumina powder),
19 parts of flame retardant (12.5 parts of aluminum hydroxide powder, 6.5 parts of nano antimony trioxide powder),
10 parts of R-902+ titanium dioxide powder,
0.3 part of BYK-333 leveling agent,
0.1 part of BYK-057 defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite.
The component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 5
The embodiment provides a flame-retardant structural adhesive suitable for roller coating, which comprises the following formula:
the component A comprises the following raw materials in parts by mass:
23 parts of alicyclic epoxy resin,
two (17) parts of alicyclic epoxy resin,
5 parts of hydroxyl-terminated silicon rubber,
22 parts of heat-conducting filler (11 parts of powdered diamond and 11 parts of modified spherical alumina powder),
16 parts of flame retardant (11 parts of aluminum hydroxide powder and 5 parts of nano antimony trioxide powder),
11 parts of R-902+ titanium dioxide powder,
0.25 part of BYK-333 leveling agent,
0.15 part of BYK-057 defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite.
The component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 6
The embodiment provides a flame-retardant structural adhesive with high thermal conductivity, which is suitable for roll coating and comprises the following formula:
the component A comprises the following raw materials in parts by mass:
23 parts of alicyclic epoxy resin,
17 parts of two alicyclic epoxy resins, namely,
5 parts of hydroxyl-terminated silicon rubber,
25 parts of heat-conducting filler (14 parts of powdered diamond, 11 parts of modified spherical alumina powder),
15 parts of flame retardant (10 parts of aluminum hydroxide powder and 5 parts of nano antimony trioxide powder),
9 parts of R-902+ titanium dioxide powder,
0.25 part of BYK-333 leveling agent,
0.15 part of BYK-057 defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite.
The component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 7
The embodiment provides a flame-retardant structural adhesive with high reflectivity suitable for roll coating, which comprises the following formula:
the component A comprises the following raw materials in parts by mass:
23 parts of alicyclic epoxy resin,
two (17) parts of alicyclic epoxy resin,
5 parts of hydroxyl-terminated silicon rubber,
20 parts of heat-conducting filler (10 parts of powdered diamond and 10 parts of modified spherical alumina powder),
15 parts of flame retardant (10 parts of aluminum hydroxide powder and 5 parts of nano antimony trioxide powder),
14 parts of R-902+ titanium dioxide powder,
0.25 part of BYK-333 leveling agent,
0.15 part of BYK-057 defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite.
The component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 8
The embodiment provides a flame-retardant structural adhesive suitable for roller coating and having a good flame-retardant effect, and the formula of the flame-retardant structural adhesive is as follows:
the component A comprises the following raw materials in parts by mass:
30 parts of alicyclic epoxy resin, namely 30 parts of alicyclic epoxy resin,
two 10 parts of alicyclic epoxy resin and 10 parts of epoxy resin,
5 parts of hydroxyl-terminated silicon rubber,
20 parts of heat-conducting filler (10 parts of powdered diamond and 10 parts of modified spherical alumina powder),
19 parts of flame retardant (12.5 parts of aluminum hydroxide powder, 6.5 parts of nano antimony trioxide powder),
10 parts of R-902+ titanium dioxide powder,
0.25 part of BYK-333 leveling agent,
0.15 part of BYK-057 defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite.
The component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 9
The embodiment provides a flame-retardant structural adhesive suitable for screen printing, which comprises the following formula:
the component A comprises the following raw materials in parts by mass:
16 parts of alicyclic epoxy resin, namely, cycloaliphatic epoxy resin,
24 parts of two alicyclic epoxy resins, namely 24 parts,
5 parts of hydroxyl-terminated silicon rubber,
22 parts of heat-conducting filler (11 parts of powdered diamond and 11 parts of modified spherical alumina powder),
16 parts of flame retardant (11 parts of aluminum hydroxide powder and 5 parts of nano antimony trioxide powder),
11 parts of R-902+ titanium dioxide powder,
0.2 part of a digao 450 leveling agent,
0.2 part of BYK-066N defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite;
the component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 10
The embodiment provides a flame-retardant structural adhesive with high thermal conductivity suitable for screen printing, which comprises the following formula:
the component A comprises the following raw materials in parts by mass:
16 parts of alicyclic epoxy resin, namely, cycloaliphatic epoxy resin,
24 parts of two alicyclic epoxy resins, namely 24 parts,
5 parts of hydroxyl-terminated silicon rubber,
25 parts of heat-conducting filler (14 parts of powdered diamond, 11 parts of modified spherical alumina powder),
15 parts of flame retardant (10 parts of aluminum hydroxide powder and 5 parts of nano antimony trioxide powder),
9 parts of R-902+ titanium dioxide powder,
0.2 part of a digao 450 leveling agent,
0.2 part of BYK-066N defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite.
The component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 11
The embodiment provides a flame-retardant structural adhesive with high reflectivity suitable for screen printing, which comprises the following formula:
the component A comprises the following raw materials in parts by mass:
16 parts of alicyclic epoxy resin, namely, cycloaliphatic epoxy resin,
24 parts of two alicyclic epoxy resins, namely cycloaliphatic epoxy resin,
5 parts of hydroxyl-terminated silicon rubber,
20 parts of heat-conducting filler (10 parts of powdered diamond and 10 parts of modified spherical alumina powder),
15 parts of flame retardant (10 parts of aluminum hydroxide powder and 5 parts of nano antimony trioxide powder),
14 parts of R-902+ titanium dioxide powder,
0.2 part of a flatting agent with a molecular weight of 450 digao,
0.2 part of BYK-066N defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite;
the component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 12
The embodiment provides a flame-retardant structural adhesive with a prominent flame-retardant effect, which is suitable for dip-coating glass fiber cloth, and the formula of the flame-retardant structural adhesive is as follows:
the component A comprises the following raw materials in parts by mass:
16 parts of alicyclic epoxy resin, namely, cycloaliphatic epoxy resin,
24 parts of two alicyclic epoxy resins, namely 24 parts,
5 parts of hydroxyl-terminated silicon rubber,
20 parts of heat-conducting filler (10 parts of powdered diamond and 10 parts of modified spherical alumina powder),
19 parts of flame retardant (12.5 parts of aluminum hydroxide powder, 6.5 parts of nano antimony trioxide powder),
10 parts of R-902+ titanium dioxide powder,
0.2 part of a digao 450 leveling agent,
0.2 part of BYK-066N defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite;
the component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 13
The embodiment provides a flame-retardant structural adhesive suitable for manufacturing a prepreg by dip-coating glass fiber cloth, which comprises the following formula:
the component A comprises the following raw materials in parts by mass:
30 parts of alicyclic epoxy resin, namely 30 parts of alicyclic epoxy resin,
two 10 parts of alicyclic epoxy resin and 10 parts of epoxy resin,
5 parts of hydroxyl-terminated silicon rubber,
22 parts of powder diamond as a heat-conducting filler,
16 parts of fire retardant, namely aluminum hydroxide powder,
11 parts of R-902+ titanium dioxide powder,
0.3 part of BYK-333 leveling agent,
0.1 part of BYK-057 defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite;
the component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 14
The embodiment provides a flame-retardant structural adhesive suitable for manufacturing a prepreg by dip-coating glass fiber cloth, which comprises the following formula:
the component A comprises the following raw materials in parts by mass:
30 parts of alicyclic epoxy resin, namely 30 parts of alicyclic epoxy resin,
two 10 parts of alicyclic epoxy resin and 10 parts of epoxy resin,
5 parts of hydroxyl-terminated silicon rubber,
22 parts of heat-conducting filler, namely modified spherical alumina powder,
16 parts of flame retardant, namely nano antimony trioxide powder,
11 parts of R-902+ titanium dioxide powder,
0.3 part of BYK-333 leveling agent,
0.1 part of BYK-057 defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite.
The component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 15
The embodiment provides a flame-retardant structural adhesive suitable for roller coating, which comprises the following formula:
the component A comprises the following raw materials in parts by mass:
23 parts of alicyclic epoxy resin,
two (17) parts of alicyclic epoxy resin,
5 parts of hydroxyl-terminated silicon rubber,
22 parts of powder diamond as a heat-conducting filler,
16 parts of aluminum hydroxide powder serving as a flame retardant,
11 parts of R-902+ titanium dioxide powder,
0.25 part of BYK-333 leveling agent,
0.15 part of BYK-057 defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite.
The component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex,
0.2 part of boron trifluoride-benzylamine complex.
Example 16
The embodiment provides a flame-retardant structural adhesive suitable for roller coating, which comprises the following formula:
the component A comprises the following raw materials in parts by mass:
23 parts of alicyclic epoxy resin,
17 parts of two alicyclic epoxy resins, namely,
5 parts of hydroxyl-terminated silicon rubber,
22 parts of heat-conducting filler, namely modified spherical alumina powder,
16 parts of flame retardant, namely nano antimony trioxide powder,
11 parts of R-902+ titanium dioxide powder,
0.25 part of BYK-333 leveling agent,
0.15 part of BYK-057 defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite;
the component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex,
0.2 part of boron trifluoride-benzylamine complex.
Example 17
The embodiment provides a flame-retardant structural adhesive suitable for screen printing, which comprises the following formula:
the component A comprises the following raw materials in parts by mass:
16 parts of alicyclic epoxy resin, namely, cycloaliphatic epoxy resin,
24 parts of two alicyclic epoxy resins, namely cycloaliphatic epoxy resin,
5 parts of hydroxyl-terminated silicon rubber,
22 parts of powder diamond as a heat-conducting filler,
16 parts of aluminum hydroxide powder serving as a flame retardant,
11 parts of R-902+ titanium dioxide powder,
0.2 part of a digao 450 leveling agent,
0.2 part of BYK-066N defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite;
the component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
Example 18
The embodiment provides a flame-retardant structural adhesive suitable for screen printing, which comprises the following formula:
the component A comprises the following raw materials in parts by mass:
16 parts of alicyclic epoxy resin, namely, cycloaliphatic epoxy resin,
24 parts of two alicyclic epoxy resins, namely 24 parts,
5 parts of hydroxyl-terminated silicon rubber,
22 parts of heat-conducting filler, namely modified spherical alumina powder,
16 parts of flame retardant, namely nano antimony trioxide powder,
11 parts of R-902+ titanium dioxide powder,
0.2 part of a digao 450 leveling agent,
0.2 part of BYK-066N defoaming agent,
2 parts of KH-560 coupling agent,
1.8 parts of SN-2311 dispersant,
1.8 parts of SD-2 organic bentonite.
The component B comprises the following raw materials in parts by mass:
99.8 parts of methylhexahydrophthalic anhydride,
0.2 part of boron trifluoride-benzylamine complex.
The mass ratio of the component A to the component B in the above example is 1: 0.3, mixing and stirring uniformly.
The performance test methods of the glues obtained in examples 1, 2, 3,4, 13 and 14 are as follows: soaking glass fiber cloth in the glue, taking out the glue, semi-curing, cutting into strips with the width of 25mm, hot-pressing between copper foil and glass at 180 ℃ or between the copper foil and an aluminum plate after oil removal, acid cleaning and passivation, curing for 10 minutes, and testing the 180-degree peel strength. The reflectivity was measured on glass substrates, which were coated with glue by means of roller coating onto 2 sheets of glass, cured one sheet at 180 ℃ for 10 minutes and one sheet at 290 ℃ for 10 minutes, compared to the reflectivity after baking at 290 ℃ for 10 minutes and curing at 180 ℃ for 10 minutes. The color difference is measured by coating on 2 aluminum plates by roller coating, curing for 10 minutes at 180 ℃ and baking for 10 minutes at 290 ℃, and comparing the color difference value between baking for 10 minutes at 290 ℃ and curing for 10 minutes at 180 ℃.
The performance test methods of the glues obtained in example 5, example 6, example 7, example 8, example 15 and example 16 are as follows: and (3) rolling the glass and an aluminum plate subjected to oil removal, acid pickling and passivation by using a wire rod, respectively coating 25mm copper foil, vacuumizing and defoaming, placing the glass and the aluminum plate at 180 ℃ for baking for 10 minutes, and testing 180-degree peel strength after cooling. The reflectivity was measured on glass substrates, which were coated with glue by means of roller coating onto 2 sheets of glass, cured one sheet at 180 ℃ for 10 minutes and one sheet at 290 ℃ for 10 minutes, compared to the reflectivity after baking at 290 ℃ for 10 minutes and curing at 180 ℃ for 10 minutes. The color difference test roller is coated on an aluminum plate with 2 pieces without copper foil, cured at 180 ℃ for 10 minutes, and baked at 290 ℃ for 10 minutes to compare the reflectivity and the yellowing with the normal curing.
The performance test methods of the glues obtained in example 9, example 10, example 11, example 12, example 17 and example 18 are as follows: screen-printing on glass and an aluminum plate subjected to oil removal, acid cleaning and passivation by using a 150-mesh screen plate, covering a copper foil with a thickness of 25mm respectively, vacuumizing and defoaming, placing at 180 ℃, baking for 10 minutes, cooling and testing 180-degree peel strength. The reflectance was measured on a glass substrate using a 150 mesh screen printed onto 2 sheets of glass, one sheet cured at 180 ℃ for 10 minutes, one sheet baked at 290 ℃ for 10 minutes, and the reflectance was compared between baking at 290 ℃ for 10 minutes and curing at 180 ℃ for 10 minutes. Color difference test 150 mesh screen printing was performed on 2 sheets of non-copper clad aluminum plate, cured at 180 ℃ for 10 minutes, and one was baked at 290 ℃ for 10 minutes to compare the reflectance and yellowing to normal curing. Wherein the thickness of the 150-mesh printing glue is 18 +/-1 mu m, and the gluing thickness of the roller is adjusted in a 16-20 mu m interval and has the same thickness, the contrast reflectivity and the yellowing property.
In all the examples, the thermal conductivity is measured by casting a rubber block with the thickness of more than 1cm in a 10cm × 10cm mould by using rubber, polishing the surface by using a polisher after the curing is completed, coating a layer of heat-conducting silicone grease on the upper surface and the lower surface, and placing the polished silicone grease in a thermal conductivity meter to measure the thermal conductivity. All examples flame retardant tests samples 5mm thick, 13mm wide and 125mm long were made for testing.
The test results are shown in the following table:
in the table:
1. the viscosity test method comprises the following steps: the viscosity was measured with a six-speed rotational viscometer for epoxy glue systems at 25 ℃ using a digital display viscometer, Shanghainem NDJ-8S.
2. 180 ° peel strength test method: the 180 DEG peel strength was determined in accordance with GB/T2790-1995 standard. Tested using a smart ZQ-990LA universal tester.
In the examples, the 180 DEG peel strength was more than 2kg/25mm, and the excellent peel strength was obtained.
3. The thermal conductivity test method comprises the following steps: thermal conductivity measurements were performed according to ASTM D5470 standard. Testing by using Hunan DRPL-2 thermal conductivity tester. The composite heat-conducting filler and a single heat-conducting filler are respectively used in the examples for testing, and the thermal conductivity of the examples of the composite heat-conducting filler exceeds 2W/(m.K).
Comparing the above-mentioned embodiment can know that the thermal conductivity of a heat conduction filler reduces alone, need use the powder of different particle diameters to match each other and can reach better effect. The powder diamond has high thermal conductivity but large particle size, gaps between the solidified powder and the powder are large and the thermal conductivity is low, the modified alumina powder has small particle size but the thermal conductivity is inferior to that of the powder diamond, the two kinds of powder are compounded, and the modified alumina powder can be filled around the powder diamond to improve the thermal conductivity. The heat conductivity of the composite heat-conducting powder meets the use requirement of high-end electronic products, and the problem of aging deformation caused by slow heat dissipation and local high temperature due to poor heat conduction of most adhesives in the electronic products is solved.
4. The reflectivity test method comprises the following steps: the preparation of the samples is carried out strictly according to the provisions of the relevant national standard GB 9271-1988. Tested using a proficient council model C84-III reflectance meter. After reflow soldering for 10 minutes at 290 ℃, the reflectivity is slightly reduced, and the heat-resistant oxidation property is good.
5. The flame retardant test method comprises the following steps: UL94 flame retardant test method
HB level horizontal burn test;
V0-V2 rating vertical burn test;
HB: the lowest flame retardant rating in the UL94 standard. Requiring a burn rate of less than 40 mm per minute for samples 3 to 13mm thick; a sample less than 3mm thick with a burning rate less than 70 mm per minute; or extinguished before the 100 mm mark;
v-2: after two 10 second burn tests on the samples, the flame extinguished within 60 seconds. The cotton wool below 30cm can be ignited.
V-1: after two 10 second burn tests on the samples, the flame extinguished within 60 seconds. The cotton wool below 30cm cannot be ignited.
V-0: after two 10 second burn tests on the samples, the flame extinguished within 10 seconds.
Compared with the independent use of different flame retardant powders, the aluminum hydroxide has better flame retardancy, and the nano antimony trioxide is a flame retardant aid and can play a better flame retardant role only by being matched with other flame retardant materials. The flame retardant after compounding is better than the effect of singly using one flame retardant.
6. The color difference testing method comprises the following steps: the color of the coating is tested by a color difference meter according to GB 11186.1-1989. The test was carried out using a three-en-time SC-10 colorimeter. Δ E represents the magnitude of the total color difference:
Δ E in the range of 0-0.25 means very little or no, an ideal match;
Δ E in the range of 0.25-0.5 represents a minor, acceptable match;
Δ E in the range of 0.5-1.0 represents slight to moderate, and is acceptable in some applications;
Δ E in the range of 1.0-2.0 means moderate, acceptable in certain applications;
Δ E is in the range of 2.0-4.0 indicating a gap, acceptable for certain applications;
Δ E above 4.0 represents a very large value, unacceptable in most applications.
It can be seen that the sample wafer which is subjected to reflow soldering at 290 ℃ is compared with the sample wafer which is not subjected to reflow soldering, and the comprehensive color difference is small and acceptable.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (8)
1. The utility model provides a fire-retardant structure of high temperature resistant high heat conduction high reflection glues which characterized in that: the structural adhesive is composed of a component A and a component B:
the component A comprises the following raw materials in parts by mass:
10-30 parts of alicyclic epoxy resin,
10-30 parts of a second alicyclic epoxy resin,
5-10 parts of silicon rubber,
20-40 parts of heat-conducting filler,
10-20 parts of a flame retardant,
8-16 parts of titanium dioxide powder,
0.1 to 1 portion of a leveling agent,
0.1 to 0.3 portion of defoaming agent,
2-10 parts of a silane coupling agent,
1-3 parts of a dispersing agent,
1-3 parts of organic bentonite;
the component B comprises the following raw materials in parts by mass:
99.5 to 99.9 portions of phthalic anhydride,
0.1-0.5 part of boron trifluoride amine complex accelerator;
the cycloaliphatic epoxy resin I is 3, 4-epoxy cyclohexane carboxylic acid-3 ', 4' -epoxy cyclohexane methyl ester, and the cycloaliphatic epoxy resin II is epoxidized polybutadiene resin.
2. The high-temperature-resistant high-thermal-conductivity high-reflection flame-retardant structural adhesive according to claim 1, characterized in that: the heat-conducting filler is composed of diamond and modified spherical alumina according to the mass ratio of 1-1.5: 1.
3. The high-temperature-resistant high-thermal-conductivity high-reflection flame-retardant structural adhesive according to claim 1, characterized in that: the flame retardant consists of aluminum hydroxide and nano antimony trioxide according to the mass ratio of 1.5-2.5: 1.
4. The high-temperature-resistant high-thermal-conductivity high-reflection flame-retardant structural adhesive according to claim 1, characterized in that: the phthalic anhydride is at least one of methyl tetrahydrophthalic anhydride MeTHPA, methyl hexahydrophthalic anhydride MeHHPA and methyl nadic anhydride MNA.
5. The high-temperature-resistant high-thermal-conductivity high-reflection flame-retardant structural adhesive according to claim 1, characterized in that: the boron trifluoride amine complex accelerator is at least one of boron trifluoride-benzylamine complex and boron trifluoride-2, 4-dimethylaniline complex.
6. A preparation method of the flame-retardant structural adhesive as claimed in any one of claims 1 to 5, which is characterized in that:
under the stirring state, firstly mixing the alicyclic epoxy resin I and the alicyclic epoxy resin II, heating at 80 ℃ until the alicyclic epoxy resin I and the alicyclic epoxy resin II are dissolved, then adding the silicon rubber, heating at 120 ℃ for dehydration condensation for 2 hours, then adding the silane coupling agent, the dispersing agent, the organic bentonite, the flatting agent, the antifoaming agent, the titanium dioxide, the heat-conducting filler and the flame retardant, stirring uniformly, and filtering to obtain a component A;
mixing phthalic anhydride and boron trifluoride amine complex, heating at 80 ℃ to dissolve, and filtering to obtain a component B;
when in use, the component A and the component B are mixed according to the mass ratio of 1: 0.3, mixing uniformly to obtain the flame-retardant structural adhesive with high temperature resistance, high heat conductivity and high reflection.
7. The application of the flame-retardant structural adhesive as claimed in any one of claims 1 to 5, wherein: the adhesive is used for bonding the copper foil and the glass substrate, the copper foil and the aluminum substrate or used as an adhesive of a PCB (printed Circuit Board).
8. A glass-based miniLED substrate, characterized in that: the glass and the copper foil of the glass-based miniLED substrate are bonded by the flame-retardant structural adhesive according to any one of claims 1 to 5.
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| CN111040698A (en) * | 2019-12-18 | 2020-04-21 | 镇江利德尔复合材料有限公司 | Epoxy resin pouring sealant, preparation method and novel electric drive motor |
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| US5420202A (en) * | 1994-04-15 | 1995-05-30 | Shell Oil Company | Epoxidized low viscosity rubber toughening modifiers for cycloaliphatic epoxy resins |
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Denomination of invention: A flame-retardant structural adhesive with high temperature resistance, high thermal conductivity, and high reflection and its application Effective date of registration: 20231225 Granted publication date: 20230516 Pledgee: Hefei high tech Company limited by guarantee Pledgor: HEFEI VIGON MATERIAL TECHNOLOGIES Co.,Ltd. Registration number: Y2023980074263 |
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