CN109705784A - A kind of high-peeling strength epoxy construction adhesive and preparation method thereof - Google Patents
A kind of high-peeling strength epoxy construction adhesive and preparation method thereof Download PDFInfo
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- CN109705784A CN109705784A CN201811468067.2A CN201811468067A CN109705784A CN 109705784 A CN109705784 A CN 109705784A CN 201811468067 A CN201811468067 A CN 201811468067A CN 109705784 A CN109705784 A CN 109705784A
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- component
- peeling strength
- epoxy resin
- mixing
- curing agent
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000004593 Epoxy Substances 0.000 title description 9
- 239000000853 adhesive Substances 0.000 title description 8
- 230000001070 adhesive effect Effects 0.000 title description 8
- 238000010276 construction Methods 0.000 title description 4
- 239000003822 epoxy resin Substances 0.000 claims abstract description 35
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 35
- 239000002994 raw material Substances 0.000 claims abstract description 29
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 150000001412 amines Chemical class 0.000 claims abstract description 16
- 229920006332 epoxy adhesive Polymers 0.000 claims abstract description 16
- 229910002012 Aerosil® Inorganic materials 0.000 claims abstract description 14
- 239000000945 filler Substances 0.000 claims abstract description 13
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 12
- 239000002002 slurry Substances 0.000 claims abstract description 10
- 239000003085 diluting agent Substances 0.000 claims abstract description 8
- 239000012745 toughening agent Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 27
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 18
- 239000000463 material Substances 0.000 claims description 17
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 16
- 238000007664 blowing Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 12
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 11
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 claims description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 229920005989 resin Polymers 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- 229920000459 Nitrile rubber Polymers 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 229930185605 Bisphenol Natural products 0.000 claims description 4
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 4
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 4
- 229910021485 fumed silica Inorganic materials 0.000 claims description 4
- 239000011863 silicon-based powder Substances 0.000 claims description 4
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 claims description 4
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 125000003368 amide group Chemical group 0.000 claims description 3
- 239000011258 core-shell material Substances 0.000 claims description 3
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 3
- 239000000539 dimer Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229920002635 polyurethane Polymers 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- YSUQLAYJZDEMOT-UHFFFAOYSA-N 2-(butoxymethyl)oxirane Chemical group CCCCOCC1CO1 YSUQLAYJZDEMOT-UHFFFAOYSA-N 0.000 claims description 2
- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 claims description 2
- WTYYGFLRBWMFRY-UHFFFAOYSA-N 2-[6-(oxiran-2-ylmethoxy)hexoxymethyl]oxirane Chemical compound C1OC1COCCCCCCOCC1CO1 WTYYGFLRBWMFRY-UHFFFAOYSA-N 0.000 claims description 2
- KUAUJXBLDYVELT-UHFFFAOYSA-N 2-[[2,2-dimethyl-3-(oxiran-2-ylmethoxy)propoxy]methyl]oxirane Chemical compound C1OC1COCC(C)(C)COCC1CO1 KUAUJXBLDYVELT-UHFFFAOYSA-N 0.000 claims description 2
- 241000790917 Dioxys <bee> Species 0.000 claims description 2
- 229910003978 SiClx Inorganic materials 0.000 claims description 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 claims description 2
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 claims description 2
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 2
- 239000004843 novolac epoxy resin Substances 0.000 claims description 2
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 229910000077 silane Inorganic materials 0.000 claims description 2
- HBGPNLPABVUVKZ-POTXQNELSA-N (1r,3as,4s,5ar,5br,7r,7ar,11ar,11br,13as,13br)-4,7-dihydroxy-3a,5a,5b,8,8,11a-hexamethyl-1-prop-1-en-2-yl-2,3,4,5,6,7,7a,10,11,11b,12,13,13a,13b-tetradecahydro-1h-cyclopenta[a]chrysen-9-one Chemical compound C([C@@]12C)CC(=O)C(C)(C)[C@@H]1[C@H](O)C[C@]([C@]1(C)C[C@@H]3O)(C)[C@@H]2CC[C@H]1[C@@H]1[C@]3(C)CC[C@H]1C(=C)C HBGPNLPABVUVKZ-POTXQNELSA-N 0.000 claims 1
- PFRGGOIBYLYVKM-UHFFFAOYSA-N 15alpha-hydroxylup-20(29)-en-3-one Natural products CC(=C)C1CCC2(C)CC(O)C3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 PFRGGOIBYLYVKM-UHFFFAOYSA-N 0.000 claims 1
- NFVPEIKDMMISQO-UHFFFAOYSA-N 4-[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC=C(O)C=C1 NFVPEIKDMMISQO-UHFFFAOYSA-N 0.000 claims 1
- ZYUVGYBAPZYKSA-UHFFFAOYSA-N 5-(3-hydroxybutan-2-yl)-4-methylbenzene-1,3-diol Chemical compound CC(O)C(C)C1=CC(O)=CC(O)=C1C ZYUVGYBAPZYKSA-UHFFFAOYSA-N 0.000 claims 1
- SOKRNBGSNZXYIO-UHFFFAOYSA-N Resinone Natural products CC(=C)C1CCC2(C)C(O)CC3(C)C(CCC4C5(C)CCC(=O)C(C)(C)C5CCC34C)C12 SOKRNBGSNZXYIO-UHFFFAOYSA-N 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 claims 1
- NHADDZMCASKINP-HTRCEHHLSA-N decarboxydihydrocitrinin Natural products C1=C(O)C(C)=C2[C@H](C)[C@@H](C)OCC2=C1O NHADDZMCASKINP-HTRCEHHLSA-N 0.000 claims 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 238000005303 weighing Methods 0.000 description 13
- 238000012360 testing method Methods 0.000 description 6
- ZDWQSEWVPQWLFV-UHFFFAOYSA-N C(CC)[Si](OC)(OC)OC.[O] Chemical compound C(CC)[Si](OC)(OC)OC.[O] ZDWQSEWVPQWLFV-UHFFFAOYSA-N 0.000 description 4
- -1 benzyl glycidol Chemical compound 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 229920006335 epoxy glue Polymers 0.000 description 3
- 239000003292 glue Substances 0.000 description 3
- QNYBOILAKBSWFG-UHFFFAOYSA-N 2-(phenylmethoxymethyl)oxirane Chemical compound C1OC1COCC1=CC=CC=C1 QNYBOILAKBSWFG-UHFFFAOYSA-N 0.000 description 2
- HSDVRWZKEDRBAG-UHFFFAOYSA-N 2-[1-(oxiran-2-ylmethoxy)hexoxymethyl]oxirane Chemical compound C1OC1COC(CCCCC)OCC1CO1 HSDVRWZKEDRBAG-UHFFFAOYSA-N 0.000 description 2
- SHKUUQIDMUMQQK-UHFFFAOYSA-N 2-[4-(oxiran-2-ylmethoxy)butoxymethyl]oxirane Chemical compound C1OC1COCCCCOCC1CO1 SHKUUQIDMUMQQK-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
- CIPOCPJRYUFXLL-UHFFFAOYSA-N 2,3,4-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC=C(O)C(CN(C)C)=C1CN(C)C CIPOCPJRYUFXLL-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- DSROZUMNVRXZNO-UHFFFAOYSA-K tris[(1-naphthalen-1-yl-3-phenylnaphthalen-2-yl)oxy]alumane Chemical compound C=1C=CC=CC=1C=1C=C2C=CC=CC2=C(C=2C3=CC=CC=C3C=CC=2)C=1O[Al](OC=1C(=C2C=CC=CC2=CC=1C=1C=CC=CC=1)C=1C2=CC=CC=C2C=CC=1)OC(C(=C1C=CC=CC1=C1)C=2C3=CC=CC=C3C=CC=2)=C1C1=CC=CC=C1 DSROZUMNVRXZNO-UHFFFAOYSA-K 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
Abstract
The invention discloses a kind of epoxy adhesives of high-peeling strength, which is characterized in that is made of component A and B component, wherein A/B component proportion is according to mass ratio A:B=2:1;Wherein component A is prepared by the raw material of following mass percent: epoxy resin 30~60%, toughener 5~20%, diluent 3~20%, filler 20~50%, hydrophobicity aerosil 0.2~1%, silane coupling agent 1~3%, blue slurry 0.5~2%;Wherein B component is prepared by the raw material of following mass percent: Versamid curing agent 30~60%, modified amine curing agent 30~60%, promotor 1~3%, filler 5~20%, hydrophobicity aerosil 0.2~1%, silane coupling agent 1~3%.The invention also discloses preparation methods.The present invention provides a kind of epoxy adhesive of high-peeling strength, have the characteristics that the operating time is long, adhesion strength is big, peel strength is high.
Description
Technical field
The present invention relates to technical field of adhesive preparation, in particular to a kind of high-peeling strength epoxy construction adhesive and its
Preparation method.
Background technique
Epoxy resin is a kind of thermosetting resin being of wide application, and starts to occur in the latter stage in 19th century, and 20
The mid-term in century is able to fast development.Its solidfied material is mixed with curing agent by certain mass proportion by epoxy prepolymer
Solidify and obtain, it may be necessary to add some functional stuffings and auxiliary agent, and then prepare epoxy resin composite material.Due to epoxy
Resin prepolymer and curing agent are many kinds of, in addition different types of functional stuffing and auxiliary agent, this allows for preparing different performance
Epoxy resin composite material be possibly realized, meet the needs of different field.
The owned high intensity of epoxy resin, high temperature resistant, insulating properties, chemical inertness and adhesion and be used for paint, knot
The fields such as structure adhesive and composite material.But the brittleness of epoxy resin itself is big and poor impact toughness and make its application range by
It to limitation, especially some high-performance fields, thus needs to carry out it Research on Toughening, improves the comprehensive performance of resin.
Summary of the invention
Epoxide-resin glue brittleness in the prior art is big, stripper-resistance/impact resistance difference deficiency in order to solve, of the invention
There is provided a kind of epoxy adhesives of high-peeling strength for the first purpose, with the operating time is long, adhesion strength is big, removing is strong
Spend the features such as high.
The second object of the present invention is to provide the preparation method of the epoxy adhesive of above-mentioned high-peeling strength.
To achieve the above object, technical solution provided by the invention are as follows:
A kind of epoxy adhesive of high-peeling strength as an object of the present invention, is made of component A and B component,
Wherein A/B component proportion is according to mass ratio A:B=2:1;
Wherein component A is prepared by the raw material of following mass percent:
Epoxy resin 30~60%, toughener 5~20%, diluent 3~20%, filler 20~50%, hydrophobicity gas phase
Silica 0.2~1%, silane coupling agent 1~3%, blue slurry 0.5~2%;
Wherein B component is prepared by the raw material of following mass percent:
Versamid curing agent 30~60%, modified amine curing agent 30~60%, promotor 1~3%, filler 5~
20%, hydrophobicity aerosil 0.2~1%, silane coupling agent 1~3%.
In a preferred embodiment of the invention, the epoxy resin is bisphenol A type epoxy resin, bisphenol F type epoxy
The mixing of one or both of resin, novolac epoxy resin.
In a preferred embodiment of the invention, the toughener is nbr carboxyl terminal and epoxy resin pre-polymerization
One of object, core shell resin, end amido nitrile rubber, dimer acid modified epoxy resin, polyurethane modified epoxy resin are appointed
It anticipates two or more mixing.
In a preferred embodiment of the invention, the diluent is butyl glycidyl ether, benzyl glycidol
Ether, polypropylene glycol diglycidyl ether, 1,4- butanediol glycidol ether, 1,6 hexanediol diglycidylether, 1,6- hexamethylene
One of Hexanediol diglycidyl ether, neopentylglycol diglycidyl ether or any two or more mixing.
In a preferred embodiment of the invention, the filler be silicon powder, aluminium hydroxide, wollastonite, calcium carbonate,
One of talcum powder or any two or more mixing.
In a preferred embodiment of the invention, the Versamid curing agent amine value be 220,280,340,
One of 380mgKOH/g or any two or more mixing.
In a preferred embodiment of the invention, the modified amine curing agent is modified fatty amine;
In a preferred embodiment of the invention, the promotor in the B component is 2,4,6- tri- (dimethylamino first
Base) phenol (DMP-30), benzyl dimethylamine, benzyl alcohol, one of triphenylphosphine or any two or more mixing.
In a preferred embodiment of the invention, the silane coupling agent is γ-glycidyl ether oxygen propyl front three
Oxysilane (KH-560), γ-aminopropyl triethoxysilane (KH-550), vinyltriethoxysilane (A151), vinyl three
One of methoxy silane (A171), (beta-methoxy ethyoxyl) silane of vinyl three (A172) or any two or more mixing.
The preparation method of the epoxy adhesive of a kind of high-peeling strength as the second object of the present invention, by following steps
Composition:
1) preparation of component A: weighing each raw material of component A by formula, by epoxy resin, toughener, diluent, filler, dredges
Aqueous fumed silica, silane coupling agent, blue slurry are successively put into reaction kettle, are stirred by the mixing speed range of 40r/min
Mix 2h to material uniformly, no color differnece, then vacuumize 2h by the mixing speed range stirring of 20r/min, when removing stirring generates
Bubble, after blowing dispense, be sealed;
2) preparation of B component: weighing each raw material of B component by formula, by Versamid curing agent, modified amine curing
Agent, promotor, filler, hydrophobicity aerosil, silane coupling agent are successively put into reaction kettle, by the stirring of 40r/min
Velocity interval stir 2h to material uniformly, no color differnece, then by 20r/min mixing speed range stirring vacuumize 2h, remove
The bubble generated when stirring, after blowing dispense, be sealed;
3) A, B component are matched according to weight ratio A:B=2:1.
The invention has the beneficial effects that:
By introducing nbr carboxyl terminal and epoxy prepolymer, make this epoxy resin structural adhesive and metal, ceramics,
The substrates such as plastics have preferable adhesion strength, not only have toughness, but also improve the peel strength of epoxy structural rubber, adhesive strength,
Release surface situation is improved simultaneously, so that it becomes cohesional failure, there is glue on adhesives two sides;It is introduced in component A of the present invention a small amount of
Diluent reduces the viscosity of system, it is convenient to make its constructing operation, while suitable hydrophobicity aerosil is added, makes
Epoxy glue has thixotropy, and glue does not trickle everywhere after construction;Versamid curing agent is added in B component of the present invention, makes
Epoxy glue has the longer operating time, while also improving the toughness of epoxy glue.
Specific embodiment
The present invention will be further explained by way of examples below, does not therefore limit the present invention to the implementation
Among example range.
Embodiment 1
By the following component A raw material of quality weighing: bisphenol A epoxide resin (E-51) 50kg, nbr carboxyl terminal and epoxy
Resin prepolymer 10kg, 1,4- butanediol diglycidyl ether (622) 5kg, silicon powder 20kg, talcum powder 14kg, hydrophobicity gas
Aerosil 0.5kg, γ-glycidyl ether oxygen propyl trimethoxy silicane (KH-560) 1.5kg, blue slurry 1kg, above-mentioned original
Material be sequentially added into reaction kettle, by 40r/min be dispersed with stirring 2h to material uniformly, no color differnece, then by 20r/min stirring take out
Vacuum 2h, remove bubble, after blowing dispense, be sealed;
By the following B component raw material of quality weighing: Versamid curing agent 1# (amine value: 340mgKOH/g) 50kg, changing
Tri- (dimethylamino methyl) phenol (DMP-30) 1.5kg of property amine hardener 35kg, 2,4,6-, filler 10kg, hydrophobicity gas phase dioxy
SiClx 0.5kg, γ-aminopropyl triethoxysilane (KH-550) 1.5kg, above-mentioned raw materials are sequentially added into reaction kettle, by 40r/
Min be dispersed with stirring 2h to material uniformly, no color differnece, then vacuumize 2h, remove bubble, after blowing dispense, be sealed;
Embodiment 2
By the following component A raw material of quality weighing: bisphenol A epoxide resin (E-44) 50kg, nbr carboxyl terminal and epoxy
Resin prepolymer 10kg, core shell resin 6kg, benzyl glycidyl ether (XY-692) 10kg, silicon powder 20kg, talcum powder 14kg,
Hydrophobicity aerosil 0.5kg, γ-glycidyl ether oxygen propyl trimethoxy silicane (KH-560) 1.5kg, blue slurry
1kg, above-mentioned raw materials are sequentially added into reaction kettle, by 40r/min be dispersed with stirring 2h to material uniformly, no color differnece, then press
20r/min stirring vacuumizes 2h, removes bubble, after blowing dispense, be sealed;
By the following B component raw material of quality weighing: Versamid curing agent 1#30kg, Versamid curing agent 2#
It is 20kg, modified amine curing agent 35kg, 2,4,6- tri- (dimethylamino methyl) phenol (DMP-30) 1.5kg, calcium carbonate 10kg, hydrophobic
Property fumed silica 0.5kg, γ-aminopropyl triethoxysilane (KH-550) 1.5kg, above-mentioned raw materials are sequentially added into instead
Answer in kettle, by 40r/min be dispersed with stirring 2h to material uniformly, no color differnece, then vacuumize 2h, remove bubble, after blowing
Packing, is sealed;
Embodiment 3
By the following component A raw material of quality weighing: bisphenol A epoxide resin 20kg, bisphenol f type epoxy resin 35kg, carboxyl end group
Nitrile rubber and epoxy prepolymer 10kg, dimer acid modified epoxy resin 6kg, 1,2 cylohexanediol diglycidyl ethers
4kg, calcium carbonate 35kg, hydrophobicity aerosil 0.5kg, γ-glycidyl ether oxygen propyl trimethoxy silicane (KH-
560) 1.5kg, blue slurry 1kg, above-mentioned raw materials are sequentially added into reaction kettle, by 40r/min be dispersed with stirring 2h to material uniformly,
Then no color differnece vacuumizes 2h by 20r/min stirring, removes bubble, after blowing dispense, be sealed;
By the following B component raw material of quality weighing: Versamid curing agent 1#40kg, modified amine curing agent 35kg, end
It is amido nitrile rubber (ATBN) 6kg, 2,4,6- tri- (dimethylamino methyl) phenol (DMP-30) 1.5kg, calcium carbonate 10kg, hydrophobic
Property fumed silica 0.5kg, γ-aminopropyl triethoxysilane (KH-550) 1.5kg, above-mentioned raw materials are sequentially added into instead
Answer in kettle, by 40r/min be dispersed with stirring 2h to material uniformly, no color differnece, then vacuumize 2h, remove bubble, after blowing
Packing, is sealed;
Embodiment 4
By the following component A raw material of quality weighing: bisphenol A epoxide resin 10kg, bisphenol f type epoxy resin 35kg, carboxyl end group
Nitrile rubber and epoxy prepolymer 10kg, polyurethane modified epoxy resin 6kg, 1,2- cylohexanediol diglycidyl ether
4kg, calcium carbonate 35kg, hydrophobicity aerosil 0.5kg, γ-glycidyl ether oxygen propyl trimethoxy silicane (KH-
560) 1.5kg, blue slurry 1kg, above-mentioned raw materials are sequentially added into reaction kettle, by 40r/min be dispersed with stirring 2h to material uniformly,
Then no color differnece vacuumizes 2h by 20r/min stirring, removes bubble, after blowing dispense, be sealed;
By the following B component raw material of quality weighing: Versamid curing agent 1#50kg, modified amine curing agent 35kg, 2,
4,6- tri- (dimethylamino methyl) phenol (DMP-30) 1.5kg, calcium carbonate 10kg, hydrophobicity aerosil 0.5kg, γ-
Aminopropyl triethoxysilane (KH-550) 1.5kg, above-mentioned raw materials are sequentially added into reaction kettle, are dispersed with stirring by 40r/min
2h to material uniformly, no color differnece, then vacuumize 2h, remove bubble, after blowing dispense, be sealed;
Comparative example 1:
By the following component A raw material of quality weighing: bisphenol A epoxide resin 30kg, bisphenol f type epoxy resin 35kg, 1,2- ring
Hexanediol diglycidyl ether 4kg, calcium carbonate 35kg, hydrophobicity aerosil 0.5kg, γ-glycidyl ether oxygen propyl
Trimethoxy silane (KH-560) 1.5kg, blue slurry 1kg, above-mentioned raw materials are sequentially added into reaction kettle, stir by 40r/min
Disperse 2h to material uniformly, no color differnece, then vacuumize 2h by 20r/min stirring, remove bubble, after blowing dispense;
By the following B component raw material of quality weighing: tri- (dimethylamino first of Versamid curing agent 1#90kg, 2,4,6-
Base) phenol (DMP-30) 1.5kg, calcium carbonate 10kg, hydrophobicity aerosil 0.5kg, γ-aminopropyl-triethoxy silicon
Alkane (KH-550) 1.5kg, above-mentioned raw materials are sequentially added into reaction kettle, and it is uniform, colourless to material to be dispersed with stirring 2h by 40r/min
Difference, then vacuumizes 2h, removes bubble, after blowing dispense;
The above material presses A:B=2:1 (mass ratio) weighing respectively, is then bonded test piece, solidifies by 70 DEG C/2h, naturally cold
But it is tested to room temperature.
Test result is shown in Table 1:
Table 1
Testing standard is shown in Table 2:
Table 2
Test item | Testing standard | Test speed |
Room temperature tensile shear strength | GB/T 7124-2008 | 5mm/min |
70 DEG C of tensile shear strengths | GJB 444-1988 | 5mm/min |
T-type peel strength | GB/T 2791-1995 | 100mm/min |
90 ° of peel strengths | GJB 446-1988 | 100mm/min |
It can be absolutely proved by Tables 1 and 2, room temperature tensile shear strength of the invention, T-type peel strength, T-type removing effect
Fruit, 90 ° of peel strengths and 90 ° of peeling effect improve significantly.
Claims (10)
1. a kind of epoxy adhesive of high-peeling strength, which is characterized in that be made of component A and B component, wherein A/B group is distributed
Than according to mass ratio A:B=2:1;
Wherein component A is prepared by the raw material of following mass percent:
Epoxy resin 30~60%, toughener 5~20%, diluent 3~20%, filler 20~50%, hydrophobicity gas phase dioxy
SiClx 0.2~1%, silane coupling agent 1~3%, blue slurry 0.5~2%;
Wherein B component is prepared by the raw material of following mass percent:
Versamid curing agent 30~60%, modified amine curing agent 30~60%, promotor 1~3%, filler 5~20%,
Hydrophobicity aerosil 0.2~1%, silane coupling agent 1~3%.
2. a kind of epoxy adhesive of high-peeling strength as described in claim 1, which is characterized in that the epoxy resin is double
The mixing of one or both of phenol A type epoxy resin, bisphenol f type epoxy resin, novolac epoxy resin.
3. a kind of epoxy adhesive of high-peeling strength, which is characterized in that the toughener is nbr carboxyl terminal and ring
Oxygen resin prepolymer, core shell resin, end amido nitrile rubber, dimer acid modified epoxy resin, in polyurethane modified epoxy resin
One kind or any two or more mixing.
4. a kind of epoxy adhesive of high-peeling strength, which is characterized in that the diluent is butyl glycidyl ether, benzyl
Glycidol ether, polypropylene glycol diglycidyl ether, 1,4- butanediol glycidol ether, 1,6 hexanediol diglycidylether,
One of 1,6- cylohexanediol diglycidyl ether, neopentylglycol diglycidyl ether or any two or more mixing.
5. a kind of epoxy adhesive of high-peeling strength, which is characterized in that the filler is silicon powder, aluminium hydroxide, silicon ash
One of stone, calcium carbonate, talcum powder or any two or more mixing.
6. a kind of epoxy adhesive of high-peeling strength, which is characterized in that the Versamid curing agent amine value is
220,280,340, one of 380mgKOH/g or any two or more mixing.
7. a kind of epoxy adhesive of high-peeling strength, which is characterized in that the modified amine curing agent is modified fatty amine.
8. a kind of epoxy adhesive of high-peeling strength, which is characterized in that the promotor in the B component is 2,4,6- tri-
One of (dimethylamino methyl) phenol (DMP-30), benzyl dimethylamine, benzyl alcohol, triphenylphosphine are any two or more
Mixing.
9. a kind of epoxy adhesive of high-peeling strength, which is characterized in that the silane coupling agent is γ-glycidyl ether oxygen
Propyl trimethoxy silicane (KH-560), γ-aminopropyl triethoxysilane (KH-550), vinyltriethoxysilane
(A151), one of vinyltrimethoxysilane (A171), (beta-methoxy ethyoxyl) silane of vinyl three (A172) or appoint
It anticipates two or more mixing.
10. a kind of preparation method of the epoxy adhesive of high-peeling strength as described in any one of claim 1-9, by with
Lower step composition:
1) preparation of component A: each raw material of component A is weighed by formula, by epoxy resin, toughener, diluent, filler, hydrophobicity
Fumed silica, silane coupling agent, blue slurry are successively put into reaction kettle, stir 2h by the mixing speed range of 40r/min
To material uniformly, no color differnece, then vacuumize 2h by the mixing speed range stirring of 20r/min, the gas that when removing stirring generates
Bubble, after blowing dispense, be sealed;
2) preparation of B component: each raw material of B component is weighed by formula, by Versamid curing agent, modified amine curing agent, rush
It is successively put into reaction kettle into agent, filler, hydrophobicity aerosil, silane coupling agent, by the mixing speed model of 40r/min
Enclose stirring 2h to material uniformly, no color differnece, then 2h is vacuumized by the mixing speed range stirring of 20r/min, when removing stirring
The bubble of generation, after blowing dispense, be sealed;
3) A, B component are matched according to weight ratio A:B=2:1.
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CN111073570B (en) * | 2019-12-11 | 2022-02-25 | 康达新材料(集团)股份有限公司 | Medium-temperature curing high-toughness epoxy adhesive and preparation method thereof |
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