CN110157298A - A kind of modified epoxy sealant and preparation method thereof - Google Patents
A kind of modified epoxy sealant and preparation method thereof Download PDFInfo
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- CN110157298A CN110157298A CN201910465224.2A CN201910465224A CN110157298A CN 110157298 A CN110157298 A CN 110157298A CN 201910465224 A CN201910465224 A CN 201910465224A CN 110157298 A CN110157298 A CN 110157298A
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- parts
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- light stabilizer
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- preparation
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- 239000000565 sealant Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims description 28
- 239000004593 Epoxy Substances 0.000 title claims description 16
- 239000004611 light stabiliser Substances 0.000 claims abstract description 44
- 239000003822 epoxy resin Substances 0.000 claims abstract description 30
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 30
- 239000000203 mixture Substances 0.000 claims abstract description 26
- 239000006096 absorbing agent Substances 0.000 claims abstract description 25
- 241001122767 Theaceae Species 0.000 claims abstract description 21
- 235000013824 polyphenols Nutrition 0.000 claims abstract description 21
- 150000008442 polyphenolic compounds Chemical class 0.000 claims abstract description 19
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000007822 coupling agent Substances 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 11
- 239000003085 diluting agent Substances 0.000 claims abstract description 8
- 239000012745 toughening agent Substances 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 7
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 23
- 239000003292 glue Substances 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 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 18
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 15
- 150000002148 esters Chemical class 0.000 claims description 11
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 claims description 9
- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 claims description 9
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 claims description 9
- 235000005487 catechin Nutrition 0.000 claims description 9
- 229950001002 cianidanol Drugs 0.000 claims description 9
- 235000019441 ethanol Nutrition 0.000 claims description 9
- 229920001451 polypropylene glycol Polymers 0.000 claims description 9
- -1 glycidyl ester Chemical class 0.000 claims description 7
- VYKXQOYUCMREIS-UHFFFAOYSA-N methylhexahydrophthalic anhydride Chemical compound C1CCCC2C(=O)OC(=O)C21C VYKXQOYUCMREIS-UHFFFAOYSA-N 0.000 claims description 6
- QUAMTGJKVDWJEQ-UHFFFAOYSA-N octabenzone Chemical group OC1=CC(OCCCCCCCC)=CC=C1C(=O)C1=CC=CC=C1 QUAMTGJKVDWJEQ-UHFFFAOYSA-N 0.000 claims description 6
- 125000001931 aliphatic group Chemical group 0.000 claims description 5
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 5
- 239000011159 matrix material Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- MCZDHTKJGDCTAE-UHFFFAOYSA-M tetrabutylazanium;acetate Chemical compound CC([O-])=O.CCCC[N+](CCCC)(CCCC)CCCC MCZDHTKJGDCTAE-UHFFFAOYSA-M 0.000 claims description 4
- MRYQZMHVZZSQRT-UHFFFAOYSA-M tetramethylazanium;acetate Chemical compound CC([O-])=O.C[N+](C)(C)C MRYQZMHVZZSQRT-UHFFFAOYSA-M 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
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 3
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 150000003242 quaternary ammonium salts Chemical group 0.000 claims description 3
- 229920005989 resin Polymers 0.000 claims description 3
- 239000011347 resin Substances 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- PXJUBOLFJDSAQQ-UHFFFAOYSA-M tetrapropylazanium;acetate Chemical compound CC([O-])=O.CCC[N+](CCC)(CCC)CCC PXJUBOLFJDSAQQ-UHFFFAOYSA-M 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
- 229930185605 Bisphenol Natural products 0.000 claims description 2
- 229960000250 adipic acid Drugs 0.000 claims description 2
- 235000011037 adipic acid Nutrition 0.000 claims description 2
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 2
- 229940116351 sebacate Drugs 0.000 claims description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-L sebacate(2-) Chemical compound [O-]C(=O)CCCCCCCCC([O-])=O CXMXRPHRNRROMY-UHFFFAOYSA-L 0.000 claims description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical class OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 2
- ARYZCSRUUPFYMY-UHFFFAOYSA-N methoxysilane Chemical compound CO[SiH3] ARYZCSRUUPFYMY-UHFFFAOYSA-N 0.000 claims 1
- 150000002888 oleic acid derivatives Chemical class 0.000 claims 1
- 239000003963 antioxidant agent Substances 0.000 abstract description 10
- 230000003078 antioxidant effect Effects 0.000 abstract description 9
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 4
- 238000013329 compounding Methods 0.000 abstract description 2
- 230000005764 inhibitory process Effects 0.000 abstract description 2
- 238000005457 optimization Methods 0.000 abstract description 2
- 239000006097 ultraviolet radiation absorber Substances 0.000 abstract description 2
- 235000006708 antioxidants Nutrition 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 4
- 238000005538 encapsulation Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 3
- 230000000845 anti-microbial effect Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 2
- CIRMGZKUSBCWRL-LHLOQNFPSA-N (e)-10-[2-(7-carboxyheptyl)-5,6-dihexylcyclohex-3-en-1-yl]dec-9-enoic acid Chemical compound CCCCCCC1C=CC(CCCCCCCC(O)=O)C(\C=C\CCCCCCCC(O)=O)C1CCCCCC CIRMGZKUSBCWRL-LHLOQNFPSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004842 bisphenol F epoxy resin Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- LCGKKGWUTHIXIT-UHFFFAOYSA-N prop-1-ene triethoxysilane Chemical compound C=CC.C(C)O[SiH](OCC)OCC LCGKKGWUTHIXIT-UHFFFAOYSA-N 0.000 description 1
- UIIYYKQHEKITGI-UHFFFAOYSA-N propyl 2,2-dipropylpentanoate Chemical compound CCCOC(=O)C(CCC)(CCC)CCC UIIYYKQHEKITGI-UHFFFAOYSA-N 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000027772 skotomorphogenesis Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004383 yellowing Methods 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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/06—Printing inks based on fatty oils
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/08—Printing inks based on natural resins
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Sealing Material Composition (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention relates to a kind of resistance to yellow antibacterial epoxy resin sealants, including two component of A, B: where component A mainly includes 100 parts of epoxy resin, 5-12 parts of diluent, 0.3-5 parts of light stabilizer, 0.5-10 parts of coupling agent, 0.2-5 parts of dispersing agent；B component mainly includes 100 parts of curing agent, 0.2-5 parts of toughener, 0.2-3 parts of coupling agent；The light stabilizer by ultraviolet absorbing agent, OCTA292 type light stabilizer, tea polyphenols composition, the mass ratio of three kinds of substances is ultraviolet absorbing agent: OCTA292: tea polyphenols=1: 2~5: 2~5.The sealant introduces complex type light stabilizer, which realizes effective compounding by structure optimization for ultraviolet absorber, light stabilizer and antioxidant, solves the problems, such as that color inhibition is used for a long time in sealant.Meanwhile the tea polyphenols type antioxidant of introducing also has the function of antibacterial and mouldproof.
Description
Technical field
The invention belongs to sealant technical fields, and in particular to a kind of electronic seal glue technology neck of the high transparency of environment-friendly type
Domain.
Background technique
LED encapsulation is the encapsulation to luminescence chip, has relatively big difference compared to integrated antenna package, the encapsulation of LED is not only wanted
Wick can be protected by asking, but also want can light transmission, so the encapsulation of LED proposes requirements at the higher level to light transmittance.In many LED
In sealant, using epoxy resin as the sealant of matrix, there is excellent leakproofness and higher adhesive strength, be widely used in space
The fields such as boat, electronics, machinery high vacuum, the sealing bonding of high-air-tightness part.However, how epoxy resin easily xanthochromia, press down
The xanthochromia of epoxy resin processed is the key that determine epoxy resin sealant service performance.
The main channel for usually inhibiting epoxy resin sealant yellow is to add ultraviolet light in the matrix of epoxy resin to inhale
Agent or antioxidant are received, such as: the anti-yellowing agent that patent CN2013101739069 is selected is UV-40 ultraviolet absorbing agent and V78-P
The compound of phosphite kind antioxidant；The light stabilizer that patent CN2017103873215 is used is 0.2-1 parts UV-1, UV-
9, at least one of UV-12, UV-531, DL616.However, these antioxidants are mainly commercial ready-made antioxidant or purple
Ultraviolet absorbers.Though certain resisting etiolation can be played the role of in use, due to antioxidant or ultraviolet absorbing agent
Cross-linked structure cannot be formed with resin matrix, will appear transport phenomena when used for a long time, and then sealant is made to turn yellow.
Summary of the invention
To solve the deficiencies in the prior art, the present invention provides a kind of epoxy resin sealant of modification, anti-by response type
The use of oxidant effectively inhibits the migration of antioxidant or ultraviolet absorbing agent, substantially increases the resistance to Huang of sealant
Become the time.
Specific research approach is as follows:
A kind of modified epoxy sealant, including two component of A, B: where component A mainly include 100 parts of epoxy resin,
5-12 parts of diluent, 0.3-5 parts of light stabilizer, 0.5-10 parts of coupling agent, 0.2-5 parts of dispersing agent；B component mainly includes curing agent
100 parts, 0.2-5 parts of toughener, 0.2-3 parts of coupling agent；
In component A:
The epoxy resin is bisphenol A type epoxy resin, bisphenol f type epoxy resin, cycloaliphatc glycidyl ester asphalt mixtures modified by epoxy resin
Rouge；
The diluent includes trihydroxymethylpropanyltri diglycidyl ether and C12-14The mixture of aliphatic glycidyl ether
The two mass ratio is 1:0.1-1；
The light stabilizer by ultraviolet absorbing agent, OCTA292 type light stabilizer, tea polyphenols composition, described three kinds
The mass ratio of substance is ultraviolet absorbing agent: OCTA292: tea polyphenols=1: 2~5: 2~5.
The further ultraviolet absorbing agent is 2-hydroxy-4-n-octoxybenzophenone (UV-531)；
The further OCTA292 is bis- (1,2,2,6,6- pentamethyl -4- piperidines) sebacates and 1- methyl -8-
The mixture of (1,2,2,6,6- pentamethyl -4- piperidines) sebacate, density 0.99g/cm3。
Content > 65% of ester catechin, the ester catechin of high level can make tea in the further tea polyphenols
Polyphenol is effectively compounded with ultraviolet absorber and light stabilizer, forms homogeneous system；
The dispersing agent is quaternary ammonium salt substance, specifically includes tetramethyl ammonium acetate, tetrabutyl ammonium acetate, tetrapropyl acetic acid
The mixture of one or more of ammonium；Dispersing agent can be such that light stabilizer is dispersed in resin matrix.
The coupling agent is silane coupling agent, including methyltrimethoxysilane, dimethyldimethoxysil,ne, vinyl
The mixture of one or more of trimethoxy silane, vinyltriethoxysilane, ethyl orthosilicate.
In B component:
The curing agent includes that methylhexahydrophthalic anhydride, phthalic anhydride, maleic anhydride, methyl receive enlightening
One of gram acid anhydrides or a variety of mixtures；
The toughener includes polypropylene glycol diglycidyl ether, bisphenol-A-alkylene oxide addition product 2-glycidyl
One of ether, linoleic acid dimer 2-glycidyl ester, hexanedioic acid 2-glycidyl ester or a variety of mixtures；
The coupling agent includes silane coupling agent, including methyltrimethoxysilane, dimethyldimethoxysil,ne, ethylene
The mixture of one or more of base trimethoxy silane, vinyltriethoxysilane, ethyl orthosilicate.
Sealant prepared by the present invention, introduces complex type light stabilizer, and the complex type light stabilizer is by UV absorption
Agent, light stabilizer and antioxidant realize effective compounding by structure optimization, and the use of the complex type light stabilizer is preferable
Solve the problems, such as that color inhibition is used for a long time in sealant.Meanwhile the tea polyphenols type antioxidant of introducing also has the function of antibacterial,
It can effectively solve the problems, such as that product goes mouldy when used for a long time in wet condition, product is more environmentally friendly.
The present invention also provides the preparation method of sealant, concrete scheme is as follows:
The preparation of A glue:
(1) preparation of light stabilizer: by ultraviolet absorbing agent, OCTA292 type light stabilizer, tea polyphenols by quality proportioning according to
It is secondary to be added in ethanol solution, slow evaporation solvent after dissolution is sufficiently stirred, evaporates while stirring, after being evaporated to no ethyl alcohol outflow
Obtain colorless viscous shape liquid, as complex type light stabilizer.
(2) epoxy resin, diluent, coupling agent, dispersing agent first the preparation of A glue: are added to the reaction kettle of high-speed stirred
In, temperature is increased after being sufficiently stirred to 50-70 DEG C, and complex type light stabilizer is then slowly added dropwise, continues to stir after being added dropwise
20-60min is reacted, cooling discharge obtains A glue.
The preparation of B glue: being added sequentially in stirred tank after curing agent, curing accelerator, toughener are prepared in mass ratio,
60-80 DEG C of whipping temp, the B glue that cools down to obtain quickly is stirred after 20-60min.
According to use environment, A glue, B glue using when proportion can be controlled in 5-3:1, solidification temperature is 90-120 DEG C, solidification
Time 2-10min.
Complex type light stabilizer is made by unique technique in sealant made from this preparation method, which will resist
Oxidisability, UV resistant irradiation and anti-mildew performance effectively increase the light transmittance and weatherability of sealant in one.Meanwhile
The quaternary ammonium salt dispersants used in the preparation process of A glue can be such that the viscosity of sealant reduces, and processing is more convenient, and is solidifying
When also act as the effect of curing accelerator, improve curing efficiency.
Specific embodiment
The principles and features of the present invention are described below, and illustrated embodiment is served only for explaining the present invention, is not intended to
It limits the scope of the invention.
Embodiment 1:
A kind of modified epoxy sealant, including two component of A, B: where component A mainly includes bisphenol A epoxide resin
(E44) 100 parts, trihydroxymethylpropanyltri diglycidyl ether and C12-14Aliphatic glycidyl ether mixture (mass ratio 1:
0.3) totally 8 parts, 2 parts of complex type light stabilizer, 3 parts of methyltrimethoxysilane, 1 part of tetramethyl ammonium acetate；B component mainly includes
100 parts of methylhexahydrophthalic anhydride, 2 parts of polypropylene glycol diglycidyl ether, 1 part of methyltrimethoxysilane；The light
Stabilizer is ultraviolet absorbing agent (UV-531): OCTA292: tea polyphenols=1: 2.5: 2.5, wherein the content of ester catechin
73%.The modified epoxy sealant the preparation method is as follows:
The preparation of A glue:
(1) ultraviolet absorbing agent, OCTA292 type light stabilizer, tea polyphenols the preparation of complex type light stabilizer: are pressed into quality
Proportion is added sequentially in ethanol solution, and the additional amount of ethyl alcohol is 5 times of three substance gross masses.After completely dissolution to three kinds of substances
Slow evaporation solvent, evaporates while stirring, and 60-75 DEG C of evaporating temperature is evaporated to after the outflow of no ethyl alcohol to obtain colorless viscous shape liquid,
As complex type light stabilizer.
(2) epoxy resin, diluent, coupling agent, dispersing agent first the preparation of A glue: are added to high-speed stirring by quality proportioning
Temperature is increased in the reaction kettle mixed, after being sufficiently stirred to 50-70 DEG C, and complex type light stabilizer is then slowly added dropwise, is added dropwise
After continue to be stirred to react 20-60min, cooling discharge obtains A glue.
The preparation of B glue: being added sequentially in stirred tank after curing agent, curing accelerator, toughener are prepared in mass ratio,
60-80 DEG C of whipping temp, the B glue that cools down to obtain quickly is stirred after 20-60min.
Embodiment 2:
A kind of modified epoxy sealant, including two component of A, B: where component A mainly includes bisphenol A epoxide resin
(E51) 100 parts, trihydroxymethylpropanyltri diglycidyl ether and C12-14Aliphatic glycidyl ether mixture (mass ratio 1:
0.3) totally 8 parts, 3 parts of complex type light stabilizer, 3.6 parts of methyltrimethoxysilane, 0.5 part of tetramethyl ammonium acetate；B component is main
Including 100 parts of phthalic anhydride, 2 parts of polypropylene glycol diglycidyl ether, 1 part of methyltrimethoxysilane；The light is stablized
Agent is ultraviolet absorbing agent (UV-531): OCTA292: tea polyphenols=1: 2.5: 2.5, wherein the content 73% of ester catechin.
The preparation method is the same as that of Example 1.
Embodiment 3:
A kind of modified epoxy sealant, including two component of A, B: where component A mainly includes bisphenol F epoxy resin
(NPEF-170) 100 parts, trihydroxymethylpropanyltri diglycidyl ether and C12-14Mixture (the mass ratio of aliphatic glycidyl ether
1:0.3) totally 9 parts, 3 parts of complex type light stabilizer, 3.6 parts of methyltrimethoxysilane, 0.5 part of tetrabutyl ammonium acetate；B component master
It to include 100 parts of methylhexahydrophthalic anhydride, 2 parts of polypropylene glycol diglycidyl ether, 1 part of methyltrimethoxysilane；
The light stabilizer is ultraviolet absorbing agent (UV-531): OCTA292: tea polyphenols=1: 2.5: 2.5, wherein ester catechin
Content 73%.The preparation method is the same as that of Example 1.
Embodiment 4:
A kind of modified epoxy sealant, including two component of A, B: where component A mainly includes cycloaliphatc glycidyl
100 parts of ester epoxy resin (CY184), trihydroxymethylpropanyltri diglycidyl ether and C12-14The mixture of aliphatic glycidyl ether
Totally 9 parts of (mass ratio 1:0.5), 3 parts of complex type light stabilizer, 3.6 parts of methyltrimethoxysilane, 0.5 part of tetrabutyl ammonium acetate；
B component mainly includes 100 parts of methylnadic anhydride, 2 parts of polypropylene glycol diglycidyl ether, 1 part of methyltrimethoxysilane；
The light stabilizer is ultraviolet absorbing agent (UV-531): OCTA292: tea polyphenols=1: 2: 3, wherein the content of ester catechin
65%.The preparation method is the same as that of Example 1.
Embodiment 5:
A kind of modified epoxy sealant, including two component of A, B: where component A mainly includes bisphenol A epoxide resin
(E44) 100 parts, trihydroxymethylpropanyltri diglycidyl ether and C12-14Aliphatic glycidyl ether mixture (mass ratio 1:
0.3) totally 8 parts, 2 parts of complex type light stabilizer, 6 parts of vinyltriethoxysilane, 1 part of tetrapropyl ammonium acetate；B component is mainly wrapped
Include 2 parts of methyl ethylene triethoxysilane；The light stabilizer is ultraviolet absorbing agent (UV-531): OCTA292: tea polyphenols
=1: 2.5: 2.5, the wherein content 73% of ester catechin.The preparation method is the same as that of Example 1.
Embodiment 6:
A kind of modified epoxy sealant, including two component of A, B: where component A mainly includes bisphenol A epoxide resin
(E51) 100 parts, trihydroxymethylpropanyltri diglycidyl ether and C12-14Aliphatic glycidyl ether mixture (mass ratio 1:
0.3) totally 8 parts, 2 parts of complex type light stabilizer, 4.7 parts of dimethyldimethoxysil,ne, 1 part of tetrapropyl ammonium acetate；B component is main
Including 2.3 parts of dimethyldimethoxysil,ne；The light stabilizer is ultraviolet absorbing agent (UV-531): OCTA292: tea polyphenols
=1: 2.5: 2.5, the wherein content 73%. of ester catechin
Comparative example 1:
A kind of modified epoxy sealant, including two component of A, B: where component A mainly includes bisphenol A epoxide resin
(E44) 100 parts, trihydroxymethylpropanyltri diglycidyl ether and C12-14Aliphatic glycidyl ether mixture (mass ratio 1:
0.3) totally 8 parts, ultraviolet absorbing agent ultraviolet absorbing agent UV-40 (0.4 part), antioxidant 1010 (1 part), methyl trimethoxy oxygroup silicon
3 parts of alkane；B component mainly includes 100 parts of methylhexahydrophthalic anhydride, 2 parts of polypropylene glycol diglycidyl ether, methyl trimethoxy
1 part of oxysilane, 2 parts of diethylenetriamine curing accelerator.The preparation method is as follows:
The preparation of A glue: by formula sequentially add bisphenol A type epoxy resin E44, trihydroxymethylpropanyltri diglycidyl ether,
C12-14Aliphatic glycidyl ether diluent, ultraviolet absorbing agent UV-40, antioxidant 1010, methyltrimethoxysilane, high speed
Disperse 30min, 60 DEG C of dispersion temperature, cooling discharge obtains A glue after dispersion；
The preparation of B glue: by methylhexahydrophthalic anhydride, polypropylene glycol diglycidyl ether, methyl trimethoxy oxygroup silicon
Alkane, diethylenetriamine are matched in mass ratio to be added sequentially in stirred tank, 70 DEG C of whipping temp, is dropped after being quickly stirred 30min
It is warm to obtain B glue.
Comparative example 2:
A kind of modified epoxy sealant, including two component of A, B: where component A mainly includes cycloaliphatc glycidyl
100 parts of ester epoxy resin (CY184), trihydroxymethylpropanyltri diglycidyl ether and C12-14The mixture of aliphatic glycidyl ether
Totally 9 parts of (mass ratio 1:0.5), UV-40 (0.4 part), antioxidant 1010 (1 part), 3.6 parts of methyltrimethoxysilane；B component master
It to include 100 parts of methylnadic anhydride, 2 parts of polypropylene glycol diglycidyl ether, 1 part of methyltrimethoxysilane.Preparation side
Method is the same as comparative example 1.
After being mixed to above-described embodiment and comparative example by different ratio, glue cake is made in solidification, tests its draftability respectively
Energy, UV resistant performance and anti-microbial property.Wherein the test of tensile property using GB/T 1040-2006 " plastic tensile performance
Test ", ultraviolet light performance uses wavelength for 365nm, intensity 30mW/cm2Ultraviolet light 2h, then test
Light transmittance attenuation at 465 and 400nm, anti-microbial property test use GB/T 31402-2015 " frosting anti-microbial property
Test method ".
Concrete outcome is as follows:
Each embodiment performance of table 1. compares
By above data as it can be seen that the complex type light stabilizer condition of cure that uses of the present invention is mild, there is preferable resistance to Huang
Change and antibacterial effect, and mechanical property is more excellent.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of modified epoxy sealant, including two component of A, B: where component A mainly includes 100 parts of epoxy resin, dilute
Release 5-12 parts of agent, 0.3-5 parts of light stabilizer, 0.5-10 parts of coupling agent, 0.2-5 parts of dispersing agent；B component mainly includes curing agent
100 parts, 0.2-5 parts of toughener, 0.2-3 parts of coupling agent；The light stabilizer is stablized by ultraviolet absorbing agent, OCTA292 type light
Agent, tea polyphenols composition, the mass ratio of three kinds of substances is ultraviolet absorbing agent: OCTA292: tea polyphenols=1: 2~5:
2~5.
2. a kind of modified epoxy sealant according to claim 1, it is characterised in that in component A:
The epoxy resin is bisphenol A type epoxy resin, bisphenol f type epoxy resin, cycloaliphatc glycidyl ester epoxy resin；
The diluent includes trihydroxymethylpropanyltri diglycidyl ether and C12-14Both mixtures of aliphatic glycidyl ether
Mass ratio is 1:0.1-1；
The ultraviolet absorbing agent is 2-hydroxy-4-n-octoxybenzophenone (UV-531)
The OCTA292 is bis- (1,2,2,6,6- pentamethyl -4- piperidines) sebacates and 1- methyl -8- (1,2,2,6,6- five
Methyl -4- piperidines) sebacate mixture, density 0.99g/cm3；
Content > 65% of ester catechin in the tea polyphenols；
The dispersing agent is quaternary ammonium salt substance, specifically includes tetramethyl ammonium acetate, tetrabutyl ammonium acetate, in tetrapropyl ammonium acetate
One or more of mixtures；Dispersing agent can be such that light stabilizer is dispersed in resin matrix；
The coupling agent is silane coupling agent, including methyltrimethoxysilane, dimethyldimethoxysil,ne, vinyl front three
The mixture of one or more of oxysilane, vinyltriethoxysilane, ethyl orthosilicate.
3. a kind of modified epoxy sealant according to claim 1, it is characterised in that in B component: the curing agent
Including one of methylhexahydrophthalic anhydride, phthalic anhydride, maleic anhydride, methylnadic anhydride or more
The mixture of kind；
The toughener includes polypropylene glycol diglycidyl ether, bisphenol-A-alkylene oxide addition product diglycidyl ether, Asia
One of oleic acid dimer 2-glycidyl ester, hexanedioic acid 2-glycidyl ester or a variety of mixtures；
The coupling agent includes silane coupling agent, including methyltrimethoxysilane, dimethyldimethoxysil,ne, vinyl three
The mixture of one or more of methoxy silane, vinyltriethoxysilane, ethyl orthosilicate.
4. preparation requires modified epoxy sealant described in any one of 1-3 entirely, include the following steps:
(1) preparation of light stabilizer: ultraviolet absorbing agent, OCTA292 type light stabilizer, tea polyphenols are successively added by quality proportioning
Enter into ethanol solution, slow evaporation solvent after dissolution is sufficiently stirred, evaporates while stirring, obtains nothing after being evaporated to no ethyl alcohol outflow
Color viscous liquid, as complex type light stabilizer.
(2) preparation of A glue: first epoxy resin, diluent, coupling agent, dispersing agent are added in the reaction kettle of high-speed stirred, filled
Temperature is increased to 50-70 DEG C after dividing stirring, and complex type light stabilizer is then slowly added dropwise, continues to be stirred to react after being added dropwise
20-60min, cooling discharge obtain A glue.
(3) preparation of B glue: being added sequentially in stirred tank after curing agent, curing accelerator, toughener are prepared in mass ratio,
60-80 DEG C of whipping temp, the B glue that cools down to obtain quickly is stirred after 20-60min.
5. the preparation method of sealant according to claim 4, which is characterized in that the additional amount of ethyl alcohol is in step (1)
5 times of ultraviolet absorbing agent, OCTA292 type light stabilizer and tea polyphenols gross mass.
6. the preparation method of sealant according to claim 4, which is characterized in that the evaporating temperature of ethyl alcohol in step (1)
It is 60-75 DEG C.
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Denomination of invention: A modified epoxy resin sealant and its preparation method Granted publication date: 20210409 Pledgee: Agricultural Bank of China Tongling Branch Pledgor: SHANGHAI KAIJIN NEW MATERIAL TECHNOLOGY CO.,LTD. Registration number: Y2024980017937 |