CN116925686A - Silane modified bi-component flame retardant adhesive and preparation method thereof - Google Patents
Silane modified bi-component flame retardant adhesive and preparation method thereof Download PDFInfo
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- CN116925686A CN116925686A CN202310931925.7A CN202310931925A CN116925686A CN 116925686 A CN116925686 A CN 116925686A CN 202310931925 A CN202310931925 A CN 202310931925A CN 116925686 A CN116925686 A CN 116925686A
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- China
- Prior art keywords
- epoxy resin
- parts
- flame retardant
- component
- modified
- 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.)
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 131
- 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 130
- 238000002360 preparation method Methods 0.000 title claims abstract description 56
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 41
- 239000000853 adhesive Substances 0.000 title claims abstract description 40
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 13
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 13
- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 109
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims abstract description 109
- 229920001276 ammonium polyphosphate Polymers 0.000 claims abstract description 109
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 67
- 239000004593 Epoxy Substances 0.000 claims abstract description 59
- 239000003094 microcapsule Substances 0.000 claims abstract description 56
- 239000003822 epoxy resin Substances 0.000 claims abstract description 54
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 54
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 32
- 239000000945 filler Substances 0.000 claims abstract description 25
- 239000004014 plasticizer Substances 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000004526 silane-modified polyether Substances 0.000 claims abstract description 18
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 239000004611 light stabiliser Substances 0.000 claims abstract description 6
- 239000002516 radical scavenger Substances 0.000 claims abstract description 6
- 239000013008 thixotropic agent Substances 0.000 claims abstract description 6
- 239000002250 absorbent Substances 0.000 claims abstract description 3
- 230000002745 absorbent Effects 0.000 claims abstract description 3
- 238000001723 curing Methods 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 18
- 238000002156 mixing Methods 0.000 claims description 13
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- 239000003054 catalyst Substances 0.000 claims description 8
- 239000002270 dispersing agent Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- -1 glycidyl ester Chemical class 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000000376 reactant Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 238000000967 suction filtration Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- 229910019142 PO4 Inorganic materials 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000010452 phosphate Substances 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 229960001124 trientine Drugs 0.000 claims description 4
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 3
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 235000019830 sodium polyphosphate Nutrition 0.000 claims description 3
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 claims description 3
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 3
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims description 3
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 2
- SPAUYKHQVLTCOL-UHFFFAOYSA-N C1(=CC=CC=C1)OP(OC1=CC=CC=C1)(O)=O.C1(=CC=CC=C1)C Chemical compound C1(=CC=CC=C1)OP(OC1=CC=CC=C1)(O)=O.C1(=CC=CC=C1)C SPAUYKHQVLTCOL-UHFFFAOYSA-N 0.000 claims description 2
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- ZCLVNIZJEKLGFA-UHFFFAOYSA-H bis(4,5-dioxo-1,3,2-dioxalumolan-2-yl) oxalate Chemical compound [Al+3].[Al+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZCLVNIZJEKLGFA-UHFFFAOYSA-H 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 239000010439 graphite Substances 0.000 claims description 2
- 229910002804 graphite Inorganic materials 0.000 claims description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 2
- 239000000347 magnesium hydroxide Substances 0.000 claims description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 2
- 150000008442 polyphenolic compounds Chemical class 0.000 claims description 2
- 235000013824 polyphenols Nutrition 0.000 claims description 2
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 claims description 2
- WTLBZVNBAKMVDP-UHFFFAOYSA-N tris(2-butoxyethyl) phosphate Chemical compound CCCCOCCOP(=O)(OCCOCCCC)OCCOCCCC WTLBZVNBAKMVDP-UHFFFAOYSA-N 0.000 claims description 2
- HQUQLFOMPYWACS-UHFFFAOYSA-N tris(2-chloroethyl) phosphate Chemical compound ClCCOP(=O)(OCCCl)OCCCl HQUQLFOMPYWACS-UHFFFAOYSA-N 0.000 claims description 2
- GTRSAMFYSUBAGN-UHFFFAOYSA-N tris(2-chloropropyl) phosphate Chemical compound CC(Cl)COP(=O)(OCC(C)Cl)OCC(C)Cl GTRSAMFYSUBAGN-UHFFFAOYSA-N 0.000 claims description 2
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 2
- 229960001763 zinc sulfate Drugs 0.000 claims description 2
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims 2
- AFEQENGXSMURHA-UHFFFAOYSA-N oxiran-2-ylmethanamine Chemical compound NCC1CO1 AFEQENGXSMURHA-UHFFFAOYSA-N 0.000 claims 1
- 230000005012 migration Effects 0.000 abstract description 15
- 238000013508 migration Methods 0.000 abstract description 15
- 230000000052 comparative effect Effects 0.000 description 26
- 239000000565 sealant Substances 0.000 description 24
- 238000001556 precipitation Methods 0.000 description 15
- 238000002485 combustion reaction Methods 0.000 description 13
- 230000000694 effects Effects 0.000 description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 9
- 238000004132 cross linking Methods 0.000 description 9
- 239000010410 layer Substances 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 9
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 8
- 239000011247 coating layer Substances 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- 239000004721 Polyphenylene oxide Substances 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 229910052698 phosphorus Inorganic materials 0.000 description 6
- 239000011574 phosphorus Substances 0.000 description 6
- 229920000570 polyether Polymers 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229920000742 Cotton Polymers 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 4
- 230000004888 barrier function Effects 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229940116351 sebacate Drugs 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 2
- MCPKSFINULVDNX-UHFFFAOYSA-N drometrizole Chemical compound CC1=CC=C(O)C(N2N=C3C=CC=CC3=N2)=C1 MCPKSFINULVDNX-UHFFFAOYSA-N 0.000 description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-L sebacate(2-) Chemical compound [O-]C(=O)CCCCCCCCC([O-])=O CXMXRPHRNRROMY-UHFFFAOYSA-L 0.000 description 2
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-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
- UVDDHYAAWVNATK-VGKOASNMSA-L (z)-4-[dibutyl-[(z)-4-oxopent-2-en-2-yl]oxystannyl]oxypent-3-en-2-one Chemical compound CC(=O)\C=C(C)/O[Sn](CCCC)(CCCC)O\C(C)=C/C(C)=O UVDDHYAAWVNATK-VGKOASNMSA-L 0.000 description 1
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 1
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- LDXJRKWFNNFDSA-UHFFFAOYSA-N 2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound C1CN(CC2=NNN=C21)CC(=O)N3CCN(CC3)C4=CN=C(N=C4)NCC5=CC(=CC=C5)OC(F)(F)F LDXJRKWFNNFDSA-UHFFFAOYSA-N 0.000 description 1
- FUIQBJHUESBZNU-UHFFFAOYSA-N 2-[(dimethylazaniumyl)methyl]phenolate Chemical compound CN(C)CC1=CC=CC=C1O FUIQBJHUESBZNU-UHFFFAOYSA-N 0.000 description 1
- GTEXIOINCJRBIO-UHFFFAOYSA-N 2-[2-(dimethylamino)ethoxy]-n,n-dimethylethanamine Chemical compound CN(C)CCOCCN(C)C GTEXIOINCJRBIO-UHFFFAOYSA-N 0.000 description 1
- JQMFQLVAJGZSQS-UHFFFAOYSA-N 2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]-N-(2-oxo-3H-1,3-benzoxazol-6-yl)acetamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)NC1=CC2=C(NC(O2)=O)C=C1 JQMFQLVAJGZSQS-UHFFFAOYSA-N 0.000 description 1
- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-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
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 1
- LVACOMKKELLCHJ-UHFFFAOYSA-N 3-trimethoxysilylpropylurea Chemical compound CO[Si](OC)(OC)CCCNC(N)=O LVACOMKKELLCHJ-UHFFFAOYSA-N 0.000 description 1
- UWSMKYBKUPAEJQ-UHFFFAOYSA-N 5-Chloro-2-(3,5-di-tert-butyl-2-hydroxyphenyl)-2H-benzotriazole Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC(N2N=C3C=C(Cl)C=CC3=N2)=C1O UWSMKYBKUPAEJQ-UHFFFAOYSA-N 0.000 description 1
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- DJEQZVQFEPKLOY-UHFFFAOYSA-N N,N-dimethylbutylamine Chemical compound CCCCN(C)C DJEQZVQFEPKLOY-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229920000388 Polyphosphate Polymers 0.000 description 1
- FDLQZKYLHJJBHD-UHFFFAOYSA-N [3-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC(CN)=C1 FDLQZKYLHJJBHD-UHFFFAOYSA-N 0.000 description 1
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
- YHEPZZFDBQOSSN-UHFFFAOYSA-N bis(1,2,2,6,6-pentamethylpiperidin-4-yl) decanedioate;1-o-methyl 10-o-(1,2,2,6,6-pentamethylpiperidin-4-yl) decanedioate Chemical compound COC(=O)CCCCCCCCC(=O)OC1CC(C)(C)N(C)C(C)(C)C1.C1C(C)(C)N(C)C(C)(C)CC1OC(=O)CCCCCCCCC(=O)OC1CC(C)(C)N(C)C(C)(C)C1 YHEPZZFDBQOSSN-UHFFFAOYSA-N 0.000 description 1
- 239000004841 bisphenol A epoxy resin Substances 0.000 description 1
- 239000004842 bisphenol F epoxy resin Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- OCWYEMOEOGEQAN-UHFFFAOYSA-N bumetrizole Chemical compound CC(C)(C)C1=CC(C)=CC(N2N=C3C=C(Cl)C=CC3=N2)=C1O OCWYEMOEOGEQAN-UHFFFAOYSA-N 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
- 235000019438 castor oil Nutrition 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000009841 combustion method Methods 0.000 description 1
- DDSWIYVVHBOISO-UHFFFAOYSA-N ctk0i1982 Chemical compound N[SiH](N)N DDSWIYVVHBOISO-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- AYOHIQLKSOJJQH-UHFFFAOYSA-N dibutyltin Chemical compound CCCC[Sn]CCCC AYOHIQLKSOJJQH-UHFFFAOYSA-N 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- JKGITWJSGDFJKO-UHFFFAOYSA-N ethoxy(trihydroxy)silane Chemical group CCO[Si](O)(O)O JKGITWJSGDFJKO-UHFFFAOYSA-N 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 239000004845 glycidylamine epoxy resin Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012796 inorganic flame retardant Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000013008 moisture curing Methods 0.000 description 1
- NHLUVTZJQOJKCC-UHFFFAOYSA-N n,n-dimethylhexadecan-1-amine Chemical compound CCCCCCCCCCCCCCCCN(C)C NHLUVTZJQOJKCC-UHFFFAOYSA-N 0.000 description 1
- VZUGBLTVBZJZOE-KRWDZBQOSA-N n-[3-[(4s)-2-amino-1,4-dimethyl-6-oxo-5h-pyrimidin-4-yl]phenyl]-5-chloropyrimidine-2-carboxamide Chemical compound N1=C(N)N(C)C(=O)C[C@@]1(C)C1=CC=CC(NC(=O)C=2N=CC(Cl)=CN=2)=C1 VZUGBLTVBZJZOE-KRWDZBQOSA-N 0.000 description 1
- GLTDLAUASUFHNK-UHFFFAOYSA-N n-silylaniline Chemical compound [SiH3]NC1=CC=CC=C1 GLTDLAUASUFHNK-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 239000004588 polyurethane sealant Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000004590 silicone sealant Substances 0.000 description 1
- 125000004469 siloxy group Chemical group [SiH3]O* 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
Classifications
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- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- 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
- C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- 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
Abstract
The application discloses a silane modified bi-component flame retardant adhesive and a preparation method thereof, wherein the flame retardant adhesive comprises a component A and a component B, and the component A comprises 200-400 parts of silane modified polyether, 100-200 parts of flame retardant plasticizer, 1-400 parts of filler, 3-10 parts of ultraviolet absorbent, 3-10 parts of light stabilizer, 15-35 parts of thixotropic agent, 30-50 parts of silane coupling agent, 10-40 parts of first curing agent, 10-20 parts of curing accelerator and 5-15 parts of water scavenger; the component B comprises 300 to 500 parts of epoxy resin, 1 to 350 parts of filler, 2 to 150 parts of filler, 250 to 350 parts of flame retardant plasticizer, 5 to 15 parts of deionized water and 20 to 40 parts of second curing agent, wherein the filler 2 is epoxy resin-SiO 2 Microcapsule modified ammonium polyphosphate, and modified ammonium polyphosphate is flame-retardantThe efficiency is increased, the compatibility is improved, and the migration resistance of the flame retardant adhesive is improved.
Description
Technical Field
The application relates to the field of silane modified sealants, in particular to a silane modified bi-component flame retardant adhesive and a preparation method thereof.
Background
The silane modified sealant has the advantages of both silicone sealant and polyurethane sealant, has the characteristics of wide adhesiveness, low VOC emission and the like, and is widely applied to various industrial fields. However, the flame retardant property of the sealant is poor, the sealant is easy to burn under open fire or high temperature, and the comprehensive performance of the single-component sealant can not meet all process requirements along with the continuous improvement of the flame retardant requirement of products and the continuous acceleration of production beats.
Therefore, the two-component sealant with flame retardant property receives more and more attention in the market, the inorganic phosphorus flame retardant or the organic phosphorus flame retardant is usually added into the flame retardant sealant, the addition amount of the flame retardant is generally large in order to enhance the flame retardant efficiency, the mechanical property of the flame retardant sealant is obviously reduced when the addition amount is increased, and the problems of unsatisfactory compatibility, high volatility, combustion dripping and the like of the phosphorus flame retardant are also caused.
Disclosure of Invention
The application provides a silane modified bi-component flame retardant adhesive and a preparation method thereof, aiming at solving the problems that the flame retardant effect of the flame retardant sealant is poor, the strength is reduced due to large addition amount of a flame retardant, the compatibility of the flame retardant in the sealant is poor, the flame retardant is easy to volatilize and separate out, and the like.
In a first aspect, the application provides a silane modified bi-component flame retardant adhesive, which comprises an A component and a B component, wherein the A component and the B component comprise the following raw materials in parts by weight:
and (3) a component A:
200-400 parts of silane modified polyether;
100-200 parts of flame retardant plasticizer;
1-400 parts of filler;
3-10 parts of ultraviolet absorber;
3-10 parts of light stabilizer;
15-35 parts of thixotropic agent;
30-50 parts of silane coupling agent;
10-40 parts of a first curing agent;
10-20 parts of a curing accelerator;
5-15 parts of a water scavenger;
and the component B comprises the following components:
300-500 parts of epoxy resin;
1-350 parts of filler;
150-250 parts of filler;
250-350 parts of flame retardant plasticizer;
deionized water 5-15;
20-40 parts of a second curing agent;
the filler 2 is epoxy resin-SiO 2 Microcapsule modified ammonium polyphosphate.
Preferably, the epoxy resin comprises one or a combination of a plurality of bisphenol A epoxy resin, bisphenol F epoxy resin, polyphenol glycidyl ether epoxy resin, aliphatic glycidyl ether epoxy resin, glycidyl ester epoxy resin and glycidyl amine epoxy resin.
Preferably, the ultraviolet absorber comprises one or a combination of several of 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole, 2- (2 '-hydroxy-3' -tert-butyl-5 '-methylphenyl) -5-chlorobenzotriazole and 2- (2' -hydroxy-3 ',5' -di-tert-butylphenyl) -5-chlorobenzotriazole.
Preferably, the method comprises the steps of, the light stabilizer comprises bis-2, 6-tetramethyl piperidinol sebacate, bis (1, 2, 6-pentamethyl piperidinol sebacate) a combination of one or more of bis (1, 2, 6-pentamethyl-4-piperidine) sebacate and 1-methyl-8- (1, 2, 6-pentamethyl-4-piperidine) sebacate.
Preferably, the thixotropic agent comprises one or a combination of several of polyamide wax, hydrogenated castor oil, fumed silica.
Preferably, the silane coupling agent comprises one or a combination of a plurality of gamma-aminopropyl trimethoxysilane, gamma-aminopropyl triethoxysilane, N-beta- (aminoethyl) -gamma-aminopropyl trimethoxysilane, phenylamino-silane, triamino silane, gamma-mercaptopropyl trimethoxysilane, gamma-ureido propyl trimethoxysilane and gamma-ureido propyl trihexyloxy silane, gamma-methacryloxypropyl trimethoxysilane and gamma-glycidyl ether propyl trimethoxysilane.
Preferably, the first curing agent comprises one or a combination of more than one of ethylenediamine, diethylenetriamine, polyethylene polyamine, m-phenylenediamine, m-xylylenediamine, amine addition curing agent and phenol amino alcohol curing agent.
Preferably, the curing accelerator comprises one or a combination of several of 2,4, 6-tri (dimethylaminomethyl) phenol, triethylamine, triethanolamine, benzyl dimethylamine, 1, 8-diaza [5,4,0] undecene-7, o-hydroxybenzyl dimethylamine.
Preferably, the water scavenger comprises one or a combination of several of vinyl trimethoxy silane and vinyl triethoxy silane.
Preferably, the second curing agent comprises one or more of dibutyl tin bis (acetylacetonate) and dibutyl tin laurate.
Preferably, the volume ratio of the component A to the component B is 1: (1-5).
By adopting the technical scheme, the silane modified polyether in the component A takes polyether as a long chain, the silane modified polyether sealant is blocked by siloxy groups, a network structure which takes a silicon-oxygen bond as a crosslinking point and is connected with a flexible polyether long chain is formed by room temperature moisture curing, the cohesive energy of the polyether is lower, the strength is not high due to the nonpolar structure of the polyether, a sea-island structure is formed by mixing the silane modified polyether with the epoxy resin in the component B, the epoxy resin is distributed in the silane modified polyether, the high strength after self curing and the high adhesive property to a base material enable the performance of the integral flame retardant adhesive to be more stable, the defect that the strength of the polyether is insufficient can be overcome, and the flame retardant sealant with excellent physical and chemical properties is obtained.
Preferably, the flame retardant plasticizer comprises one or a combination of more of tri (2-chloroethyl) phosphate, tri (2-chloropropyl) phosphate, triethyl phosphate, triphenyl phosphate, tri (1, 3-dichloroisopropyl) phosphate, tributoxyethyl phosphate and toluene diphenyl phosphate.
Preferably, the filler 1 comprises one or a combination of several of aluminum hydroxide, magnesium hydroxide, expanded graphite, borate, aluminum oxalate and zinc sulfate.
Through adopting above-mentioned technical scheme, fire-retardant plasticizer is phosphate organic phosphorus flame retardant, through the overburden that produces by phosphoric acid plays the effect of coverage and isolated the contact of high heat and combustible gas when burning, the polymetaphosphoric acid of production is strong acid simultaneously, as powerful dehydrating agent, can make polymer dehydration carbonization, especially contains oxygen-containing group in silane modified polyether and the epoxy, and the organic flame retardant of adding phosphate can make flame retardant effect more showing. Meanwhile, the filler 1 can be used as a flame-retardant synergist, has high stability, can play a role in durable burning resistance, is matched with an organic phosphorus flame retardant, can enhance the flame-retardant effect, and can not influence the mechanical property of the obtained flame-retardant adhesive.
Preferably, the epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate comprises the following raw materials in percentage by mass (0.1-0.3): 0.15 to 0.25 of epoxy resin of 1, tetraethoxysilane and ammonium polyphosphate.
Preferably, the epoxy resin is bisphenol a type epoxy resin, and the epoxy value of the epoxy resin is 0.4-0.54.
Preferably, the ammonium polyphosphate is a long chain ammonium polyphosphate of type II.
The ammonium polyphosphate is an efficient inorganic flame retardant, the decomposition temperature is high, phosphoric acid generated by decomposition can be covered on the surface of the heat insulation layer in the combustion process, and the phosphoric acid and the polymer form a carbonization layer together, so that the heat insulation effect is achieved, the supply of oxygen is reduced, and the continuous combustion is prevented. In the combustion process, ammonium polyphosphate can also generate inert gases such as ammonia gas, so that the concentration of the combustible gas can be greatly diluted, the gas-phase flame retardant effect is achieved, and nitrogen contained in the ammonium polyphosphate can also be rapidly decomposed to absorb a large amount of heat. However, the ammonium polyphosphate is used as an acid source, and part of the ammonium polyphosphate and the filler in the flame retardant adhesive are subjected to esterification reaction, so that the formation of a carbon layer in the combustion process is destroyed, and the flame retardant efficiency is reduced. Meanwhile, ammonium polyphosphate has poor migration resistance and water resistance, and can be separated out to the surface or react with water after a period of time, so that the flame retardant glue can lose flame retardant effect after the ammonium polyphosphate absorbs moisture.
By adopting the technical scheme, the epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate can protect the ammonium polyphosphate from losing flame retardant effect due to reaction with hydroxyl groups on the surface of filler in a system, and epoxy resin-SiO (SiO) 2 The coating layer of the microcapsule can effectively inhibit the ammonium polyphosphate from contacting with water and reacting. The epoxy resin on the surface of the ammonium polyphosphate can increase the compatibility of the ammonium polyphosphate and the polymer and improve the migration resistance of the ammonium polyphosphate. SiO (SiO) 2 The nano particles are covered on the surface of the ammonium polyphosphate, a remarkable inorganic barrier can be generated in the combustion process, the ammonium polyphosphate is prevented from being degraded, the thickness and the mechanical strength of the carbon layer are further increased, and the epoxy resin coating layer can increase the thermal stability of the ammonium polyphosphate. The synergistic effect between the phosphorus-containing flame retardant and the silicon-containing compound can effectively prevent fire and isolate flame from spreading, and effectively improve the flame retardant efficiency.
And, epoxy resin-SiO 2 The epoxy resin on the surface of the microcapsule modified ammonium polyphosphate can be crosslinked with silane modified polyether in the middle of the component A to form a crosslinked network structure, so that on one hand, the ammonium polyphosphate flame retardant is not easy to separate out to the surface of the flame retardant adhesive, on the other hand, the crosslinking density of the flame retardant adhesive is increased, the flame retardant plasticizer in the component A and the flame retardant plasticizer in the component B are easy to volatilize, and are easy to drip after burning, and dripping flame and burning substances can possibly cause secondary ignition, so that the volatilization of the flame retardant plasticizer can be effectively inhibited by increasing the crosslinking density in the flame retardant adhesive, and meanwhile, the density of the flame retardant adhesive is enhanced, and the phenomenon of dripping cotton burning is not easy to occur in the burning process.
Preferably, epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate is prepared by the following steps:
s1, adding distilled water into a solvent, uniformly mixing, adding sodium polyphosphate, a dispersing agent and a catalyst 1, stirring and mixing for 15-20 min at 35-45 ℃, then adding tetraethoxysilane, reacting for 3-5 h at 40-50 ℃, and then carrying out suction filtration, washing and drying to obtain a modified ammonium polyphosphate pre-reactant;
s2, sequentially adding epoxy resin, a curing agent, a modified ammonium polyphosphate pre-reactant, a dispersing agent and a catalyst 2 into a solvent, stirring and dispersing for 20-40 min, heating the solution to 80-90 ℃, stirring and reacting for 2-3 h, and performing suction filtration, washing and drying after the reaction is finished to obtain the epoxy resin-SiO 2 Microcapsule modified ammonium polyphosphate.
Preferably, the dispersing agent comprises one or a combination of a plurality of sodium dodecyl sulfate and sodium dodecyl benzene sulfonate; the curing agent comprises one or a combination of more of triethylene tetramine, ethylenediamine, diethylenetriamine, tetraethylenepentamine, m-phenylenediamine and m-xylylene.
Preferably, the solvent comprises one or more of absolute ethanol and methanol.
Preferably, the catalyst 1 is ammonia water; the catalyst 2 is one or a combination of a plurality of N, N-dimethyl cyclohexane, bis (2-dimethylaminoethyl) ether, triethylenediamine, N, N, N ', N' -tetramethyl alkylene diamine, N, N, N ', N' -pentamethyl diethylenetriamine, triethylamine, N, N-dimethyl benzylamine, N, N-dimethyl hexadecylamine and N, N-dimethyl butylamine.
Preferably, the addition amount of the dispersing agent is 0.5-2.5% of the mass of the ammonium polyphosphate, and the addition amount of the curing agent is 5-20% of the mass of the epoxy resin.
Preferably, the mass ratio of the solvent to the ammonium polyphosphate in the step S1 is (2.5 to 3.5): 1, a step of; in the S2 step, the mass ratio of the solvent to the modified ammonium polyphosphate pre-reactant is (2-2.8): 1.
preferably, the addition amount of the catalyst 1 is 35-45% of the mass of the ammonium polyphosphate; the addition amount of the catalyst 2 is 1-2% of the mass of the modified ammonium polyphosphate pre-reactant.
By adopting the technical scheme, the ethyl orthosilicate forms a layer of nano silicon dioxide coating layer on the surface of the ammonium polyphosphate, and the nano silicon dioxide coating layer is used as an inorganic barrier, so that on one hand, the degradation of the polyphosphate can be inhibited in the combustion process, and on the other hand, the thickness of the carbon layer can be increased, and the flame retardant effect is improved. And then coating a layer of epoxy resin on the surface, wherein the epoxy resin has good compatibility with the base material, and can form a crosslinked network structure with silane modified polyether, so that the compactness of the flame retardant adhesive is increased, and the precipitation of the flame retardant and the occurrence of dripping phenomenon after combustion are inhibited.
In a second aspect, the application also provides a preparation method of the silane modified bi-component flame retardant adhesive, which comprises the following steps:
and (3) preparation of the component A: mixing silane modified polyether, flame retardant plasticizer, filler 1, ultraviolet absorbent, light stabilizer and thixotropic agent, stirring at a speed of 1000-1200 rpm under a vacuum condition of 90-100 ℃ for 0.5-1 h, cooling to 40-50 ℃, adding silane coupling agent, first curing agent, curing accelerator and water scavenger, and stirring uniformly to obtain a component A; and (3) preparation of a component B: and uniformly stirring and mixing the epoxy resin, the filler 1, the filler 2, the flame-retardant plasticizer, the deionized water and the second curing agent under a vacuum condition to obtain the component B.
Preferably, the vacuum degree is-0.09 to-0.1 Mpa under the vacuum condition.
In summary, the application has the following beneficial effects:
1. the silane modified polyether contained in the component A can form an island structure with the epoxy resin in the component B, the high strength of the epoxy resin can overcome the problem of insufficient cohesive energy low strength caused by a nonpolar structure of the polyether, and the performance of the flame-retardant sealant and the bonding performance with a base material are enhanced.
2. The component B of the application is added with epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate, the ammonium polyphosphate and the flame retardant plasticizer existing in the system can form a phosphoric acid coating layer in the combustion process, can effectively isolate heat and reduce oxygen supply, and the generated ammonia gas is inert gas to play a role in gas-phase flame retardance, and passes through epoxy resin-SiO 2 Further modification of the microcapsules can increase the compatibility of ammonium polyphosphate with polymers on the one hand and the coating layer can be provided withEffectively inhibit the ammonium polyphosphate from directly contacting with water, losing flame retardance after moisture absorption, and can increase the migration resistance of sodium polyphosphate; on the other hand, the silicon dioxide contained in the coating layer can form a remarkable inorganic barrier in the combustion process while playing a role of blocking and protecting, and a carbon layer is formed on the surface to enhance the flame retardant efficiency.
3. Epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate can be cross-linked with silane modified polyether in the component A to form a reticular structure, so that volatilization of the flame-retardant plasticizer and precipitation of the ammonium polyphosphate can be effectively inhibited, and combustion dripping phenomenon caused by the flame-retardant plasticizer can be effectively inhibited after the compactness of the flame-retardant sealant is increased through the cross-linking effect, and secondary ignition is prevented.
Detailed Description
Epoxy resin-SiO 2 Preparation example of microcapsule modified ammonium polyphosphate
Preparation example 1, an epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate is prepared by the following method:
s1, adding 100g of distilled water into 300g of absolute ethyl alcohol, uniformly mixing, adding 100g of ammonium polyphosphate (the ammonium polyphosphate is II-type long-chain ammonium polyphosphate, the average polymerization degree is 1500), 2g of sodium dodecyl sulfate and 40g of ammonia water, stirring and mixing for 20min at 40 ℃, adding 20g of tetraethoxysilane, reacting for 4h at 50 ℃, and carrying out suction filtration, washing and drying to obtain a modified ammonium polyphosphate pre-reactant;
s2, sequentially adding 20g of epoxy resin E51 (with an epoxy value of 0.48-0.54), 2g of triethylene tetramine, 100g of modified ammonium polyphosphate prerectant, 1g of sodium dodecyl benzene sulfonate and 2g of N, N-dimethyl cyclohexane into 240g of absolute ethyl alcohol, stirring and dispersing for 30min, heating the solution to 90 ℃, stirring and reacting for 3h, and filtering, washing and drying after the reaction is finished to obtain the epoxy resin-SiO 2 Microcapsule modified ammonium polyphosphate.
Preparation example 2, an epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate was different from preparation example 1 only in that the amount of ethyl orthosilicate added was 10g.
Preparation example 3, an epoxy resin-SiO 2 MicrogelThe capsule modified ammonium polyphosphate differed from preparation example 1 only in that the amount of ethyl orthosilicate added was 30g.
Preparation example 4, an epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate was different from preparation example 1 only in that the addition amount of the epoxy resin E51 was 15g.
Preparation example 5, an epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate was different from preparation example 1 only in that the addition amount of the epoxy resin E51 was 25g.
Preparation example 6, an epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate was different from preparation example 1 only in that the amount of ethyl orthosilicate added was 8g.
Preparation example 7, an epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate was different from preparation example 1 only in that the amount of ethyl orthosilicate added was 35g.
Preparation example 8, an epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate was different from preparation example 1 only in that the addition amount of the epoxy resin E51 was 12g.
Preparation example 9, an epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate was different from preparation example 1 only in that the addition amount of the epoxy resin E51 was 30g.
Preparation example 10, an epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate is different from the preparation example 1 in that the microcapsule modified ammonium polyphosphate is prepared according to the following method:
adding 100g of distilled water into 300g of absolute ethyl alcohol, uniformly mixing, adding 100g of ammonium polyphosphate, 2g of sodium dodecyl sulfate and 40g of ammonia water, stirring and mixing for 20min at 40 ℃, adding 20g of ethyl orthosilicate, reacting for 4h at 50 ℃, and carrying out suction filtration, washing and drying to obtain SiO 2 Modified ammonium polyphosphate.
Preparation example 11, an epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate is different from the preparation example 1 in that the microcapsule modified ammonium polyphosphate is prepared according to the following method:
sequentially adding 20g of epoxy resin E51 (with an epoxy value of 0.48-0.54), 2g of triethylene tetramine, 100g of ammonium polyphosphate and 1g of sodium dodecyl benzene sulfonate into 240g of absolute ethyl alcohol, stirring and dispersing for 30min, heating the solution to 50 ℃, stirring and reacting for 3h, and filtering, washing and drying after the reaction is finished to obtain the epoxy resin modified ammonium polyphosphate.
Examples
Example 1, a silane modified two-component flame retardant adhesive, was prepared as follows:
and (3) preparation of the component A: 3kg of silane modified polyether (model SAX 400), 1.5kg of triethyl phosphate, 3.5kg of aluminum hydroxide, 0.07kg of 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole, 0.07kg of light stabilizer 292 and 0.25kg of polyamide wax (molecular weight of 500-800) are mixed, stirred for 1h at a speed of 1000rpm under a vacuum condition of 100 ℃, cooled to 40 ℃, added with 0.4kg of gamma-aminopropyl trimethoxysilane, 0.25kg of ethylenediamine, 0.15kg of triethanolamine and 0.1kg of vinyl trimethoxysilane, and uniformly stirred to obtain a component A.
And (3) preparation of a component B: 4kg of epoxy resin E51 (with the epoxy value of 0.48-0.54), 3kg of aluminum hydroxide, 2kg of epoxy resin-SiO 2 microcapsule modified ammonium polyphosphate prepared in preparation example 1, 3kg of triphenyl phosphate, 0.1kg of deionized water and 0.3kg of di (acetylacetonate) dibutyl tin are stirred and mixed uniformly under vacuum condition to obtain the component B.
Wherein the vacuum degree is-0.1 Mpa under vacuum condition.
Examples 2 to 19, a silane-modified two-component flame retardant adhesive, differing from example 1 only in the proportions of the raw materials used, are shown in Table I:
formulations of examples 1 to 19
Wherein example 2 and example 3 employ rings prepared in preparation example 2Oxygen resin-SiO 2 microcapsule modified ammonium polyphosphate; example 8 and example 9 use the epoxy resin-SiO obtained in preparation example 3 2 Microcapsule modified ammonium polyphosphate; examples 10 and 11 employ the epoxy resin-SiO obtained in preparation example 4 2 Microcapsule modified ammonium polyphosphate; examples 12 and 13 use the epoxy resin-SiO obtained in preparation example 5 2 Microcapsule modified ammonium polyphosphate.
Example 20A silane-modified two-component flame retardant adhesive differs from example 1 only in that the epoxy resin-SiO obtained in example 6 was used in equal amounts 2 Microcapsule modified ammonium polyphosphate replaces epoxy resin-SiO prepared in preparation example 1 2 Microcapsule modified ammonium polyphosphate.
Example 21A silane-modified two-component flame retardant adhesive differs from example 1 only in that the epoxy resin-SiO obtained in example 7 was used in equal amounts 2 Microcapsule modified ammonium polyphosphate replaces epoxy resin-SiO prepared in preparation example 1 2 Microcapsule modified ammonium polyphosphate.
Example 22A silane-modified two-component flame retardant adhesive differs from example 1 only in that the epoxy resin-SiO obtained in example 8 was used in equal amounts 2 Microcapsule modified ammonium polyphosphate replaces epoxy resin-SiO prepared in preparation example 1 2 Microcapsule modified ammonium polyphosphate.
Example 23A silane-modified two-component flame retardant adhesive differs from example 1 only in that the same amount of epoxy resin-SiO as prepared in preparation example 9 was used 2 Microcapsule modified ammonium polyphosphate replaces epoxy resin-SiO prepared in preparation example 1 2 Microcapsule modified ammonium polyphosphate.
Example 24, a silane-modified two-component flame retardant adhesive, differs from example 1 only in that the amount of aluminum hydroxide added during the preparation of the a component is 2.8kg; in the preparation process of the component B, the addition amount of the aluminum hydroxide is 2.2kg.
Example 25, a silane-modified two-component flame retardant adhesive, differs from example 1 only in that the amount of aluminum hydroxide added during the preparation of the a component is 4.2kg; in the preparation process of the component B, the addition amount of the aluminum hydroxide is 2.8kg.
Comparative example
Comparative example 1A silane-modified two-component flame retardant adhesive was different from example 1 only in that the epoxy resin-SiO obtained in preparation example 1 2 The addition amount of the microcapsule modified ammonium polyphosphate was 1.2kg.
Comparative example 2, a silane-modified two-component flame retardant adhesive, was different from example 1 only in that the epoxy resin-SiO obtained in preparation example 1 2 The addition amount of the microcapsule modified ammonium polyphosphate was 2.8kg.
Comparative example 3, a silane-modified two-component flame retardant adhesive, was different from example 1 only in that the same amount of the epoxy resin-SiO obtained in preparation example 10 was used 2 Microcapsule modified ammonium polyphosphate replaces epoxy resin-SiO prepared in preparation example 1 2 Microcapsule modified ammonium polyphosphate.
Comparative example 4A silane-modified two-component flame retardant adhesive was different from example 1 only in that the same amount of epoxy resin-SiO as prepared in preparation example 11 was used 2 Microcapsule modified ammonium polyphosphate replaces epoxy resin-SiO prepared in preparation example 1 2 Microcapsule modified ammonium polyphosphate.
Comparative example 5A silane-modified two-component flame retardant adhesive differs from example 1 only in that the epoxy resin-SiO obtained in preparation example 1 was replaced with an equivalent amount of ammonium polyphosphate 2 Microcapsule modified ammonium polyphosphate.
Performance test
1. Flame retardant testing: according to GB/T13488-92 rubber Combustion Performance determination vertical Combustion method, flame retardant grades are rated according to the standard and whether the phenomenon that the drop ignites cotton wool occurs is tested.
2. Mechanical property test: according to GB/T528-2009 test for tensile stress Strain Properties of vulcanized rubber or thermoplastic rubber, the tensile strength (MPa) of a sample after curing for 7d under standard conditions at a temperature of (23+ -2) deg.C was tested, wherein the sample was prepared according to the standard type I.
3. Test of migration resistance: coating a sample on the surface of an aluminum alloy plate, curing for 7d under the same curing condition, standing for 28d under the same environment, comparing the precipitation conditions of the surface of the sample, dividing the sample into 5 grades, wherein no precipitation is marked as grade I, slight precipitation is marked as grade II, precipitation is marked as grade III, more precipitation is marked as grade IV, and serious precipitation is marked as grade V.
The test results are shown in Table II:
test results of flame retardant Properties and mechanical Properties
According to Table II, in combination with example 1, comparative example 1 and comparative example 2, it can be seen that the flame retardant rating of comparative example 1 and comparative example 2 is FV-1, flame retardant is not dropped, tensile strength is slightly lowered compared with example 1, and there is a slight precipitation, which means that the flame retardant performance of comparative example 1 and comparative example 2 is lower than that of example 1, and mechanical properties are lowered compared with example 1. The reason for this may be that the epoxy resin-SiO in comparative example 1 2 The amount of the microcapsule-modified ammonium polyphosphate added was reduced, below the desired range, epoxy resin-SiO in comparative example 2 2 The addition amount of the microcapsule modified ammonium polyphosphate is increased, which is higher than the required range, when the epoxy resin-SiO 2 When the addition amount of the microcapsule modified ammonium polyphosphate is reduced, the flame retardant efficiency is also reduced, the crosslinking density between the microcapsule modified ammonium polyphosphate and silane modified polyether is also reduced, and the mechanical property of the flame retardant sealant is reduced; when epoxy resin-SiO 2 When the addition amount of the microcapsule modified ammonium polyphosphate is increased, agglomeration is easy, and the mechanical property of the flame-retardant sealant can be reduced due to excessive addition amount of the flame retardant.
As can be seen from the combination of example 1 and comparative example 3, comparative example 3 has a flame retardant rating of FV-2, drop-in cotton burns, a significant decrease in tensile strength compared to example 1, and more precipitation, indicating a significant decrease in flame retardancy of comparative example 3 compared to example 1, and a significant decrease in migration resistance and mechanical properties. The reason for this is probably that in comparative example 3, ammonium polyphosphate was only modified by silica microcapsule, on one hand, the effect of epoxy resin was lacking, the compatibility of ammonium polyphosphate and silane-modified polyether was poor, the migration resistance was lowered, the flame retardant property was lowered, on the other hand, crosslinking with silane-modified polyether was not possible, the crosslinking density was lowered, precipitation of small molecular substances such as flame retardant plasticizer was difficult to be suppressed, and the mechanical property was lowered.
As can be seen from the combination of example 1 and comparative example 4, comparative example 4 has a flame retardant rating of FV-1, is free from dropping cotton, has a significantly reduced tensile strength as compared with example 1, and precipitates out, indicating that the flame retardancy of comparative example 4 is reduced as compared with example 1, and has reduced migration resistance and mechanical properties. The reason for this may be that the ammonium polyphosphate in comparative example 4 was modified only with an epoxy resin, and the inorganic barrier formed by the lack of silica during the combustion process was degraded in flame retardant performance of the flame retardant sealer.
As can be seen from the combination of example 1 and comparative example 5, comparative example 5 has a flame retardant rating of FV-2, is flame-retardant with drop cotton, has a significantly reduced tensile strength compared with example 1, and has severe precipitation, indicating that the flame retardancy of comparative example 5 has significantly reduced migration resistance and mechanical properties compared with example 1. The reason for this is probably that the ammonium polyphosphate in comparative example 5 was not modified, and on the one hand, the compatibility with the silane oligomer and the epoxy resin was not good, the migration resistance was significantly reduced, and on the other hand, a crosslinked structure could not be formed, and precipitation of small molecular substances such as a flame retardant plasticizer could not be suppressed, and the flame retardant property and the mechanical property were significantly reduced.
In combination with examples 1 and examples 2 to 19, it can be seen that the flame retardant rating, tensile strength and migration resistance of examples 2 to 19 are not significantly changed from example 1, indicating that the flame retardant properties, mechanical properties and migration resistance of examples 2 to 19 are not significantly changed from example 1. The reason for this may be that examples 2 to 19 only changed the ratio of the raw materials of the flame-retardant sealant within the required range, indicating that changing the ratio of the raw materials within the required range has no significant effect on the performance of the flame-retardant sealant.
Combine example 1 and example20 and example 21, it can be seen that example 20 and example 21 show a slight decrease in mechanical properties and a slight precipitation compared to example 1, indicating a slight decrease in migration resistance of example 20, probably due to the epoxy resin-SiO in example 20 2 SiO of microcapsule modified ammonium polyphosphate 2 The inorganic layer coated on the surface of ammonium polyphosphate has reduced effect, and ammonium polyphosphate has slight precipitation phenomenon.
In combination with example 1, example 22 and example 23, it can be seen that example 22 and example 23 have a reduced mechanical properties compared to example 1 and are slightly precipitated, indicating that the mechanical properties and migration resistance of example 22 and example 23 are reduced compared to example 1. This may be due to the epoxy-SiO in example 22 2 The epoxy resin content of the microcapsule-modified ammonium polyphosphate was reduced, epoxy resin-SiO in example 23 2 The epoxy resin content of the microcapsule modified ammonium polyphosphate is increased, the reduction of the epoxy resin content reduces the crosslinking density, the probability of small molecules overflowing the surface of the flame-retardant sealant is increased, and the reduction of the crosslinking density is accompanied with the reduction of the mechanical property of the flame-retardant sealant; when the addition amount of the epoxy resin is increased, the addition amount of the epoxy resin is saturated, and the addition amount of the epoxy resin is increased, so that the coating rate of the ammonium polyphosphate surface is not increased, even the coating rate is reduced, and the mechanical property and the migration resistance of the flame-retardant sealant are reduced.
In combination with examples 1, 24 and 25, it can be seen that the flame retardant rating of example 24 is reduced as compared with example 1 to FV-1, and that the mechanical properties of both example 24 and example 25 are reduced, indicating that the flame retardant properties of example 24 are reduced, and that the mechanical properties of example 24 and example 25 are reduced as compared with example 1. The reason for this may be that in example 24, the addition amount of aluminum hydroxide is reduced, the reduction of filler would reduce the reinforcing effect, the mechanical properties of the flame-retardant sealant are reduced, and at the same time, aluminum hydroxide also plays a role in flame-retardant synergism, and the flame-retardant performance of the flame-retardant sealant is increased together with the flame-retardant plasticizer, the addition amount of aluminum hydroxide is reduced, the flame-retardant synergism is reduced, and the flame-retardant performance is reduced; and when the addition amount of aluminum hydroxide is increased, the excessive addition of the filler can lead to the reduction of the mechanical property of the flame-retardant sealant.
The present embodiment is only for explanation of the present application and is not to be construed as limiting the present application, and modifications to the present embodiment, which may not creatively contribute to the present application as required by those skilled in the art after reading the present specification, are all protected by patent laws within the scope of claims of the present application.
Claims (10)
1. The silane modified bi-component flame retardant adhesive is characterized by comprising an A component and a B component, wherein the A component and the B component comprise the following raw materials in parts by weight:
and (3) a component A:
200-400 parts of silane modified polyether;
100-200 parts of flame retardant plasticizer;
1-400 parts of filler;
3-10 parts of ultraviolet absorber;
3-10 parts of light stabilizer;
15-35 parts of thixotropic agent;
30-50 parts of silane coupling agent;
10-40 parts of a first curing agent;
10-20 parts of a curing accelerator;
5-15 parts of a water scavenger;
and the component B comprises the following components:
300-500 parts of epoxy resin;
1-350 parts of filler;
150-250 parts of filler;
250-350 parts of flame retardant plasticizer;
deionized water 5-15;
20-40 parts of a second curing agent;
the filler 2 is epoxy resin-SiO 2 Microcapsule modified ammonium polyphosphate.
2. The silane-modified two-component flame retardant adhesive according to claim 1, wherein the epoxy resin comprises one or a combination of a bisphenol a type epoxy resin, a bisphenol F type epoxy resin, a polyphenol type glycidyl ether epoxy resin, an aliphatic glycidyl ether epoxy resin, a glycidyl ester type epoxy resin, and a glycidyl amine type epoxy resin.
3. The silane-modified two-component flame retardant adhesive according to claim 1, wherein the flame retardant plasticizer comprises one or a combination of several of tri (2-chloroethyl) phosphate, tri (2-chloropropyl) phosphate, triethyl phosphate, triphenyl phosphate, tri (1, 3-dichloroisopropyl) phosphate, tributoxyethyl phosphate and toluene diphenyl phosphate.
4. The silane-modified two-component flame retardant adhesive according to claim 1, wherein the filler 1 comprises one or a combination of several of aluminum hydroxide, magnesium hydroxide, expanded graphite, borate, aluminum oxalate, and zinc sulfate.
5. The silane-modified two-component flame retardant adhesive of claim 1, wherein the epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate comprises the following raw materials in percentage by mass (0.1-0.3): 0.15 to 0.25 of epoxy resin of 1, tetraethoxysilane and ammonium polyphosphate.
6. The silane-modified two-component flame-retardant adhesive according to claim 5, wherein the epoxy resin is bisphenol a type epoxy resin, and the epoxy value of the epoxy resin is 0.4-0.54.
7. The silane-modified two-component flame retardant adhesive of claim 5, wherein said epoxy resin-SiO 2 The microcapsule modified ammonium polyphosphate is prepared by the following steps:
s1, adding distilled water into a solvent, uniformly mixing, adding sodium polyphosphate, a dispersing agent and a catalyst 1, stirring and mixing for 15-20 min at 35-45 ℃, then adding tetraethoxysilane, reacting for 3-5 h at 40-50 ℃, and then carrying out suction filtration, washing and drying to obtain a modified ammonium polyphosphate pre-reactant;
s2, sequentially adding epoxy resin, a curing agent, a modified ammonium polyphosphate pre-reactant, a dispersing agent and a catalyst 2 into a solvent, stirring and dispersing for 20-40 min, heating the solution to 80-90 ℃, stirring and reacting for 2-3 h, and performing suction filtration, washing and drying after the reaction is finished to obtain the epoxy resin-SiO 2 Microcapsule modified ammonium polyphosphate.
8. The silane-modified two-component flame retardant adhesive of claim 7, wherein the dispersant comprises one or a combination of sodium dodecyl sulfate and sodium dodecyl benzene sulfonate; the curing agent comprises one or a combination of more of triethylene tetramine, ethylenediamine, diethylenetriamine, tetraethylenepentamine, m-phenylenediamine and m-xylylene.
9. The silane-modified two-component flame retardant adhesive according to claim 7, wherein the addition amount of the dispersing agent is 0.5-2.5% of the mass of ammonium polyphosphate, and the addition amount of the curing agent is 5-20% of the mass of the epoxy resin.
10. The preparation method of the silane modified two-component flame retardant adhesive according to any one of claims 1 to 9, which is characterized by comprising the following steps:
and (3) preparation of the component A: mixing silane modified polyether, flame retardant plasticizer, filler 1, ultraviolet absorbent, light stabilizer and thixotropic agent, stirring at a speed of 1000-1200 rpm under a vacuum condition of 90-100 ℃ for 0.5-1 h, cooling to 40-50 ℃, adding silane coupling agent, first curing agent, curing accelerator and water scavenger, and stirring uniformly to obtain a component A;
and (3) preparation of a component B: and uniformly stirring and mixing the epoxy resin, the filler 1, the filler 2, the flame-retardant plasticizer, the deionized water and the second curing agent under a vacuum condition to obtain the component B.
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