JP5704972B2 - Adhesive composition and adhesive tape - Google Patents
Adhesive composition and adhesive tape Download PDFInfo
- Publication number
- JP5704972B2 JP5704972B2 JP2011049166A JP2011049166A JP5704972B2 JP 5704972 B2 JP5704972 B2 JP 5704972B2 JP 2011049166 A JP2011049166 A JP 2011049166A JP 2011049166 A JP2011049166 A JP 2011049166A JP 5704972 B2 JP5704972 B2 JP 5704972B2
- Authority
- JP
- Japan
- Prior art keywords
- pressure
- meth
- sensitive adhesive
- adhesive composition
- filler
- 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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- 239000000203 mixture Substances 0.000 title claims description 73
- 239000000853 adhesive Substances 0.000 title claims description 55
- 230000001070 adhesive effect Effects 0.000 title claims description 55
- 239000002390 adhesive tape Substances 0.000 title claims description 16
- 239000004820 Pressure-sensitive adhesive Substances 0.000 claims description 107
- 239000000178 monomer Substances 0.000 claims description 68
- 239000002270 dispersing agent Substances 0.000 claims description 53
- 239000000945 filler Substances 0.000 claims description 39
- 229920000058 polyacrylate Polymers 0.000 claims description 36
- 239000010410 layer Substances 0.000 claims description 30
- -1 phosphate ester salt Chemical class 0.000 claims description 23
- 239000002253 acid Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 13
- 150000001412 amines Chemical class 0.000 claims description 12
- 239000003999 initiator Substances 0.000 claims description 12
- 239000012790 adhesive layer Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 229910019142 PO4 Inorganic materials 0.000 claims description 5
- 239000010452 phosphate Substances 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 46
- 229940048053 acrylate Drugs 0.000 description 45
- 238000003860 storage Methods 0.000 description 18
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 17
- 239000003431 cross linking reagent Substances 0.000 description 13
- 229920000642 polymer Polymers 0.000 description 10
- 238000000576 coating method Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- 239000011248 coating agent Substances 0.000 description 7
- 238000005259 measurement Methods 0.000 description 7
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 6
- 239000011231 conductive filler Substances 0.000 description 6
- 230000007423 decrease Effects 0.000 description 6
- 230000003993 interaction Effects 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 5
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 4
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 230000014759 maintenance of location Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 229920001223 polyethylene glycol Polymers 0.000 description 4
- 238000012719 thermal polymerization Methods 0.000 description 4
- UHFFVFAKEGKNAQ-UHFFFAOYSA-N 2-benzyl-2-(dimethylamino)-1-(4-morpholin-4-ylphenyl)butan-1-one Chemical compound C=1C=C(N2CCOCC2)C=CC=1C(=O)C(CC)(N(C)C)CC1=CC=CC=C1 UHFFVFAKEGKNAQ-UHFFFAOYSA-N 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 3
- 239000002202 Polyethylene glycol Substances 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 238000012662 bulk polymerization Methods 0.000 description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 3
- 239000003505 polymerization initiator Substances 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- 239000011800 void material Substances 0.000 description 3
- FKTHNVSLHLHISI-UHFFFAOYSA-N 1,2-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC=C1CN=C=O FKTHNVSLHLHISI-UHFFFAOYSA-N 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O ammonium group Chemical group [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 2
- 239000012965 benzophenone Substances 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- 238000005227 gel permeation chromatography Methods 0.000 description 2
- 229920006158 high molecular weight polymer Polymers 0.000 description 2
- 239000012948 isocyanate Substances 0.000 description 2
- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 2
- 150000002513 isocyanates Chemical class 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000003472 neutralizing effect Effects 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920006267 polyester film Polymers 0.000 description 2
- 229920001451 polypropylene glycol Polymers 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000010526 radical polymerization reaction Methods 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000006188 syrup Substances 0.000 description 2
- 235000020357 syrup Nutrition 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- QNODIIQQMGDSEF-UHFFFAOYSA-N (1-hydroxycyclohexyl)-phenylmethanone Chemical compound C=1C=CC=CC=1C(=O)C1(O)CCCCC1 QNODIIQQMGDSEF-UHFFFAOYSA-N 0.000 description 1
- FVQMJJQUGGVLEP-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOOC(C)(C)C FVQMJJQUGGVLEP-UHFFFAOYSA-N 0.000 description 1
- WXPWZZHELZEVPO-UHFFFAOYSA-N (4-methylphenyl)-phenylmethanone Chemical compound C1=CC(C)=CC=C1C(=O)C1=CC=CC=C1 WXPWZZHELZEVPO-UHFFFAOYSA-N 0.000 description 1
- VBQCFYPTKHCPGI-UHFFFAOYSA-N 1,1-bis(2-methylpentan-2-ylperoxy)cyclohexane Chemical compound CCCC(C)(C)OOC1(OOC(C)(C)CCC)CCCCC1 VBQCFYPTKHCPGI-UHFFFAOYSA-N 0.000 description 1
- NNOZGCICXAYKLW-UHFFFAOYSA-N 1,2-bis(2-isocyanatopropan-2-yl)benzene Chemical compound O=C=NC(C)(C)C1=CC=CC=C1C(C)(C)N=C=O NNOZGCICXAYKLW-UHFFFAOYSA-N 0.000 description 1
- ZXHZWRZAWJVPIC-UHFFFAOYSA-N 1,2-diisocyanatonaphthalene Chemical compound C1=CC=CC2=C(N=C=O)C(N=C=O)=CC=C21 ZXHZWRZAWJVPIC-UHFFFAOYSA-N 0.000 description 1
- ALVZNPYWJMLXKV-UHFFFAOYSA-N 1,9-Nonanediol Chemical compound OCCCCCCCCCO ALVZNPYWJMLXKV-UHFFFAOYSA-N 0.000 description 1
- UICXTANXZJJIBC-UHFFFAOYSA-N 1-(1-hydroperoxycyclohexyl)peroxycyclohexan-1-ol Chemical compound C1CCCCC1(O)OOC1(OO)CCCCC1 UICXTANXZJJIBC-UHFFFAOYSA-N 0.000 description 1
- NQUXRXBRYDZZDL-UHFFFAOYSA-N 1-(2-prop-2-enoyloxyethyl)cyclohexane-1,2-dicarboxylic acid Chemical compound OC(=O)C1CCCCC1(CCOC(=O)C=C)C(O)=O NQUXRXBRYDZZDL-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- IVIDDMGBRCPGLJ-UHFFFAOYSA-N 2,3-bis(oxiran-2-ylmethoxy)propan-1-ol Chemical compound C1OC1COC(CO)COCC1CO1 IVIDDMGBRCPGLJ-UHFFFAOYSA-N 0.000 description 1
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 1
- IEQWWMKDFZUMMU-UHFFFAOYSA-N 2-(2-prop-2-enoyloxyethyl)butanedioic acid Chemical compound OC(=O)CC(C(O)=O)CCOC(=O)C=C IEQWWMKDFZUMMU-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- KUBDPQJOLOUJRM-UHFFFAOYSA-N 2-(chloromethyl)oxirane;4-[2-(4-hydroxyphenyl)propan-2-yl]phenol Chemical compound ClCC1CO1.C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 KUBDPQJOLOUJRM-UHFFFAOYSA-N 0.000 description 1
- WYGWHHGCAGTUCH-UHFFFAOYSA-N 2-[(2-cyano-4-methylpentan-2-yl)diazenyl]-2,4-dimethylpentanenitrile Chemical compound CC(C)CC(C)(C#N)N=NC(C)(C#N)CC(C)C WYGWHHGCAGTUCH-UHFFFAOYSA-N 0.000 description 1
- SYEWHONLFGZGLK-UHFFFAOYSA-N 2-[1,3-bis(oxiran-2-ylmethoxy)propan-2-yloxymethyl]oxirane Chemical compound C1OC1COCC(OCC1OC1)COCC1CO1 SYEWHONLFGZGLK-UHFFFAOYSA-N 0.000 description 1
- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 description 1
- CKSAKVMRQYOFBC-UHFFFAOYSA-N 2-cyanopropan-2-yliminourea Chemical compound N#CC(C)(C)N=NC(N)=O CKSAKVMRQYOFBC-UHFFFAOYSA-N 0.000 description 1
- XMLYCEVDHLAQEL-UHFFFAOYSA-N 2-hydroxy-2-methyl-1-phenylpropan-1-one Chemical compound CC(C)(O)C(=O)C1=CC=CC=C1 XMLYCEVDHLAQEL-UHFFFAOYSA-N 0.000 description 1
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 1
- RIWRBSMFKVOJMN-UHFFFAOYSA-N 2-methyl-1-phenylpropan-2-ol Chemical compound CC(C)(O)CC1=CC=CC=C1 RIWRBSMFKVOJMN-UHFFFAOYSA-N 0.000 description 1
- RCEJCSULJQNRQQ-UHFFFAOYSA-N 2-methylbutanenitrile Chemical compound CCC(C)C#N RCEJCSULJQNRQQ-UHFFFAOYSA-N 0.000 description 1
- SEILKFZTLVMHRR-UHFFFAOYSA-N 2-phosphonooxyethyl 2-methylprop-2-enoate Chemical group CC(=C)C(=O)OCCOP(O)(O)=O SEILKFZTLVMHRR-UHFFFAOYSA-N 0.000 description 1
- BIISIZOQPWZPPS-UHFFFAOYSA-N 2-tert-butylperoxypropan-2-ylbenzene Chemical compound CC(C)(C)OOC(C)(C)C1=CC=CC=C1 BIISIZOQPWZPPS-UHFFFAOYSA-N 0.000 description 1
- KFGFVPMRLOQXNB-UHFFFAOYSA-N 3,5,5-trimethylhexanoyl 3,5,5-trimethylhexaneperoxoate Chemical compound CC(C)(C)CC(C)CC(=O)OOC(=O)CC(C)CC(C)(C)C KFGFVPMRLOQXNB-UHFFFAOYSA-N 0.000 description 1
- QISZCVLALJOROC-UHFFFAOYSA-N 3-(2-hydroxyethyl)-4-(2-prop-2-enoyloxyethyl)phthalic acid Chemical compound OCCC1=C(CCOC(=O)C=C)C=CC(C(O)=O)=C1C(O)=O QISZCVLALJOROC-UHFFFAOYSA-N 0.000 description 1
- UXTGJIIBLZIQPK-UHFFFAOYSA-N 3-(2-prop-2-enoyloxyethyl)phthalic acid Chemical compound OC(=O)C1=CC=CC(CCOC(=O)C=C)=C1C(O)=O UXTGJIIBLZIQPK-UHFFFAOYSA-N 0.000 description 1
- NHQDETIJWKXCTC-UHFFFAOYSA-N 3-chloroperbenzoic acid Chemical compound OOC(=O)C1=CC=CC(Cl)=C1 NHQDETIJWKXCTC-UHFFFAOYSA-N 0.000 description 1
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 1
- VFXXTYGQYWRHJP-UHFFFAOYSA-N 4,4'-azobis(4-cyanopentanoic acid) Chemical compound OC(=O)CCC(C)(C#N)N=NC(C)(CCC(O)=O)C#N VFXXTYGQYWRHJP-UHFFFAOYSA-N 0.000 description 1
- RTANHMOFHGSZQO-UHFFFAOYSA-N 4-methoxy-2,4-dimethylpentanenitrile Chemical compound COC(C)(C)CC(C)C#N RTANHMOFHGSZQO-UHFFFAOYSA-N 0.000 description 1
- ORTNTAAZJSNACP-UHFFFAOYSA-N 6-(oxiran-2-ylmethoxy)hexan-1-ol Chemical compound OCCCCCCOCC1CO1 ORTNTAAZJSNACP-UHFFFAOYSA-N 0.000 description 1
- YFEKCGCUBYDMAS-UHFFFAOYSA-N 7,7-dimethyl-2-(2,4,4-trimethylpentan-2-yl)octaneperoxoic acid Chemical compound CC(C)(C)CCCCC(C(=O)OO)C(C)(C)CC(C)(C)C YFEKCGCUBYDMAS-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052582 BN Inorganic materials 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-M Butyrate Chemical compound CCCC([O-])=O FERIUCNNQQJTOY-UHFFFAOYSA-M 0.000 description 1
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Natural products CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 1
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- ZMDDERVSCYEKPQ-UHFFFAOYSA-N Ethyl (mesitylcarbonyl)phenylphosphinate Chemical compound C=1C=CC=CC=1P(=O)(OCC)C(=O)C1=C(C)C=C(C)C=C1C ZMDDERVSCYEKPQ-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 1
- 239000005058 Isophorone diisocyanate Substances 0.000 description 1
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N N-phenyl amine Natural products NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 1
- QORUGOXNWQUALA-UHFFFAOYSA-N N=C=O.N=C=O.N=C=O.C1=CC=C(C(C2=CC=CC=C2)C2=CC=CC=C2)C=C1 Chemical compound N=C=O.N=C=O.N=C=O.C1=CC=C(C(C2=CC=CC=C2)C2=CC=CC=C2)C=C1 QORUGOXNWQUALA-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- 229920000538 Poly[(phenyl isocyanate)-co-formaldehyde] Polymers 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- LFOXEOLGJPJZAA-UHFFFAOYSA-N [(2,6-dimethoxybenzoyl)-(2,4,4-trimethylpentyl)phosphoryl]-(2,6-dimethoxyphenyl)methanone Chemical compound COC1=CC=CC(OC)=C1C(=O)P(=O)(CC(C)CC(C)(C)C)C(=O)C1=C(OC)C=CC=C1OC LFOXEOLGJPJZAA-UHFFFAOYSA-N 0.000 description 1
- MZVQCMJNVPIDEA-UHFFFAOYSA-N [CH2]CN(CC)CC Chemical group [CH2]CN(CC)CC MZVQCMJNVPIDEA-UHFFFAOYSA-N 0.000 description 1
- GUCYFKSBFREPBC-UHFFFAOYSA-N [phenyl-(2,4,6-trimethylbenzoyl)phosphoryl]-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C(=O)C1=C(C)C=C(C)C=C1C GUCYFKSBFREPBC-UHFFFAOYSA-N 0.000 description 1
- KYIKRXIYLAGAKQ-UHFFFAOYSA-N abcn Chemical compound C1CCCCC1(C#N)N=NC1(C#N)CCCCC1 KYIKRXIYLAGAKQ-UHFFFAOYSA-N 0.000 description 1
- 229940114077 acrylic acid Drugs 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 1
- 150000008366 benzophenones Chemical class 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- HIFVAOIJYDXIJG-UHFFFAOYSA-N benzylbenzene;isocyanic acid Chemical class N=C=O.N=C=O.C=1C=CC=CC=1CC1=CC=CC=C1 HIFVAOIJYDXIJG-UHFFFAOYSA-N 0.000 description 1
- ZNAAXKXXDQLJIX-UHFFFAOYSA-N bis(2-cyclohexyl-3-hydroxyphenyl)methanone Chemical compound C1CCCCC1C=1C(O)=CC=CC=1C(=O)C1=CC=CC(O)=C1C1CCCCC1 ZNAAXKXXDQLJIX-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 229920006037 cross link polymer Polymers 0.000 description 1
- 229910002026 crystalline silica Inorganic materials 0.000 description 1
- YQHLDYVWEZKEOX-UHFFFAOYSA-N cumene hydroperoxide Chemical compound OOC(C)(C)C1=CC=CC=C1 YQHLDYVWEZKEOX-UHFFFAOYSA-N 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- PODOEQVNFJSWIK-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethoxyphenyl)methanone Chemical compound COC1=CC(OC)=CC(OC)=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 PODOEQVNFJSWIK-UHFFFAOYSA-N 0.000 description 1
- VFHVQBAGLAREND-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 VFHVQBAGLAREND-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 125000002960 margaryl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 125000005641 methacryl group Chemical group 0.000 description 1
- ZQMHJBXHRFJKOT-UHFFFAOYSA-N methyl 2-[(1-methoxy-2-methyl-1-oxopropan-2-yl)diazenyl]-2-methylpropanoate Chemical compound COC(=O)C(C)(C)N=NC(C)(C)C(=O)OC ZQMHJBXHRFJKOT-UHFFFAOYSA-N 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- SJPFBRJHYRBAGV-UHFFFAOYSA-N n-[[3-[[bis(oxiran-2-ylmethyl)amino]methyl]phenyl]methyl]-1-(oxiran-2-yl)-n-(oxiran-2-ylmethyl)methanamine Chemical compound C1OC1CN(CC=1C=C(CN(CC2OC2)CC2OC2)C=CC=1)CC1CO1 SJPFBRJHYRBAGV-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 125000002560 nitrile group Chemical group 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- AFEQENGXSMURHA-UHFFFAOYSA-N oxiran-2-ylmethanamine Chemical compound NCC1CO1 AFEQENGXSMURHA-UHFFFAOYSA-N 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- OKJMWOSMAIIUAG-UHFFFAOYSA-N oxonickel oxygen(2-) titanium(4+) Chemical compound [O-2].[O-2].[Ti+4].[Ni]=O OKJMWOSMAIIUAG-UHFFFAOYSA-N 0.000 description 1
- 125000000913 palmityl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 125000002958 pentadecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000005502 peroxidation Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- HPAFOABSQZMTHE-UHFFFAOYSA-N phenyl-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)C1=CC=CC=C1 HPAFOABSQZMTHE-UHFFFAOYSA-N 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- BWJUFXUULUEGMA-UHFFFAOYSA-N propan-2-yl propan-2-yloxycarbonyloxy carbonate Chemical compound CC(C)OC(=O)OOC(=O)OC(C)C BWJUFXUULUEGMA-UHFFFAOYSA-N 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- OPQYOFWUFGEMRZ-UHFFFAOYSA-N tert-butyl 2,2-dimethylpropaneperoxoate Chemical compound CC(C)(C)OOC(=O)C(C)(C)C OPQYOFWUFGEMRZ-UHFFFAOYSA-N 0.000 description 1
- VNJISVYSDHJQFR-UHFFFAOYSA-N tert-butyl 4,4-dimethylpentaneperoxoate Chemical compound CC(C)(C)CCC(=O)OOC(C)(C)C VNJISVYSDHJQFR-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
-
- 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
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
-
- 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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
-
- 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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
-
- 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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/314—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive layer and/or the carrier being conductive
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
-
- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
Description
本発明は、粘着組成物、及び粘着テープに関する。特に、本発明は、粘着剤成分と、熱伝導性フィラーや導電性フィラーなどのフィラーとを含有する粘着組成物、及びそれを用いた粘着テープに関する。 The present invention relates to an adhesive composition and an adhesive tape. In particular, the present invention relates to a pressure-sensitive adhesive composition containing a pressure-sensitive adhesive component and a filler such as a heat conductive filler or a conductive filler, and a pressure-sensitive adhesive tape using the same.
従来、粘着剤成分と熱伝導性フィラーとを含有する粘着組成物からなる粘着剤層を備えた熱伝導性の粘着テープや、同様に、粘着剤成分と導電性フィラーとを含有する粘着組成物からなる粘着剤層を備えた導電性の粘着テープなどが知られている。これらの粘着テープは、電子部品やそれを収容した筐体などに貼り付けて使用される場合がある。 Conventionally, a heat-conductive pressure-sensitive adhesive tape having a pressure-sensitive adhesive layer comprising a pressure-sensitive adhesive composition containing a pressure-sensitive adhesive component and a heat conductive filler, and a pressure-sensitive adhesive composition containing a pressure-sensitive adhesive component and a conductive filler in the same manner A conductive pressure-sensitive adhesive tape provided with a pressure-sensitive adhesive layer is known. These adhesive tapes may be used by being attached to an electronic component or a housing that houses the electronic component.
例えば、プラズマディスプレイパネル(PDP)、集積回路(IC)チップなどのような電子部品は、その高性能化に伴って発熱量が増大しており、そのため温度上昇による機能障害対策を講じる必要性が生じている。上記観点から、電子部品などの発熱体にはヒートシンクなどの放熱体が取り付けられているが、電子部品と放熱体との熱的接続性が低いと十分な冷却性能が得られないことから、これらを熱伝導性の粘着テープを用いて接合している。 For example, electronic components such as plasma display panels (PDP) and integrated circuit (IC) chips have increased in heat generation as their performance has increased, and therefore, it is necessary to take countermeasures against functional failures due to temperature rise. Has occurred. From the above viewpoint, a heat radiator such as a heat sink is attached to a heating element such as an electronic component. However, if the thermal connectivity between the electronic component and the heat radiator is low, sufficient cooling performance cannot be obtained. Are bonded using heat conductive adhesive tape.
上記のような粘着テープとしては、特許文献1〜4に開示されている紫外線硬化型の粘着テープが提案されており、例えば、特許文献1及び2では、(メタ)アクリル系単量体、(メタ)アクリル系重合体、開始剤、及び熱伝導性を有するフィラーを含む粘着剤組成物が用いられている。また、特許文献3及び4では、熱伝導性を有するフィラーして、金属酸化物や金属水酸化物を用いるとともに、粘着剤成分として、(メタ)アクリル系単量体と高分子系分散剤のみが用いられている。 As the above-mentioned pressure-sensitive adhesive tape, ultraviolet curable pressure-sensitive adhesive tapes disclosed in Patent Documents 1 to 4 have been proposed. For example, in Patent Documents 1 and 2, a (meth) acrylic monomer, ( A pressure-sensitive adhesive composition containing a (meth) acrylic polymer, an initiator, and a filler having thermal conductivity is used. In Patent Documents 3 and 4, a metal oxide or metal hydroxide is used as a filler having thermal conductivity, and only a (meth) acrylic monomer and a polymer dispersant are used as an adhesive component. Is used.
しかしながら、特許文献3及び4に開示されているような硬化後に樹脂成分となる粘着剤成分として(メタ)アクリル系単量体のみを含む系では、粘着組成物をテープ化した際に高分子量化した樹脂成分を得にくいため凝集力が不足する。そのため、共重合可能な極性基を有する(メタ)アクリル系単量体を含む系では、架橋剤として多官能の(メタ)アクリル系単量体を添加してこれらを光重合することで、凝集力を向上させる手段が取られているが、全ての(メタ)アクリル系単量体を架橋ポリマーとして共重合させると、粘着テープ自身が硬くなり、粘着力の低下等を招く。また、粘着組成物が(メタ)アクリル系重合体を含有しない場合、粘着組成物の粘度のコントロールが基本的に困難となり、種々の目的に応じた粘着テープの設計及び塗工方法への適用が制限される。 However, in a system containing only a (meth) acrylic monomer as a pressure-sensitive adhesive component that becomes a resin component after curing as disclosed in Patent Documents 3 and 4, a high molecular weight is obtained when the pressure-sensitive adhesive composition is taped. Since it is difficult to obtain a resin component, the cohesive force is insufficient. Therefore, in a system containing a (meth) acrylic monomer having a copolymerizable polar group, a polyfunctional (meth) acrylic monomer is added as a crosslinking agent, and these are photopolymerized, thereby agglomerating. A means for improving the force is taken, but if all (meth) acrylic monomers are copolymerized as a cross-linked polymer, the pressure-sensitive adhesive tape itself becomes hard, resulting in a decrease in pressure-sensitive adhesive force and the like. In addition, when the pressure-sensitive adhesive composition does not contain a (meth) acrylic polymer, it is basically difficult to control the viscosity of the pressure-sensitive adhesive composition. Limited.
上記観点から、特許文献1及び2のように、粘着剤成分として(メタ)アクリル系単量体だけでなく、(メタ)アクリル系重合体も含有する粘着剤組成物を使用することが好ましいが、これらの(メタ)アクリル系重合体を含む粘着剤組成物は保存すると粘度が大きく変化する性質があり、そのため安定性に劣り、塗工性が低下しやすいという問題がある。また、このような(メタ)アクリル系重合体も含有する粘着組成物は、高湿環境下で粘着力が低下しやすいだけでなく、高温環境下で保持力が低下しやすいという問題がある。 From the above viewpoint, it is preferable to use a pressure-sensitive adhesive composition containing not only a (meth) acrylic monomer but also a (meth) acrylic polymer as a pressure-sensitive adhesive component as in Patent Documents 1 and 2. The pressure-sensitive adhesive composition containing these (meth) acrylic polymers has a property that the viscosity greatly changes when stored, and therefore has a problem that the stability is inferior and the coating property tends to be lowered. In addition, the pressure-sensitive adhesive composition containing such a (meth) acrylic polymer has a problem that not only the pressure-sensitive adhesive force tends to decrease under a high humidity environment but also the holding power tends to decrease under a high-temperature environment.
本発明は上記課題を解決するものであり、本発明の目的は、安定性に優れるとともに、塗工性に優れ、また高湿保存後でも高粘着力を有し、さらに高温環境下でも高保持力を有する粘着組成物、及びそれを用いた粘着テープを提供することにある。 The present invention solves the above-mentioned problems, and the object of the present invention is excellent in stability, excellent in coating properties, and has high adhesive strength even after storage at high humidity, and is also highly retained in a high temperature environment. It is providing the adhesive composition which has force, and an adhesive tape using the same.
本発明の一局面によれば、(メタ)アクリル酸アルキルエステル単官能単量体(A)、極性基含有単官能単量体(B)、(メタ)アクリル系重合体(C)、開始剤(D)、並びに直鎖構造の主骨格の片末端に極性基を有し、酸価及びアミン価を有しており、水に対して不溶性の両性分散剤(E)を少なくとも含む粘着剤成分と、フィラー(F)とを含有する粘着組成物が提供される。 According to one aspect of the present invention, (meth) acrylic acid alkyl ester monofunctional monomer (A), polar group-containing monofunctional monomer (B), (meth) acrylic polymer (C), initiator (D), as well as the main one end of the scaffold to have a polar group, and have a acid value and amine value, the pressure-sensitive adhesive component comprising insoluble amphoteric dispersant (E) at least against water of linear structure And a pressure-sensitive adhesive composition containing the filler (F).
上記粘着組成物は、粘着剤成分として、(メタ)アクリル系重合体(C)を含有するだけでなく、直鎖構造の主骨格の片末端に極性基を有し、酸価及びアミン価を有しており、水に対して不溶性の両性分散剤(E)も含有するから、フィラー(F)と(メタ)アクリル系重合体(C)との接触を抑えることができるとともに、粘着組成物を可塑化することができる。その結果、安定性に優れるとともに、高湿保存後でも高粘着力を有し、高温環境下でも高保持力を有する粘着組成物を得ることができる。なお、本明細書において、(メタ)アクリルとは、アクリルまたはメタクリルを意味する。 The pressure-sensitive adhesive composition not only contains the (meth) acrylic polymer (C) as a pressure-sensitive adhesive component, but also has a polar group at one end of the main skeleton having a linear structure, and has an acid value and an amine value. Yes to have, because contains insoluble amphoteric dispersant (E) with respect to water, it is possible to suppress the contact between the filler (F) and (meth) acrylic polymer (C), the adhesive composition Can be plasticized. As a result, it is possible to obtain a pressure-sensitive adhesive composition that is excellent in stability, has high adhesive strength even after high-humidity storage, and has high retention strength even in a high temperature environment. In the present specification, (meth) acryl means acryl or methacryl.
上記粘着組成物において、(メタ)アクリル系重合体(C)は、好ましくは100,000以上の重量平均分子量を有し、また、上記粘着組成物は、粘着剤成分全量に対して、(メタ)アクリル系重合体(C)を、好ましくは1〜30質量%含有する。 In the pressure-sensitive adhesive composition, the (meth) acrylic polymer (C) preferably has a weight average molecular weight of 100,000 or more, and the pressure-sensitive adhesive composition is (meta ) The acrylic polymer (C) is preferably contained in an amount of 1 to 30% by mass.
上記粘着組成物において、両性分散剤(E)は、好ましくは極性基として、リン酸エステル塩を有する。 In the above pressure-sensitive adhesive composition, the amphoteric dispersant (E) preferably has a phosphate ester salt as a polar group.
また、上記粘着組成物は、フィラー(F)100質量部に対して、両性分散剤(E)を、好ましくは0.5〜7.5質量部含有する。 Moreover, the said adhesive composition contains 0.5-7.5 mass parts of an amphoteric dispersing agent (E) with respect to 100 mass parts of fillers (F) preferably.
さらに、上記両性分散剤(E)は、好ましくは、(メタ)アクリル酸アルキルエステル単官能単量体(A)及び極性基含有単官能単量体(B)の両方に対して可溶性を有する。 Furthermore, the amphoteric dispersant (E) is preferably soluble in both the ( meth) acrylic acid alkyl ester monofunctional monomer (A) and the polar group-containing monofunctional monomer (B).
そして、本発明の他の局面によれば、上記粘着組成物を含有する粘着剤層を備えた粘着テープが提供される。上記粘着テープにおいて、フィラー(F)は、好ましくは、粘着剤層の50%以下の平均粒径を有し、かつ粘着剤層の厚さ以下の最大粒径を有する。 And according to the other situation of this invention, the adhesive tape provided with the adhesive layer containing the said adhesive composition is provided. In the above-mentioned pressure-sensitive adhesive tape, the filler (F) preferably has an average particle diameter of 50% or less of the pressure-sensitive adhesive layer and a maximum particle diameter equal to or smaller than the thickness of the pressure-sensitive adhesive layer.
本発明によれば、安定性及び塗工性に優れるとともに、高湿保存後でも高粘着力を有し、さらに高温環境下でも高保持力を有する粘着組成物を得ることができる。それゆえ、上記粘着組成物を含有する粘着剤層を備えた粘着テープは、熱伝導性の粘着テープや導電性の粘着テープとして好適に使用することができる。 ADVANTAGE OF THE INVENTION According to this invention, while being excellent in stability and coating property, it has the high adhesive force even after high-humidity storage, Furthermore, the adhesive composition which has a high holding power also in a high temperature environment can be obtained. Therefore, the pressure-sensitive adhesive tape including the pressure-sensitive adhesive layer containing the pressure-sensitive adhesive composition can be suitably used as a heat conductive pressure-sensitive adhesive tape or a conductive pressure-sensitive adhesive tape.
本実施の形態の粘着組成物では、(メタ)アクリル酸アルキルエステル単官能単量体(A)と、極性基含有単官能単量体(B)と、(メタ)アクリル系重合体(C)と、開始剤(D)と、さらに直鎖構造の主骨格の片末端に極性基を有し、酸価及びアミン価を有する両性分散剤(E)とを含有する粘着剤成分が使用される。 In the pressure-sensitive adhesive composition of the present embodiment, the (meth) acrylic acid alkyl ester monofunctional monomer (A), the polar group-containing monofunctional monomer (B), and the (meth) acrylic polymer (C) And an initiator component (D) and an amphoteric dispersant (E) having a polar group at one end of the main skeleton having a linear structure and having an acid value and an amine value are used. .
酸価及びアミン価を有する両性分散剤(E)を使用すれば、フィラー(F)と(メタ)アクリル系重合体(C)とを含有する粘着組成物であっても、両性分散剤(E)がフィラー(F)の表面に被着し、(メタ)アクリル系重合体(C)とフィラー(F)との相互作用が抑えられ、それによって粘着組成物の安定性を向上できる。また、フィラー(F)の表面への分散剤の被着は酸価を示す極性基の酸性基部分が主として機能するが、上記両性分散剤(E)は、アミン価を示す塩基性基部分も有するから、該塩基性基部分が(メタ)アクリル系重合体(C)の極性基とイオン結合等により結合し、それによって高湿保存後でもブリードアウトを抑えることができるとともに、両性分散剤(E)によって粘着組成物を可塑化することができる。その結果、高湿保存後に高粘着力を有するとともに、高温環境下でも高保持力を有する粘着組成物を得ることができる。これに対して、酸価のみを有する分散剤を使用した場合、(メタ)アクリル系重合体(C)とフィラー(F)との接触は抑えられるが、粘着剤層を高湿保存した場合に(メタ)アクリル系重合体(C)が粘着剤層の表面にブリードアウトしやすくなり、粘着力が低下する。また、アミン価のみを有する分散剤を使用すると、分散剤がフィラー(F)に十分に被着しないため、安定性が低下する。 If an amphoteric dispersant (E) having an acid value and an amine value is used, even if the adhesive composition contains a filler (F) and a (meth) acrylic polymer (C), the amphoteric dispersant (E ) Adheres to the surface of the filler (F), the interaction between the (meth) acrylic polymer (C) and the filler (F) is suppressed, and thereby the stability of the pressure-sensitive adhesive composition can be improved. In addition, the adhesion of the dispersant to the surface of the filler (F) mainly functions in the acidic group portion of the polar group showing an acid value. The amphoteric dispersant (E) also has a basic group portion showing an amine value. Therefore, the basic group part is bonded to the polar group of the (meth) acrylic polymer (C) by an ionic bond or the like, whereby bleed-out can be suppressed even after high-humidity storage, and the amphoteric dispersant ( The adhesive composition can be plasticized by E). As a result, it is possible to obtain a pressure-sensitive adhesive composition having a high adhesive strength after high-humidity storage and a high holding power even under a high temperature environment. On the other hand, when a dispersant having only an acid value is used, contact between the (meth) acrylic polymer (C) and the filler (F) is suppressed, but when the pressure-sensitive adhesive layer is stored at high humidity. The (meth) acrylic polymer (C) tends to bleed out on the surface of the pressure-sensitive adhesive layer, and the adhesive strength is reduced. In addition, when a dispersant having only an amine value is used, the dispersant is not sufficiently adhered to the filler (F), so that the stability is lowered.
さらに、上記両性分散剤(E)は、直鎖状の主骨格を有し、主骨格の片末端のみに極性基を有するから、両性分散剤(E)とフィラー(F)との相互作用が少なく、それによって安定性の低下が抑えられる。これに対して、分散剤のフィラー(F)への被着を考えれば、複数の分岐鎖に酸性基部分及び塩基性基部分を有する極性基を備えた櫛形構造の分散剤を使用することも考えられるが、このような櫛形構造を有する分散剤を使用した場合、分散剤とフィラー(F)との相互作用が強くなりすぎ、また相溶性が低下して、寧ろ粘着組成物の安定性が低下しやすい。 Furthermore, since the amphoteric dispersant (E) has a linear main skeleton and a polar group only at one end of the main skeleton, the interaction between the amphoteric dispersant (E) and the filler (F) Less, thereby reducing stability degradation. On the other hand, considering the adhesion of the dispersant to the filler (F), a comb-shaped dispersant having a polar group having an acidic group portion and a basic group portion in a plurality of branched chains may be used. Although it is conceivable, when a dispersant having such a comb structure is used, the interaction between the dispersant and the filler (F) becomes too strong, the compatibility is lowered, and rather the stability of the adhesive composition. It tends to decline.
本実施の形態において、両性分散剤(E)の極性基としては、リン酸基とアンモニウム基とを有するリン酸エステル塩、硫酸基とアンモニウム基とを有する硫酸エステル塩などが挙げられ、これらの中でもリン酸エステル塩が好ましい。また、これらの極性基による酸価は、好ましくは10〜300mgKOH/g、より好ましくは14〜150mgKOH/g、さらに好ましくは77〜132mgKOH/gであり、アミン価は、好ましくは10〜300mgKOH/g、より好ましくは20〜150mgKOH/g、さらに好ましくは21〜74mgKOH/gである。なお、本明細書において、酸価とは、分散剤固形分1gを中和するのに必要なKOHのmg数を意味し、アミン価とは、分散剤固形分1gを中和するのに必要なHClに当量のKOHのmg数を意味する。 In the present embodiment, examples of the polar group of the amphoteric dispersant (E) include a phosphoric acid ester salt having a phosphoric acid group and an ammonium group, and a sulfuric acid ester salt having a sulfuric acid group and an ammonium group. Of these, phosphate ester salts are preferred. The acid value due to these polar groups is preferably 10 to 300 mgKOH / g, more preferably 14 to 150 mgKOH / g, still more preferably 77 to 132 mgKOH / g, and the amine value is preferably 10 to 300 mgKOH / g. More preferably, it is 20-150 mgKOH / g, More preferably, it is 21-74 mgKOH / g. In the present specification, the acid value means the number of mg of KOH necessary for neutralizing 1 g of the solid content of the dispersant, and the amine value is necessary for neutralizing 1 g of the solid content of the dispersant. Means the number of mg of KOH equivalent to HCl.
さらに、両性分散剤(E)の直鎖状の主骨格は、ポリエチレングリコールやポリプロピレングリコールなどのポリエーテル、及びポリエステルからなる群から選ばれる少なくとも1種のポリマー鎖からなることが好ましく、これらの中でも、ポリプロピレングリコールを含む主骨格がより好ましい。両性分散剤(E)がこのようなポリマー鎖を有する高分子系分散剤である場合、両性分散剤(E)の重量平均分子量は、好ましくは500〜3,000である。なお、本明細書において、重量平均分子量は、GPC(ゲルパーミエーションクロマトグラフィ)によるポリスチレン換算重量平均分子量を意味する(溶媒:テトラヒドロフラン)。市場で入手可能な両性分散剤(E)としては、具体的には、例えば、ビックケミー社製のDisperBYK−101、DisperBYK−106;楠本化成社製のDISPALON DA−325、DISPALON DA−234、DISPALON 300−257などが挙げられる。これらの中でも、水に対して不溶性を有し、使用される(メタ)アクリル酸アルキルエステル単官能単量体(A)及び極性基含有単官能単量体(B)の両方に対して可溶性を有するものがより好ましい。このような両性分散剤(E)は(メタ)アクリル酸アルキルエステル単官能単量体(A)及び極性基含有単官能単量体(B)の重合体との相溶性に優れているため、小粒径のフィラー(F)を高充填で含有する粘着組成物であっても、粘度の上昇が抑えられ、得られる粘着剤層に形成されるボイド等の発生を低減することができ、塗工性をさらに改善することができる。このような両性分散剤(E)としては、上記した主骨格にポリエチレングリコールを有する高分子量の両性分散剤が挙げられ、市場で入手可能なものとしては、上記のビックケミー社製のDisperBYK−106が挙げられる。 Furthermore, the linear main skeleton of the amphoteric dispersant (E) is preferably composed of at least one polymer chain selected from the group consisting of polyethers such as polyethylene glycol and polypropylene glycol, and polyesters. Among these, A main skeleton containing polypropylene glycol is more preferable. When the amphoteric dispersant (E) is a polymer dispersant having such a polymer chain, the amphoteric dispersant (E) preferably has a weight average molecular weight of 500 to 3,000. In addition, in this specification, a weight average molecular weight means the polystyrene conversion weight average molecular weight by GPC (gel permeation chromatography) (solvent: tetrahydrofuran). Specific examples of the amphoteric dispersant (E) available in the market include, for example, DisperBYK-101 and DisperBYK-10 6 manufactured by Big Chemie ; DISALON DA-325, DISPALON DA-234, DISPALON manufactured by Enomoto Kasei Co., Ltd. 300-257 and the like. Among these, it is insoluble in water and is soluble in both the (meth) acrylic acid alkyl ester monofunctional monomer (A) and the polar group-containing monofunctional monomer (B) used. What has is more preferable. Such an amphoteric dispersant (E) is excellent in compatibility with the polymer of the (meth) acrylic acid alkyl ester monofunctional monomer (A) and the polar group-containing monofunctional monomer (B). Even in a pressure-sensitive adhesive composition containing a small filler (F) with a small particle size, the increase in viscosity can be suppressed and the occurrence of voids and the like formed in the resulting pressure-sensitive adhesive layer can be reduced. Workability can be further improved. Examples of such an amphoteric dispersant (E) include high-molecular-weight amphoteric dispersants having polyethylene glycol in the main skeleton, and those available in the market include DisperBYK-106 manufactured by Big Chemie. Can be mentioned.
両性分散剤(E)の含有量は、フィラー(F)100質量部に対して、好ましくは0.5〜7.5質量部である。両性分散剤(E)の含有量が少なすぎると、安定性が低下したり、高湿保存後の粘着力が低下する傾向がある。一方、両性分散剤(E)の含有量が多すぎると、架橋密度が低下し、高温環境下での保持力が低下する傾向がある。 The content of the amphoteric dispersant (E) is preferably 0.5 to 7.5 parts by mass with respect to 100 parts by mass of the filler (F). When there is too little content of an amphoteric dispersing agent (E), there exists a tendency for stability to fall or for the adhesive force after high-humidity storage to fall. On the other hand, when there is too much content of an amphoteric dispersing agent (E), there exists a tendency for a crosslinking density to fall and for the retention power in a high temperature environment to fall.
次に、本実施の形態の他の粘着剤成分について具体的に説明する。
(メタ)アクリル酸アルキルエステル単官能単量体(A)としては、炭素数20以下のアルキル基を有する単官能単量体を使用することができ、具体的には、例えば、メチル(メタ)アクリレート、エチル(メタ)アクリレート、プロピル(メタ)アクリレート、ブチル(メタ)アクリレート、イソブチル(メタ)アクリレート、イソアミル(メタ)アクリレート、ヘキシル(メタ)アクリレート、2−エチルヘキシル(メタ)アクリレート、オクチル(メタ)アクリレート、イソオクチル(メタ)アクリレート、イソノニル(メタ)アクリレート、イソデシル(メタ)アクリレート、ラウリル(メタ)アクリレート、ペンタデシル(メタ)アクリレート、ヘキサデシル(メタ)アクリレート、ヘプタデシル(メタ)アクリレート、オクタデシル(メタ)アクリレートなどが挙げられる。これらは単独でまたは複数使用してもよいが、これらの中でも、ブチル(メタ)アクリレート、2−エチルヘキシル(メタ)アクリレート、及びイソオクチル(メタ)アクリレートからなる群から選ばれる少なくとも1種が好ましい。
Next, the other adhesive component of this Embodiment is demonstrated concretely.
As the (meth) acrylic acid alkyl ester monofunctional monomer (A), a monofunctional monomer having an alkyl group having 20 or less carbon atoms can be used. Specifically, for example, methyl (meth) Acrylate, ethyl (meth) acrylate, propyl (meth) acrylate, butyl (meth) acrylate, isobutyl (meth) acrylate, isoamyl (meth) acrylate, hexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, octyl (meth) Acrylate, isooctyl (meth) acrylate, isononyl (meth) acrylate, isodecyl (meth) acrylate, lauryl (meth) acrylate, pentadecyl (meth) acrylate, hexadecyl (meth) acrylate, heptadecyl (meth) acrylate, octade Such as Le (meth) acrylate. These may be used alone or in combination, and among these, at least one selected from the group consisting of butyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, and isooctyl (meth) acrylate is preferable.
(メタ)アクリル酸アルキルエステル単官能単量体(A)の含有量は、粘着剤成分全量中、好ましくは55〜90質量%であり、より好ましくは60〜85質量%である。(メタ)アクリル酸アルキルエステル単官能単量体(A)の含有量が上記範囲外では、粘着力が低下する傾向がある。 The content of the (meth) acrylic acid alkyl ester monofunctional monomer (A) is preferably 55 to 90% by mass and more preferably 60 to 85% by mass in the total amount of the pressure-sensitive adhesive component. When the content of the (meth) acrylic acid alkyl ester monofunctional monomer (A) is outside the above range, the adhesive strength tends to decrease.
極性基含有単官能単量体(B)としては、極性基と炭素数20以下のアルキル基とを有する単官能単量体を使用することができ、具体的には、例えば、(メタ)アクリル酸、イタコン酸、2−(メタ)アクリロイロキシエチルコハク酸、2−(メタ)アクリロイロキシエチルヘキサヒドロフタル酸、2−(メタ)アクリロイロキシエチルフタル酸などのカルボキシル基含有単官能単量体;2−ヒドロキシエチル(メタ)アクリレート、2−ヒドロキシプロピル(メタ)アクリレート、2−ヒドロキシブチル(メタ)アクリレート、2−(メタ)アクリロイロキシエチル−2−ヒドロキシエチルフタル酸などの水酸基含有単官能単量体;2−(メタ)アクリロイルオキシエチルアシッドフォスフェート、2−(メタ)メタクリロイルオキシエチルアシッドフォスフェートなどのリン酸基含有単官能単量体;ジメチルアミノエチル(メタ)アクリレート、ジエチルアミノエチル(メタ)アクリレートなどのアミノ基含有単官能単量体;(メタ)アクリロニトリルなどのニトリル基含有単官能単量体;N−ビニル−2−ピロリドンなどの窒素環含有単官能単量体などが挙げられる。これらは単独でまたは複数使用してもよいが、これらの中でも、反応性の官能基を有する架橋剤を添加することにより単量体が三次元架橋構造を形成し、高温環境下でも高い保持力を確保することができる、カルボキシル基含有単官能単量体、及び水酸基含有単官能単量体からなる群から選ばれる少なくとも1種が好ましい。 As the polar group-containing monofunctional monomer (B), a monofunctional monomer having a polar group and an alkyl group having 20 or less carbon atoms can be used. Specifically, for example, (meth) acrylic Monofunctional monofunctional carboxyl group such as acid, itaconic acid, 2- (meth) acryloyloxyethyl succinic acid, 2- (meth) acryloyloxyethyl hexahydrophthalic acid, 2- (meth) acryloyloxyethyl phthalic acid, etc. Hydroxyl content such as 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, 2- (meth) acryloyloxyethyl-2-hydroxyethylphthalic acid Monofunctional monomer; 2- (meth) acryloyloxyethyl acid phosphate, 2- (meth) methacryloyloxyethyl Phosphoric acid group-containing monofunctional monomers such as acid phosphate; Amino group-containing monofunctional monomers such as dimethylaminoethyl (meth) acrylate and diethylaminoethyl (meth) acrylate; Nitrile group-containing monomers such as (meth) acrylonitrile Functional monomers; nitrogen ring-containing monofunctional monomers such as N-vinyl-2-pyrrolidone These may be used alone or in combination, but among these, the monomer forms a three-dimensional cross-linking structure by adding a cross-linking agent having a reactive functional group, and has high holding power even in a high-temperature environment. Is preferably at least one selected from the group consisting of a carboxyl group-containing monofunctional monomer and a hydroxyl group-containing monofunctional monomer.
極性基含有単官能単量体(B)の含有量は、粘着剤成分全量中、好ましくは1〜15質量%であり、より好ましくは1〜8質量%である。極性基含有単官能単量体(B)の含有量が1質量%以上であれば、高湿保存後により高い粘着力を得ることができる。一方、極性基含有単官能単量体(B)の含有量が15質量%以下であれば、高温環境下でさらに高い保持力を得ることができる。 The content of the polar group-containing monofunctional monomer (B) is preferably 1 to 15% by mass and more preferably 1 to 8% by mass in the total amount of the pressure-sensitive adhesive component. When the content of the polar group-containing monofunctional monomer (B) is 1% by mass or more, higher adhesive strength can be obtained after high-humidity storage. On the other hand, if the content of the polar group-containing monofunctional monomer (B) is 15% by mass or less, higher holding power can be obtained in a high temperature environment.
(メタ)アクリル系重合体(C)としては、既述した(メタ)アクリル酸アルキルエステル単官能単量体(A)または(メタ)アクリル酸アルキルエステル単官能単量体(A)と極性基含有単官能単量体(B)とをモノマー成分として含有する重合体を用いることができ、これらの中でも、(メタ)アクリル酸アルキルエステル単官能単量体(A)とカルボキシル基含有単官能単量体との重合体がより好ましい。このような極性基を有する単量体をモノマー成分として用いることにより、金属製部材に対して高い粘着力が得られる一方、フィラー(F)との相互作用により粘着組成物の安定性が低下しやすいが、本実施の形態の粘着組成物は上記両性分散剤(E)を含有するため、安定性に優れた粘着組成物を得ることができる。また、(メタ)アクリル系重合体(C)は、(メタ)アクリル酸アルキルエステル単官能単量体(A)と同種の単量体をモノマー成分として含有することが好ましく、ブチル(メタ)アクリレート、2−エチルヘキシル(メタ)アクリレート、及びイソオクチル(メタ)アクリレートからなる群から選ばれる少なくとも1種の単量体をモノマー成分として含有することがより好ましい。 As the (meth) acrylic polymer (C), the aforementioned (meth) acrylic acid alkyl ester monofunctional monomer (A) or (meth) acrylic acid alkyl ester monofunctional monomer (A) and a polar group are used. A polymer containing a monofunctional monomer (B) as a monomer component can be used. Among these, a (meth) acrylic acid alkyl ester monofunctional monomer (A) and a carboxyl group-containing monofunctional monomer can be used. A polymer with a monomer is more preferred. By using such a monomer having a polar group as a monomer component, high adhesive strength can be obtained for a metal member, while the stability of the adhesive composition is reduced due to the interaction with the filler (F). Although it is easy, since the adhesive composition of this Embodiment contains the said amphoteric dispersant (E), the adhesive composition excellent in stability can be obtained. Further, the (meth) acrylic polymer (C) preferably contains a monomer of the same type as the (meth) acrylic acid alkyl ester monofunctional monomer (A) as a monomer component, and butyl (meth) acrylate. It is more preferable that at least one monomer selected from the group consisting of 2-ethylhexyl (meth) acrylate and isooctyl (meth) acrylate is contained as a monomer component.
(メタ)アクリル系重合体(C)の重量平均分子量は、好ましくは100,000以上であり、より好ましくは1,000,000〜3,000,000である。高分子量の重合体を用いることにより、高粘着力を有する粘着組成物を得ることができ、また、このような高分子量の重合体を用いても、本実施の形態の粘着組成物は上記両性分散剤(E)を含有するため、安定性に優れた粘着組成物を得ることができる。 The weight average molecular weight of the (meth) acrylic polymer (C) is preferably 100,000 or more, more preferably 1,000,000 to 3,000,000. By using a high molecular weight polymer, a pressure-sensitive adhesive composition having a high adhesive force can be obtained. Even when such a high molecular weight polymer is used, the pressure-sensitive adhesive composition of the present embodiment has the above amphoteric properties. Since the dispersant (E) is contained, an adhesive composition having excellent stability can be obtained.
(メタ)アクリル系重合体(C)の含有量は、粘着剤成分全量中、好ましくは1〜30質量%であり、より好ましくは3〜20質量%である。(メタ)アクリル系重合体(C)の含有量が1質量%以上であれば、高湿保存後により高い粘着力を得ることができる。一方、(メタ)アクリル系重合体(C)の含有量が30質量%以下であれば、粘着組成物がより低粘度となり、塗工不良をさらに低減することができる。 The content of the (meth) acrylic polymer (C) is preferably 1 to 30% by mass and more preferably 3 to 20% by mass in the total amount of the pressure-sensitive adhesive component. When the content of the (meth) acrylic polymer (C) is 1% by mass or more, higher adhesive strength can be obtained after high-humidity storage. On the other hand, when the content of the (meth) acrylic polymer (C) is 30% by mass or less, the pressure-sensitive adhesive composition has a lower viscosity, and coating defects can be further reduced.
(メタ)アクリル系重合体(C)を調製する方法としては、特に限定されず、従来公知の塊状重合法や溶液重合法を使用することができ、これらの中でも、(メタ)アクリル系重合体(C)を構成する単量体を媒質とし、溶剤の除去が不要な塊状重合法が好ましい。なお、(メタ)アクリル系重合体(C)は、予め重合した重合物の形態で使用してもよいし、塊状重合法を用いる場合、媒質である単量体中で重合した部分重合物の形態で使用してもよい。 The method for preparing the (meth) acrylic polymer (C) is not particularly limited, and a conventionally known bulk polymerization method or solution polymerization method can be used. Among these, the (meth) acrylic polymer is used. A bulk polymerization method in which the monomer constituting (C) is used as a medium and removal of the solvent is unnecessary is preferable. The (meth) acrylic polymer (C) may be used in the form of a polymer that has been polymerized in advance, or when using the bulk polymerization method, It may be used in the form.
開始剤(D)としては、光重合開始剤、及び熱重合開始剤からなる群から選ばれる少なくとも1種を使用できる。光重合開始剤としては、具体的には、例えば、2,4,6−トリメチルベンゾイルジフェニルホスフィンオキサイド(BASF社製,Lucirin TPO)、2,4,6−トリメチルベンゾイルフェニルエトキシホスフィンオキサイド(BASF社製,Lucirin TPO−L)などのアシルホスフィンオキサイド類;2−ベンジル−2−ジメチルアミノ−1−(4−モルフォリノフェニル)ブタノン−1(チバ社製,Irgacure 369)などのアミノケトン類;ビス(2,4,6−トリメチルベンゾイル)−フェニルホスフィンオキサイド(チバ社製,Irgacure 819)、ビス(2,6−ジメトキシベンゾイル)−2,4,4−トリメチルペンチルホスフィンオキサイド(チバ社製,CGI403)などのビスアシルホスフィンオキサイド類;ヒドロキシシクロヘキシルフェニルケトン(チバ社製,Irgacure 184)、ヒドロキシ−2−メチル−1−フェニル−プロパン−1−オン(チバ社製,Darocure 1173)などのヒドロキシケトン類;ベンゾフェノン、2,4,6−トリメチルベンゾフェノン、4−メチルベンゾフェノンなどのベンゾフェノン類;ベンジルメチルケタール(日本シーベルヘグナー社製,Esacure KB1);2−ヒドロキシ−2−メチル−[4−(1−メチルビニル)フェニル]プロパノールオリゴマー(日本シーベルヘグナー社製,Esacure KIP150)などが挙げられる。熱重合開始剤としては、具体的には、例えば、4,4’−アゾビス(4−シアノバレリック酸)、ジメチル2,2’−アゾビス(2−メチルプロピオネート)、2,2’−アゾビス(4−メトキシ−2,4−ジメチルバレロニトリル)、2,2’−アゾビス(2,4−ジメチルバレロニトリル)、2,2’−アゾビス(2−メチルプロピオニトリル)、2,2’−アゾビス(2−メチルブチロニトリル)、1,1’−アゾビス(シクロヘキサン−1−カルボニトリル)、1−[(1−シアノ−1−メチルエチル)アゾ]ホルムアミドなどのアゾ系の熱重合開始剤;クミルハイドロパーオキサイド、クミルパーオキシネオデカノエート、シクロヘキサノンパーオキサイド、1,1,3,3−テトラメチルブチルパーオキシネオデカネート、オクタノイルパーオキサイド、ラウロイルパーオキサイド、3,5,5−トリメチルヘキサノイルパーオキサイド、ベンゾイルパーオキサイド、t−ブチルパーピバレート、t−ブチルパーオキシ−2−エチルヘキサノエート、t−ブチルパーオキシイソブチレート、t−ブチルクミルパーオキサイド、t−ブチルパーオキシネオヘプタノエート、1,1−ビス(t−ヘキシルパーオキシ)シクロヘキサン、ジイソプロピルパーオキシジカルボネート、3−クロロ過安息香酸などの過酸化物系の熱重合開始剤などが挙げられる。 As the initiator (D), at least one selected from the group consisting of a photopolymerization initiator and a thermal polymerization initiator can be used. Specific examples of the photopolymerization initiator include 2,4,6-trimethylbenzoyldiphenylphosphine oxide (manufactured by BASF, Lucirin TPO), 2,4,6-trimethylbenzoylphenylethoxyphosphine oxide (manufactured by BASF). Acylphosphine oxides such as 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) butanone-1 (manufactured by Ciba, Irgacure 369); Bis (2 , 4,6-trimethylbenzoyl) -phenylphosphine oxide (manufactured by Ciba, Irgacure 819), bis (2,6-dimethoxybenzoyl) -2,4,4-trimethylpentylphosphine oxide (manufactured by Ciba, CGI403) Bisua Ruphophosphine oxides; Hydroxyketones such as hydroxycyclohexyl phenyl ketone (Ciba, Irgacure 184), hydroxy-2-methyl-1-phenyl-propan-1-one (Ciba, Darocur 1173); benzophenone, 2 , 4,6-trimethylbenzophenone, 4-methylbenzophenone and other benzophenones; benzylmethyl ketal (Nihon Sebel Hegner, Esacure KB1); 2-hydroxy-2-methyl- [4- (1-methylvinyl) phenyl] Examples include propanol oligomers (Esacure KIP150, manufactured by Nippon Sebel Hegner). Specific examples of the thermal polymerization initiator include 4,4′-azobis (4-cyanovaleric acid), dimethyl 2,2′-azobis (2-methylpropionate), and 2,2′-. Azobis (4-methoxy-2,4-dimethylvaleronitrile), 2,2′-azobis (2,4-dimethylvaleronitrile), 2,2′-azobis (2-methylpropionitrile), 2,2 ′ -Initiated thermal polymerization of azo compounds such as azobis (2-methylbutyronitrile), 1,1'-azobis (cyclohexane-1-carbonitrile), 1-[(1-cyano-1-methylethyl) azo] formamide Agents: Cumyl hydroperoxide, cumyl peroxyneodecanoate, cyclohexanone peroxide, 1,1,3,3-tetramethylbutylperoxyneodecanate, oct Noyl peroxide, lauroyl peroxide, 3,5,5-trimethylhexanoyl peroxide, benzoyl peroxide, t-butyl perpivalate, t-butylperoxy-2-ethylhexanoate, t-butylperoxyiso Peroxidation such as butyrate, t-butylcumyl peroxide, t-butylperoxyneoheptanoate, 1,1-bis (t-hexylperoxy) cyclohexane, diisopropylperoxydicarbonate, 3-chloroperbenzoic acid And physical thermal polymerization initiators.
開始剤(D)の含有量は、粘着剤成分全量中、好ましくは0.05〜5質量%であり、より好ましくは0.1〜3質量%である。開始剤(E)の含有量が0.05質量%以上であれば、高温環境下でより高い保持力を得ることができる。一方、開始剤(E)の含有量が5質量%以下であれば、低分子量成分の増加が抑えられ、高湿保存後により高い粘着力を得ることができる。 The content of the initiator (D) is preferably 0.05 to 5% by mass and more preferably 0.1 to 3% by mass in the total amount of the pressure-sensitive adhesive component. When the content of the initiator (E) is 0.05% by mass or more, higher holding power can be obtained in a high temperature environment. On the other hand, if the content of the initiator (E) is 5% by mass or less, an increase in low molecular weight components can be suppressed, and higher adhesive strength can be obtained after high-humidity storage.
本実施の形態の粘着剤組成物は、粘着剤成分の1つとして、さらに架橋剤を含有してもよい。このような架橋剤としては、分子内に架橋反応可能な官能基を有し、放射線の照射及び/又は加熱により(メタ)アクリル酸アルキルエステル単官能単量体(A)、極性基含有単官能単量体(B)、あるいはさらに架橋反応可能な極性基を有する(メタ)アクリル系重合体(C)と架橋反応し得るものが挙げられる。上記架橋反応可能な官能基としては、特に限定されないが、ビニル基、カルボキシル基、エポキシ基、イソシアネート基、水酸基などが挙げられる。このような架橋剤としては、具体的には、例えば、多官能重合性化合物、エポキシ系架橋剤、イソシアネート系架橋剤などが挙げられる。これらの中でも、ラジカル重合により架橋して、極性基含有単官能単量体(B)の極性基を減少させない、多官能重合性化合物が好ましい。 The pressure-sensitive adhesive composition of the present embodiment may further contain a crosslinking agent as one of the pressure-sensitive adhesive components. Such a cross-linking agent has a functional group capable of undergoing a cross-linking reaction in the molecule, and (meth) acrylic acid alkyl ester monofunctional monomer (A) or polar group-containing monofunctional by irradiation and / or heating. Examples thereof include those capable of undergoing a crosslinking reaction with the monomer (B) or the (meth) acrylic polymer (C) having a polar group capable of further crosslinking reaction. Although it does not specifically limit as said functional group which can be bridge | crosslinked, A vinyl group, a carboxyl group, an epoxy group, an isocyanate group, a hydroxyl group etc. are mentioned. Specific examples of such a crosslinking agent include polyfunctional polymerizable compounds, epoxy-based crosslinking agents, and isocyanate-based crosslinking agents. Among these, a polyfunctional polymerizable compound that is cross-linked by radical polymerization and does not reduce the polar group of the polar group-containing monofunctional monomer (B) is preferable.
多官能重合性化合物としては、分子内に(メタ)アクリレート基、アリル基、ビニル基などの重合可能な二重結合を2個以上有し、ラジカル重合し得る多官能モノマーや多官能オリゴマーを使用できる。具体的には、例えば、1,4−ブタンジオールジ(メタ)アクリレート、1,6−ヘキサンジオールジ(メタ)アクリレート、1,9−ノナンジオールジ(メタ)アクリレート、(ポリ)エチレングリコールジ(メタ)アクリレート、(ポリ)プロピレングリコールジ(メタ)アクリレート、ネオペンチルグリコールジ(メタ)アクリレート、ペンタエリスリトールジ(メタ)アクリレート、ペンタエリスリトールトリ(メタ)アクリレート、ペンタエリスリトールテトラ(メタ)アクリレート、トリメチロールプロパンジ(メタ)アクリレート、トリメチロールプロパントリ(メタ)アクリレート、アリル(メタ)アクリルレート、ビニル(メタ)アクリレート、ポリエステル(メタ)アクリレート、ウレタン(メタ)アクリレート、ウレタンジ(メタ)アクリレート、エポキシエステルジ(メタ)アクリレートなどが挙げられる。これらは単独でまたは複数使用してもよい。 As polyfunctional polymerizable compounds, use polyfunctional monomers and polyfunctional oligomers that have two or more polymerizable double bonds such as (meth) acrylate groups, allyl groups, and vinyl groups in the molecule and are capable of radical polymerization. it can. Specifically, for example, 1,4-butanediol di (meth) acrylate, 1,6-hexanediol di (meth) acrylate, 1,9-nonanediol di (meth) acrylate, (poly) ethylene glycol di ( (Meth) acrylate, (poly) propylene glycol di (meth) acrylate, neopentyl glycol di (meth) acrylate, pentaerythritol di (meth) acrylate, pentaerythritol tri (meth) acrylate, pentaerythritol tetra (meth) acrylate, trimethylol Propane di (meth) acrylate, trimethylolpropane tri (meth) acrylate, allyl (meth) acrylate, vinyl (meth) acrylate, polyester (meth) acrylate, urethane (meth) acrylate, urea Nji (meth) acrylate, epoxy ester di (meth) acrylate. These may be used alone or in combination.
エポキシ系架橋剤としては、分子内に2個以上のエポキシ基を有する化合物を使用できる。具体的には、例えば、ビスフェノールAエピクロルヒドリン型のエポキシ系樹脂、エチレングリシジルエーテル、ポリエチレングリコールジグリシジルエーテル、グリセリンジグリシジルエーテル、グリセリントリグリシジルエーテル、1,6−ヘキサンジオールグリシジルエーテル、トリメチロールプロパントリグリシジルエーテル、ジグリシジルアニリン、ジアミングリシジルアミン、N,N,N’,N’−テトラグリシジル−m−キシリレンジアミン、1,3−ビス(N,N’−ジアミングリシジルアミノメチル)シクロヘキサンなどが挙げられる。これらは単独でまたは複数使用してもよい。 As the epoxy-based crosslinking agent, a compound having two or more epoxy groups in the molecule can be used. Specifically, for example, bisphenol A epichlorohydrin type epoxy resin, ethylene glycidyl ether, polyethylene glycol diglycidyl ether, glycerin diglycidyl ether, glycerin triglycidyl ether, 1,6-hexanediol glycidyl ether, trimethylolpropane triglycidyl Examples include ether, diglycidyl aniline, diamine glycidyl amine, N, N, N ′, N′-tetraglycidyl-m-xylylenediamine, 1,3-bis (N, N′-diamine glycidylaminomethyl) cyclohexane, and the like. . These may be used alone or in combination.
イソシアネート系架橋剤としては、分子内に2個以上のイソシアネート基を有する化合物を使用できる。具体的には、例えば、トリレンジイソシアネート、ヘキサメチレンジイソシアネート、イソホロンジイソシアネート、キシリレンジイソシアネート、水添キシリレンジイソシアネート、ジフェニルメタンジイソシアネート、水添ジフェニルメタンジイソシアネート、テトラメチルキシリレンジイソシアネート、ナフタリンジイソシアネート、トリフェニルメタントリイソシアネート、ポリメチレンポリフェニルイソシアネート、及びこれらとトリメチロールプロパン等のポリオールとのアダクト体などが挙げられる。これらは単独でまたは複数使用してもよい。 As the isocyanate-based crosslinking agent, a compound having two or more isocyanate groups in the molecule can be used. Specifically, for example, tolylene diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate, xylylene diisocyanate, hydrogenated xylylene diisocyanate, diphenylmethane diisocyanate, hydrogenated diphenylmethane diisocyanate, tetramethylxylylene diisocyanate, naphthalene diisocyanate, triphenylmethane triisocyanate , Polymethylene polyphenyl isocyanate, and adducts of these with polyols such as trimethylolpropane. These may be used alone or in combination.
架橋剤の含有量は、粘着剤成分全量中、好ましくは0.05〜5質量%であり、より好ましくは0.1〜4質量%である。架橋剤の含有量が0.05質量%以上であれば、高温環境下でより高い保持力を得ることができる。一方、架橋剤の含有量が5質量%以下であれば、低分子量成分の増加が抑えられ、高湿保存後により高い粘着力を得ることができる。 The content of the crosslinking agent is preferably 0.05 to 5% by mass and more preferably 0.1 to 4% by mass in the total amount of the pressure-sensitive adhesive component. If content of a crosslinking agent is 0.05 mass% or more, higher holding power can be obtained in a high temperature environment. On the other hand, if the content of the crosslinking agent is 5% by mass or less, an increase in low molecular weight components can be suppressed, and higher adhesive strength can be obtained after high-humidity storage.
本実施の形態において、フィラー(F)としては、目的とする粘着テープの特性に合わせて、熱伝導性フィラー、導電性フィラー、断熱フィラー、絶縁性フィラーなどの各種のフィラーを使用できる。具体的には、例えば、水酸化アルミニウム、水酸化マグネシウム、炭酸カルシウム、炭酸マグネシウム、珪酸カルシウム、珪酸マグネシウム、酸化カルシウム、酸化マグネシウム、酸化亜鉛、酸化アルミニウム、結晶性シリカ、非結晶性シリカ、酸化チタン、酸化ニッケル、酸化鉄、酸化銅、窒化ホウ素、窒化アルミニウム、窒化珪素、カーボン、グラファイト、炭化珪素、ホウ酸アルミウイスカなどが挙げられる。これらは単独でまたは複数使用してもよい。フィラー(F)の含有量は、特に限定されるものではないが、粘着剤成分100質量部に対して、通常、50〜300質量部である。 In this Embodiment, various fillers, such as a heat conductive filler, a conductive filler, a heat insulation filler, an insulating filler, can be used as a filler (F) according to the characteristic of the target adhesive tape. Specifically, for example, aluminum hydroxide, magnesium hydroxide, calcium carbonate, magnesium carbonate, calcium silicate, magnesium silicate, calcium oxide, magnesium oxide, zinc oxide, aluminum oxide, crystalline silica, amorphous silica, titanium oxide Nickel oxide, iron oxide, copper oxide, boron nitride, aluminum nitride, silicon nitride, carbon, graphite, silicon carbide, aluminum borate whisker, and the like. These may be used alone or in combination. Although content of a filler (F) is not specifically limited, It is 50-300 mass parts normally with respect to 100 mass parts of adhesive components.
フィラー(F)は、所定厚さの粘着剤層を有する粘着テープを作製したときに、粘着剤層の厚さの50%以下の平均粒径を有するとともに、粘着剤層の厚さ以下の最大粒径を有するものが好ましい。このような平均粒径及び最大粒径を有するフィラー(F)であれば、塗工時のボイドやスジの発生をさらに低減することができる。 The filler (F) has an average particle diameter of 50% or less of the thickness of the pressure-sensitive adhesive layer and a maximum of the thickness of the pressure-sensitive adhesive layer or less when a pressure-sensitive adhesive tape having a pressure-sensitive adhesive layer is prepared. Those having a particle size are preferred. If it is a filler (F) which has such an average particle diameter and the largest particle diameter, generation | occurrence | production of the void at the time of coating and a stripe can be further reduced.
本実施の形態において、粘着組成物は、上記の粘着剤成分及びフィラー(F)を含有していれば、他の特性の向上を目的として、必要に応じて、粘着付与剤、着色剤、難燃剤、帯電防止剤などの公知の添加剤をさらに含有してもよい。 In the present embodiment, if the pressure-sensitive adhesive composition contains the above-mentioned pressure-sensitive adhesive component and filler (F), for the purpose of improving other properties, a tackifier, a colorant, a difficulty, as necessary. You may further contain well-known additives, such as a flame retardant and an antistatic agent.
本実施の形態の粘着組成物を製造する方法としては、従来公知の方法を使用することができる。例えば、上記(A)乃至(E)の各成分と、フィラー(F)とを従来公知の撹拌手段により混合する方法を採用することができる。また、塊状重合法により調製した(メタ)アクリル系重合体(C)を使用する場合、重合後に希釈剤として(メタ)アクリル酸アルキルエステル単量体(A)や極性基含有単官能単量体(B)を添加した重合体含有溶液を用いてもよい。 As a method for producing the pressure-sensitive adhesive composition of the present embodiment, a conventionally known method can be used. For example, a method of mixing the components (A) to (E) and the filler (F) with a conventionally known stirring means can be employed. Moreover, when using the (meth) acrylic-type polymer (C) prepared by the block polymerization method, (meth) acrylic-acid alkylester monomer (A) and a polar group containing monofunctional monomer as a diluent after superposition | polymerization You may use the polymer containing solution which added (B).
本実施の形態の粘着テープを製造する方法としては、従来公知の方法を使用することができる。例えば、上記のようにして得られる粘着組成物を基材の少なくとも一面上に塗工して粘着剤層を形成し、粘着剤層に放射線(X線、紫外線、電子線など)の照射及び/または粘着剤層を加熱することにより粘着テープを製造することができる。 As a method for producing the pressure-sensitive adhesive tape of the present embodiment, a conventionally known method can be used. For example, the pressure-sensitive adhesive composition obtained as described above is applied onto at least one surface of a substrate to form a pressure-sensitive adhesive layer, and the pressure-sensitive adhesive layer is irradiated with radiation (X-rays, ultraviolet rays, electron beams, etc.) and / or Or an adhesive tape can be manufactured by heating an adhesive layer.
基材としては、プラスチック製、金属製、紙製などの基材が挙げられ、これらの中でも、ポリエチレンテレフタレート、ポリプロピレンなどからなるプラスチック製基材が好ましい。これらの基材は、剥離性改良処理などの表面処理が施されていてもよい。粘着剤層の厚さは、粘着剤層を貼付した後の被着体の厚さを低減するために、好ましくは50〜250μmである。また、粘着剤層上にさらに剥離用シートを設けてもよい。放射線の照射手段としては、具体的には、例えば、ブラックライト、ケミカルランプ、低圧水銀ランプ、高圧水銀ランプ、メタルハライドランプなどが挙げられる。放射線として紫外線を使用する場合、紫外線の強度は、好ましくは約0.1〜10mW/cm2(波長:365nm)であり、照射時間は、好ましくは20秒間〜5分間である。 Examples of the base material include base materials such as plastic, metal, and paper. Among these, a plastic base made of polyethylene terephthalate, polypropylene, or the like is preferable. These base materials may be subjected to a surface treatment such as a peelability improving treatment. The thickness of the pressure-sensitive adhesive layer is preferably 50 to 250 μm in order to reduce the thickness of the adherend after applying the pressure-sensitive adhesive layer. Moreover, you may provide the sheet | seat for peeling further on an adhesive layer. Specific examples of the irradiation means include a black light, a chemical lamp, a low-pressure mercury lamp, a high-pressure mercury lamp, and a metal halide lamp. When ultraviolet rays are used as radiation, the intensity of the ultraviolet rays is preferably about 0.1 to 10 mW / cm 2 (wavelength: 365 nm), and the irradiation time is preferably 20 seconds to 5 minutes.
なお、粘着テープは、粘着剤層の上下面で被着体を強固に固定できる高い粘着力を有する必要があるが、貼り合わせ位置を誤ったり、貼り合せ面に異物が噛み込んだりした場合を考慮して、貼付直後においては、粘着剤層を被着体から剥離し、再度貼り合わせが可能となるようにリワーク性に優れていることが好ましい。本実施の形態の粘着組成物は、このようなリワーク性にも優れており、被着体に貼付された直後では、容易に粘着剤層を被着体から剥離可能な低い粘着力を有しながら、一定時間経過すると、高い粘着力を有する粘着剤層を形成できる。 The adhesive tape needs to have a high adhesive strength that can firmly fix the adherend on the upper and lower surfaces of the adhesive layer.However, if the bonding position is wrong or if foreign matter is caught in the bonding surface, Considering it, it is preferable that the adhesive layer is excellent in reworkability so that the pressure-sensitive adhesive layer is peeled off from the adherend and can be bonded again immediately after sticking. The pressure-sensitive adhesive composition of the present embodiment is also excellent in such rework properties, and has a low adhesive force that can easily peel the pressure-sensitive adhesive layer from the adherend immediately after being attached to the adherend. However, after a certain period of time, a pressure-sensitive adhesive layer having high adhesive strength can be formed.
以下、実施例によって本発明をさらに詳しく説明するが、本発明はこれら実施例に限定されるものではない。なお、以下において、「部」とあるのは、「質量部」を意味する。 EXAMPLES Hereinafter, although an Example demonstrates this invention further in detail, this invention is not limited to these Examples. In the following description, “part” means “part by mass”.
粘着組成物の各構成成分として、表1に示す(メタ)アクリル酸アルキルエステル単官能単量体、極性基含有単官能単量体、架橋剤、光重合開始剤、分散剤、及びフィラーを準備した。フィラーの最大粒径及び平均粒径は、レーザ回折式粒度分布計(マイクロトラックHRA)による測定値である。また、分散剤の水、及び各(メタ)アクリル系単量体に対する溶解性は、以下の評価によるものである。なお、表2中の略表示は、表1の種類欄の略表示と同一成分であることを示す。 As each component of the adhesive composition, the (meth) acrylic acid alkyl ester monofunctional monomer, polar group-containing monofunctional monomer, crosslinking agent, photopolymerization initiator, dispersant, and filler shown in Table 1 are prepared. did. The maximum particle size and the average particle size of the filler are values measured by a laser diffraction particle size distribution meter (Microtrac HRA). Moreover, the solubility with respect to the water of a dispersing agent and each (meth) acrylic-type monomer is based on the following evaluation. The abbreviations in Table 2 indicate the same components as the abbreviations in the type column of Table 1.
〔水に対する溶解性〕
不溶:室温下、水100g当たりの溶解量が、20g未満
可溶:室温下、水100g当たりの溶解量が、20g以上
[Solubility in water]
Insoluble: Dissolved amount per 100 g of water at room temperature is less than 20 g Soluble: Dissolved amount per 100 g of water at room temperature is 20 g or more
〔(メタ)アクリル系単量体に対する溶解性〕
不溶:室温下、各(メタ)アクリル系単量体100g当たりの溶解量が、20g未満
可溶:室温下、各(メタ)アクリル系単量体100g当たりの溶解量が、20g以上
[Solubility in (meth) acrylic monomers]
Insoluble: The dissolution amount per 100 g of each (meth) acrylic monomer is less than 20 g at room temperature. Soluble: The dissolution amount per 100 g of each (meth) acrylic monomer is 20 g or more at room temperature.
<(メタ)アクリル系重合体の調製>
温度計、撹拌プロペラ、冷却管、及び窒素ガス注入管が取り付けられた四つ口フラスコに、2−エチルヘキシルアクリレート(2EHA)450部、アクリル酸(AA)50部、及び、光重合開始剤として2−ベンジル−2−ジメチルアミノ−1−(4−モルフォリノフェニル)ブタノン−1(チバ社製,Irgacure 369)1.5部を投入し、容器内温度が50℃になるように容器を温調し、ブラックライトで紫外線(波長365nmにおける強度:5mW/cm2)を溶液に照射しながら30分間重合を行って、2EHAとAAとからなるアクリル系重合体(以下、Poly−2EHA/AAと略す)と、未反応分の2EHA及びAAとを含有するシロップを得た。得られたシロップ中のPoly−2EHA/AAの含有量は20質量%であり、重量平均分子量は100万であった。
<Preparation of (meth) acrylic polymer>
In a four-necked flask equipped with a thermometer, a stirring propeller, a condenser tube, and a nitrogen gas inlet tube, 450 parts of 2-ethylhexyl acrylate (2EHA), 50 parts of acrylic acid (AA), and 2 as a photopolymerization initiator -1.5 parts of benzyl-2-dimethylamino-1- (4-morpholinophenyl) butanone-1 (manufactured by Ciba, Irgacure 369) is added, and the temperature of the container is adjusted so that the temperature in the container becomes 50 ° C. Then, polymerization was performed for 30 minutes while irradiating the solution with ultraviolet light (intensity at wavelength of 365 nm: 5 mW / cm 2 ) with black light, and an acrylic polymer composed of 2EHA and AA (hereinafter abbreviated as Poly-2EHA / AA). And a syrup containing unreacted 2EHA and AA. The content of Poly-2EHA / AA in the obtained syrup was 20% by mass, and the weight average molecular weight was 1,000,000.
<粘着組成物の調製>
表2に示す配合量となるように各構成成分を混合撹拌し、各粘着組成物を調製した。なお、分散剤の配合量における括弧内の数値は、フィラー100部当たりの配合量である。
<Preparation of adhesive composition>
Each constituent component was mixed and stirred so as to have the blending amount shown in Table 2, and each adhesive composition was prepared. In addition, the numerical value in the parenthesis in the blending amount of the dispersant is the blending amount per 100 parts of the filler.
<粘着テープの作製>
上記で調製した各粘着組成物を剥離処理を施したポリエステルフィルム(厚さ:50μm)の一面上に表2に示す厚さとなるようにナイフコータにより塗工して、粘着剤層を形成し、さらにこの粘着剤層の上から剥離処理をしたポリエステルフィルム(厚さ:50μm)を気泡が入らないように重ね、粘着剤層の一面側から紫外線(波長365nmにおける強度:3mW/cm2)を2分間照射して、各粘着テープを作製した。
<Production of adhesive tape>
Each pressure-sensitive adhesive composition prepared above was coated on a surface of a polyester film (thickness: 50 μm) subjected to a release treatment with a knife coater so as to have the thickness shown in Table 2 to form a pressure-sensitive adhesive layer. The polyester film (thickness: 50 μm) that has been peeled from the pressure-sensitive adhesive layer is layered so that no bubbles enter, and ultraviolet light (intensity at a wavelength of 365 nm: 3 mW / cm 2 ) is applied for 2 minutes from one side of the pressure-sensitive adhesive layer. Irradiation was performed to prepare each adhesive tape.
上記のようにして得られた粘着組成物、及び粘着テープを用いて、以下の評価を行った。表3はこれらの評価結果を示す。 The following evaluation was performed using the adhesive composition and the adhesive tape obtained as described above. Table 3 shows these evaluation results.
〔安定性〕
B型粘度計(芝浦システム社製,単一筒型回転粘度計,ビストメロン)を用い、粘着組成物の調製直後の初期粘度(25℃)、粘着組成物を40℃で24時間保存した後の保存後粘度(25℃)、及び粘度の増減率を測定した。
〔Stability〕
Using a B-type viscometer (Shibaura System Co., Ltd., single-cylinder rotary viscometer, vistomer), the initial viscosity immediately after preparation of the adhesive composition (25 ° C.), and after storing the adhesive composition at 40 ° C. for 24 hours The viscosity after storage (25 ° C.) and the increase / decrease rate of the viscosity were measured.
〔粘着力〕
SUS304製の試験板上に粘着剤層を貼り合せた測定試料を作製した。この測定試料を23℃50%RHの環境下に24時間保存した後の初期粘着力と、65℃95%RHの高湿環境下に100時間保存した後の粘着テープを用い、同様にしてSUS304製の試験板上に粘着剤層を貼り合せた測定試料の保存後の粘着力とを、JIS Z 0237に準拠して測定した。
〔Adhesive force〕
A measurement sample in which an adhesive layer was bonded onto a SUS304 test plate was prepared. SUS304 was similarly used using the initial adhesive strength after storing this measurement sample in an environment of 23 ° C. and 50% RH for 24 hours and the adhesive tape after storage in a high humidity environment of 65 ° C. and 95% RH for 100 hours. The adhesive strength after storage of the measurement sample in which the pressure-sensitive adhesive layer was bonded onto the manufactured test plate was measured according to JIS Z 0237.
〔保持力〕
粘着力と同様にして作製した測定試料を用い、この測定試料を80℃及び120℃の高温環境下にそれぞれ168時間保存し、保存後の粘着剤層の保持力を、JIS Z 0237に準拠して測定して、以下の基準から保持力を評価した。
○:粘着剤層にズレが発生せず
×:粘着剤層にズレ及び落下が発生
[Retention force]
Using a measurement sample prepared in the same manner as the adhesive strength, this measurement sample was stored in a high-temperature environment of 80 ° C. and 120 ° C. for 168 hours, respectively. The retention strength of the adhesive layer after storage was in accordance with JIS Z 0237. The holding power was evaluated based on the following criteria.
○: Misalignment in the adhesive layer ×: Misalignment and fall in the adhesive layer
〔熱伝導率〕
総厚が1mmとなるように所定厚みに塗布した粘着テープを貼り合わせた測定試料を作製し、この測定試料の熱伝導率を迅速熱伝導率計(京都電子工業社製,QTM−500)で測定した。
〔Thermal conductivity〕
A measurement sample is prepared by sticking an adhesive tape applied to a predetermined thickness so that the total thickness is 1 mm, and the thermal conductivity of the measurement sample is measured with a rapid thermal conductivity meter (QTM-500, manufactured by Kyoto Electronics Industry Co., Ltd.). It was measured.
〔外観(スジ)〕
作製した粘着テープの粘着剤層を目視により観察し、粘着組成物が塗布されていない部分(スジ状の欠陥)があるかどうかを評価した。
[Appearance (Streak)]
The pressure-sensitive adhesive layer of the produced pressure-sensitive adhesive tape was visually observed to evaluate whether or not there was a portion (stripe-like defect) where the pressure-sensitive adhesive composition was not applied.
〔外観(ボイド)〕
作製した粘着テープの粘着剤層を光学顕微鏡(キーエンス社製、デジタルマイクロスコープ,VHX−500F)により観察し、粘着組成物が塗布されていない部分(ボイド)があるかどうかを評価した。
[Appearance (void)]
The pressure-sensitive adhesive layer of the produced pressure-sensitive adhesive tape was observed with an optical microscope (manufactured by Keyence Corporation, digital microscope, VHX-500F) to evaluate whether or not there was a part (void) to which the pressure-sensitive adhesive composition was not applied.
上記表に示すように、実施例の粘着組成物は、保存後の粘着組成物の粘度変化が少なく、外観上問題のない粘着剤層を形成できることが分かる。また、この粘着組成物は、高湿保存後でも高粘着力を有するだけでなく、高温環境下でも高保持力を有することが分かる。特に、水に不溶性を有し、使用した(メタ)アクリル酸アルキルエステル単官能単量体及び極性基含有単官能単量体の両方に可溶性を有する両性分散剤を用いた場合、小粒径のフィラーを用いたり、フィラーが高充填された粘着剤層を形成しても、塗工性に優れることが分かる。 As shown in the said table | surface, it turns out that the adhesive composition of an Example has little change of the viscosity of the adhesive composition after a preservation | save, and can form the adhesive layer which does not have a problem on an external appearance. Moreover, it turns out that this adhesive composition not only has a high adhesive force even after high-humidity storage, but also has a high holding power even in a high temperature environment. In particular, when using an amphoteric dispersant that is insoluble in water and soluble in both the (meth) acrylic acid alkyl ester monofunctional monomer and the polar group-containing monofunctional monomer, It can be seen that even if a filler is used or a pressure-sensitive adhesive layer highly filled with filler is formed, the coatability is excellent.
これに対して、両性分散剤を含有しない粘着組成物は、保存後に粘着組成物が増粘し、塗工不能となる程度まで粘着組成物がゲル化することが分かる。また、アミン価のみを有する分散剤や、酸価及びアミン価の両方を有していても、櫛形構造を有する分散剤を使用した場合、分散剤を使用しない場合と同様に、保存後に粘着組成物が増粘し、粘着組成物がゲル化することが分かる。これは、アミン価のみを有する分散剤を使用しても、フィラーと(メタ)アクリル系重合体との相互作用を十分に抑えることができないためと考えられる。また、櫛形構造を有する分散剤を使用した場合、分散剤とフィラーとの相互作用が大きくなるためと考えられる。 On the other hand, it can be seen that the pressure-sensitive adhesive composition containing no amphoteric dispersant is gelled to the extent that the pressure-sensitive adhesive composition thickens after storage and becomes unapplicable. In addition, when a dispersant having only an amine value, or a dispersant having both an acid value and an amine value, having a comb structure is used, the adhesive composition after storage is the same as when the dispersant is not used. It can be seen that the product thickens and the adhesive composition gels. This is presumably because the interaction between the filler and the (meth) acrylic polymer cannot be sufficiently suppressed even when a dispersant having only an amine value is used. In addition, it is considered that when a dispersant having a comb structure is used, the interaction between the dispersant and the filler is increased.
一方、酸価のみを有する分散剤を使用した場合、粘度変化は少ないが、高湿保存後の粘着力が顕著に低下することが分かる。これは、(メタ)アクリル系重合体が粘着剤層の表面にブリードアウトしたためと考えられる。 On the other hand, when a dispersant having only an acid value is used, the viscosity change is small, but it can be seen that the adhesive strength after high-humidity storage is significantly reduced. This is considered because the (meth) acrylic polymer bleeded out on the surface of the pressure-sensitive adhesive layer.
また、粘着組成物中に(メタ)アクリル系重合体を含有しない粘着組成物は、粘度が非常に低くなり、ナイフコータによる塗工時に粘着組成物が垂れてしまい、均一な厚みを有する粘着剤層を形成することができず、粘着組成物を安定に塗工することは困難であった。また、この粘着テープは粘着力や保持力が不十分であった。これは、粘着組成物中に(メタ)アクリル系重合体を含まないためと考えられる。従って、(メタ)アクリル系重合体を含まない粘着組成物は、塗工方法に応じた最適な粘度調整が非常に困難であり、それゆえ粘着組成物の設計及び塗工方法が制限されるだけでなく、特性的にも劣った。 Further, the pressure-sensitive adhesive composition containing no (meth) acrylic polymer in the pressure-sensitive adhesive composition has a very low viscosity, and the pressure-sensitive adhesive composition hangs down during coating with a knife coater, and has a uniform thickness. Thus, it was difficult to stably apply the pressure-sensitive adhesive composition. Moreover, this adhesive tape had insufficient adhesive strength and holding power. This is considered because the (meth) acrylic polymer is not included in the adhesive composition. Accordingly, the pressure-sensitive adhesive composition containing no (meth) acrylic polymer is very difficult to adjust the viscosity according to the coating method, and therefore, the design and coating method of the pressure-sensitive adhesive composition are only limited. In addition, it was inferior in characteristics.
なお、粘着剤層の厚さに対して最大粒径が大きなフィラーを用いると、塗工時に粘着剤層にスジが入ってしまい、外観不良となった。 When a filler having a maximum particle size with respect to the thickness of the pressure-sensitive adhesive layer was used, streaks entered the pressure-sensitive adhesive layer during coating, resulting in poor appearance.
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