JP2017149938A - Adhesive composition and adhesive tape using the same - Google Patents
Adhesive composition and adhesive tape using the same Download PDFInfo
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- JP2017149938A JP2017149938A JP2017024110A JP2017024110A JP2017149938A JP 2017149938 A JP2017149938 A JP 2017149938A JP 2017024110 A JP2017024110 A JP 2017024110A JP 2017024110 A JP2017024110 A JP 2017024110A JP 2017149938 A JP2017149938 A JP 2017149938A
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- sensitive adhesive
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- adhesive tape
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- 239000000203 mixture Substances 0.000 title claims abstract description 48
- 239000000853 adhesive Substances 0.000 title claims abstract description 37
- 239000002390 adhesive tape Substances 0.000 title claims abstract description 24
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 22
- 229920001400 block copolymer Polymers 0.000 claims abstract description 27
- 239000000523 sample Substances 0.000 claims abstract description 24
- 239000004014 plasticizer Substances 0.000 claims abstract description 18
- 239000011256 inorganic filler Substances 0.000 claims abstract description 14
- 229910003475 inorganic filler Inorganic materials 0.000 claims abstract description 14
- 239000004820 Pressure-sensitive adhesive Substances 0.000 claims description 56
- 229920005989 resin Polymers 0.000 claims description 26
- 239000011347 resin Substances 0.000 claims description 26
- 239000003208 petroleum Substances 0.000 claims description 22
- 239000000945 filler Substances 0.000 claims description 15
- -1 polypropylene Polymers 0.000 claims description 15
- 150000003505 terpenes Chemical class 0.000 claims description 15
- 235000007586 terpenes Nutrition 0.000 claims description 15
- 239000005011 phenolic resin Substances 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 13
- 235000013311 vegetables Nutrition 0.000 claims description 13
- 229920003002 synthetic resin Polymers 0.000 claims description 12
- 239000000057 synthetic resin Substances 0.000 claims description 12
- 239000004743 Polypropylene Substances 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 239000004793 Polystyrene Substances 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 4
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 4
- 229920002223 polystyrene Polymers 0.000 claims description 4
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 4
- 239000004800 polyvinyl chloride Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 abstract description 8
- 239000003795 chemical substances by application Substances 0.000 abstract 1
- 239000012939 laminating adhesive Substances 0.000 abstract 1
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 11
- 229920000346 polystyrene-polyisoprene block-polystyrene Polymers 0.000 description 11
- 239000013557 residual solvent Substances 0.000 description 11
- 239000000126 substance Substances 0.000 description 11
- 229910000019 calcium carbonate Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 239000011787 zinc oxide Substances 0.000 description 6
- 235000014692 zinc oxide Nutrition 0.000 description 6
- 238000005259 measurement Methods 0.000 description 5
- 229920001342 Bakelite® Polymers 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 229920000359 diblock copolymer Polymers 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- GPZYYYGYCRFPBU-UHFFFAOYSA-N 6-Hydroxyflavone Chemical compound C=1C(=O)C2=CC(O)=CC=C2OC=1C1=CC=CC=C1 GPZYYYGYCRFPBU-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000004637 bakelite Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Chemical compound CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 2
- NEHDRDVHPTWWFG-UHFFFAOYSA-N Dioctyl hexanedioate Chemical compound CCCCCCCCOC(=O)CCCCC(=O)OCCCCCCCC NEHDRDVHPTWWFG-UHFFFAOYSA-N 0.000 description 2
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 150000001278 adipic acid derivatives Chemical class 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 238000005227 gel permeation chromatography Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 229920000428 triblock copolymer Polymers 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229940058015 1,3-butylene glycol Drugs 0.000 description 1
- YEVQZPWSVWZAOB-UHFFFAOYSA-N 2-(bromomethyl)-1-iodo-4-(trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=C(I)C(CBr)=C1 YEVQZPWSVWZAOB-UHFFFAOYSA-N 0.000 description 1
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- PGIBJVOPLXHHGS-UHFFFAOYSA-N Di-n-decyl phthalate Chemical compound CCCCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCCCC PGIBJVOPLXHHGS-UHFFFAOYSA-N 0.000 description 1
- PYGXAGIECVVIOZ-UHFFFAOYSA-N Dibutyl decanedioate Chemical compound CCCCOC(=O)CCCCCCCCC(=O)OCCCC PYGXAGIECVVIOZ-UHFFFAOYSA-N 0.000 description 1
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 description 1
- ZVFDTKUVRCTHQE-UHFFFAOYSA-N Diisodecyl phthalate Chemical compound CC(C)CCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC(C)C ZVFDTKUVRCTHQE-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920002367 Polyisobutene Polymers 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000010425 asbestos Substances 0.000 description 1
- 150000001536 azelaic acids Chemical class 0.000 description 1
- 229940067597 azelate Drugs 0.000 description 1
- 235000019437 butane-1,3-diol Nutrition 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 150000001993 dienes Chemical group 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 239000000944 linseed oil Substances 0.000 description 1
- 235000021388 linseed oil Nutrition 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
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 235000012245 magnesium oxide Nutrition 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- JQCXWCOOWVGKMT-UHFFFAOYSA-N phthalic acid diheptyl ester Natural products CCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCC JQCXWCOOWVGKMT-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 239000010734 process oil Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000008262 pumice Substances 0.000 description 1
- 229910052895 riebeckite Inorganic materials 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000000790 scattering method Methods 0.000 description 1
- 150000003329 sebacic acid derivatives Chemical class 0.000 description 1
- 239000010454 slate Substances 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 229920001935 styrene-ethylene-butadiene-styrene Polymers 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
Landscapes
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
Description
本発明は、粘着剤面同士を貼り合わせた際、引き剥がしの粘着力（以下、自着力という）が大きく、粘着剤面のタックが低く、残溶剤が殆ど存在しない粘着剤組成物およびそれを用いた粘着テープに関する。 The present invention provides a pressure-sensitive adhesive composition having a large peel strength (hereinafter referred to as self-adhesive strength) when the pressure-sensitive adhesive surfaces are bonded to each other, low tackiness of the pressure-sensitive adhesive surface, and almost no residual solvent. It relates to the adhesive tape used.
生野菜類、生花類、書類、新聞、雑誌などの各種物品を結束するための粘着テープとして、結束する物品（被結束物）に対する粘着力が小さく、自着力が大きい粘着テープが汎用されている。 As an adhesive tape for bundling various items such as fresh vegetables, fresh flowers, documents, newspapers, magazines, etc., an adhesive tape that has a low adhesive force to a bundling article (bound object) and a large self-adhesive force is widely used. .
例えば、生野菜類などの結束用粘着テープとして、スチレンージエン系ブロック共重合体、粘着性付与剤、炭酸カルシウム、酸化亜鉛、酸化チタンなどの無機添加剤及び可塑剤を含有する粘着剤組成物を耐水性基材の片面に塗布してなる粘着テープが知られている（例えば、特許文献１、２）。 For example, adhesive tapes containing styrene-diene block copolymers, tackifiers, inorganic additives such as calcium carbonate, zinc oxide, titanium oxide and plasticizers as water-resistant adhesive tapes for bundling raw vegetables Adhesive tapes formed on one side of a conductive substrate are known (for example, Patent Documents 1 and 2).
上記のように、被結束物に対する粘着力が小さく、自着力が大きい結束用粘着テープについて、様々な提案がなされている。しかし、これらの結束用粘着テープは、溶剤系粘着剤が主流であったため、粘着剤中に溶剤が存在し、生野菜類などに貼り付けた場合は、問題となることがあった。 As described above, various proposals have been made for adhesive tapes for bundling that have a low adhesive force to a material to be bound and a large self-adhesive force. However, since these adhesive tapes are mainly solvent-based adhesives, there are cases where a solvent is present in the adhesives, which may cause problems when pasted on raw vegetables.
本発明は、粘着剤面同士を貼り合わせた際、引き剥がしの自着力が大きく、粘着剤面のタックが低く、残溶剤が殆ど存在しない粘着剤組成物およびそれを用いた粘着テープを提供することを目的とする。 The present invention provides a pressure-sensitive adhesive composition having a large self-adhesive strength for peeling off when the pressure-sensitive adhesive surfaces are bonded to each other, low tackiness of the pressure-sensitive adhesive surface, and almost no residual solvent, and a pressure-sensitive adhesive tape using the same. For the purpose.
すなわち、本発明は上記の課題を解決するために、以下の手段を採用する。
（１）ジブロック率が２０〜７０％であるスチレンージエン系ブロック共重合体１００質量部と、粘着性付与剤としてテルペンフェノール樹脂、または前記テルペンフェノール樹脂と石油樹脂との混合物６０〜１４０質量部と、充填剤として平均粒子径が１０μｍ以下の無機フィラー１０〜６０質量部及び可塑剤０〜１５質量部とを含有することを特徴とする粘着剤組成物。
（２）前記スチレンージエン系ブロック共重合体１００質量部に対して、前記粘着性付与剤８０〜１４０質量部と、前記無機フィラー２０〜６０質量部含有することを特徴とする（１）に記載の粘着剤組成物。
（３）合成樹脂製フィルムに、（１）または（２）に記載の粘着剤組成物を５〜５０μｍの厚みで塗布した粘着テープであって、自着力が６Ｎ／ｃｍ以上であり、粘着剤面のプローブタックが５０Ｎ／ｃｍ２以下であることを特徴とする粘着テープ。
（４）前記自着力が８Ｎ／ｃｍ以上であり、前記粘着剤面のプローブタックが３０Ｎ／ｃｍ２以下であることを特徴とする（３）に記載の粘着テープ。
（５）前記粘着性付与剤は、前記テルペンフェノール樹脂と前記石油樹脂の質量比が４：１〜１：２であることを特徴とする（３）または（４）に記載の粘着テープ。
（６）前記合成樹脂製フィルムが、ポリプロピレン、ポリエチレン、ポリエチレンテレフタレート、ポリスチレン及びポリ塩化ビニルの少なくとも一種類を含むことを特徴とする（３）〜（５）いずれか一項に記載の粘着テープ。
（７）野菜結束用である（３）〜（６）いずれか一項に記載の粘着テープ。
That is, the present invention employs the following means in order to solve the above problems.
(1) 100 parts by mass of a styrene-diene block copolymer having a diblock ratio of 20 to 70%, and 60 to 140 parts by mass of a terpene phenol resin or a mixture of the terpene phenol resin and petroleum resin as a tackifier A pressure-sensitive adhesive composition comprising 10 to 60 parts by mass of an inorganic filler having an average particle size of 10 μm or less and 0 to 15 parts by mass of a plasticizer as a filler.
(2) 80 to 140 parts by mass of the tackifier and 20 to 60 parts by mass of the inorganic filler are contained with respect to 100 parts by mass of the styrene-diene block copolymer. Adhesive composition.
(3) A pressure-sensitive adhesive tape in which the pressure-sensitive adhesive composition according to (1) or (2) is applied to a synthetic resin film in a thickness of 5 to 50 μm, and has a self-adhesive strength of 6 N / cm or more. A pressure-sensitive adhesive tape having a surface probe tack of 50 N / cm 2 or less.
(4) The pressure-sensitive adhesive tape according to (3), wherein the self-adhesion force is 8 N / cm or more and the probe tack on the pressure-sensitive adhesive surface is 30 N / cm 2 or less.
(5) The pressure-sensitive adhesive tape according to (3) or (4), wherein the tackifier has a mass ratio of the terpene phenol resin and the petroleum resin of 4: 1 to 1: 2.
(6) The pressure-sensitive adhesive tape according to any one of (3) to (5), wherein the synthetic resin film includes at least one of polypropylene, polyethylene, polyethylene terephthalate, polystyrene, and polyvinyl chloride.
(7) The adhesive tape according to any one of (3) to (6), which is for vegetable binding.
本発明は、特定のジブロック率のスチレンージエン系ブロック共重合体と、特定の粘着性付与剤、充填剤及び可塑剤を含む粘着剤組成物を、合成樹脂製フィルムに塗布することで、自着力が高く、粘着剤面のタックが低く残溶剤が殆ど存在しない粘着テープを提供する。この粘着テープは特に野菜結束用として使用した際、自着力が大きいため、輸送時のバラけることなく、また、結束物品（野菜）からの剥離も良好である。 The present invention provides a self-adhesive strength by applying a pressure-sensitive adhesive composition containing a specific diblock ratio styrene-diene block copolymer and a specific tackifier, filler and plasticizer to a synthetic resin film. The pressure-sensitive adhesive tape has a high tack, a low tackiness on the pressure-sensitive adhesive surface, and almost no residual solvent. When this adhesive tape is used especially for vegetable binding, it has a large self-adhesive force, so that it does not fluctuate during transportation, and it can be easily peeled off from the binding articles (vegetables).
本明細書における粘着剤組成物は、特定のジブロック率のスチレンージエン系ブロック共重合体と、特定の粘着性付与剤、充填剤及び可塑剤を含む。その粘着剤組成物を特定の合成樹脂製フィルムに塗布することで、粘着テープを得られる。 The pressure-sensitive adhesive composition in the present specification contains a styrene-diene block copolymer having a specific diblock ratio, a specific tackifier, a filler, and a plasticizer. An adhesive tape can be obtained by applying the adhesive composition to a specific synthetic resin film.
（スチレンージエン系ブロック共重合体）
本発明におけるスチレンージエン系ブロック共重合体は、スチレンーブタジエン系ブロック共重合体やスチレンーイソプレン系ブロック共重合体が挙げられ、これらの中のジエンユニットは部分的に、あるいは完全に水素化されていても良い。本発明に用いられるスチレンージエン系ブロック共重合体は、少なくともジブロック共重合体とトリブロック共重合体を含み、ジブロック率２０〜７０％、好ましくは、２５〜６０％であることを特徴とする。上記条件を満足することにより、本発明の粘着剤組成物として必要な自着力を得ることができる。ジブロック率が２０％より小さいと、粘着剤組成物として適度なタックが得られず好ましくない。また７０％より大きいと、適度な自着力が得られず好ましくない。
(Styrene-diene block copolymer)
Examples of the styrene-diene block copolymer in the present invention include a styrene-butadiene block copolymer and a styrene-isoprene block copolymer, in which the diene unit is partially or completely hydrogenated. May be. The styrene-diene block copolymer used in the present invention includes at least a diblock copolymer and a triblock copolymer, and has a diblock ratio of 20 to 70%, preferably 25 to 60%. . By satisfying the above conditions, the self-adhesive strength required for the pressure-sensitive adhesive composition of the present invention can be obtained. If the diblock rate is less than 20%, an appropriate tackiness cannot be obtained as the pressure-sensitive adhesive composition, which is not preferable. On the other hand, if it is larger than 70%, an appropriate self-adhesive force cannot be obtained, which is not preferable.
ジブロック率（％）は、１００×（ジブロック共重合体の質量部）／（ジブロック共重合体の質量部＋トリブロック共重合体の質量部）で算出することができる。ジブロック率は、具体的には、ゲル浸透クロマトグラフ（ＧＰＣ）法により、ＳＩＳ共重合体の分子量を測定し、得られたチャート中のジブロック共重合体に帰属されるピークと、トリブロック共重合体に帰属されるピークの面積比から算出することができる。ジブロック率を変化させる方法は、特に限定されないが、例えば、重合時に使用するカップリング剤量／開始剤量の比を変えたり、ジブロック率が異なる２種以上のＳＩＳ共重合体をブレンドしたりする方法が挙げられる。
スチレンージエン系ブロック共重合体の具体例としては、ＳＩＳ（日本ゼオン（株）製 クインタック（登録商標））、ＳＢＳ（ＪＳＲ ＴＲ）、ＳＥＢＳ（（株）クラレ製 セプトン（登録商標））等が挙げられる。
The diblock ratio (%) can be calculated by 100 × (part by weight of diblock copolymer) / (part by weight of diblock copolymer + part by weight of triblock copolymer). Specifically, the diblock rate is determined by measuring the molecular weight of the SIS copolymer by gel permeation chromatography (GPC) method, the peak attributed to the diblock copolymer in the obtained chart, and the triblock It can be calculated from the area ratio of peaks attributed to the copolymer. The method for changing the diblock ratio is not particularly limited. For example, the ratio of the amount of coupling agent / initiator used during polymerization is changed, or two or more SIS copolymers having different diblock ratios are blended. The method to do is mentioned.
Specific examples of the styrene-diene block copolymer include SIS (manufactured by Nippon Zeon Co., Ltd., Quintac (registered trademark)), SBS (JSR TR), SEBS (manufactured by Kuraray Co., Ltd., Septon (registered trademark)) and the like. It is done.
（粘着性付与剤）
本発明に用いられる粘着性付与剤はテルペンフェノール樹脂単体あるいは、テルペンフェノール樹脂と石油樹脂の混合物である。
(Tackifier)
The tackifier used in the present invention is a terpene phenol resin alone or a mixture of a terpene phenol resin and a petroleum resin.
本発明のテルペンフェノール樹脂は、市販品を使用することができる。タックと保持性のバランスからロジン変性率が５０〜８０ｍｏｌ％のものが好ましい。例としては住友ベークライト（株）製の「スミライトレジンＰＲ５１７３２（登録商標）」（融点１３０℃）、「スミライトレジンＰＲ１２６０３（登録商標）」（融点１３３℃）、等が挙げられる。 A commercial item can be used for the terpene phenol resin of this invention. A rosin modification rate of 50 to 80 mol% is preferred from the balance between tack and retention. Examples include “Sumilite Resin PR51732 (registered trademark)” (melting point: 130 ° C.), “Sumilite Resin PR12603 (registered trademark)” (melting point: 133 ° C.) manufactured by Sumitomo Bakelite Co., Ltd., and the like.
また、本発明に用いられる石油樹脂とは、Ｃ５石油樹脂、Ｃ９石油樹脂、Ｃ５Ｃ９石油樹脂やこれらを部分的に、あるいは完全に水素化した石油樹脂であり、これらの単数または複数を用いる。
Ｃ５石油樹脂の具体例としては、Ｔ−ＲＥＺ（東燃ゼネラル石油）、Ｃ５Ｃ９石油樹脂の具体例としては、クイントン（日本ゼオン（株）製（登録商標））、Ｃ９石油樹脂の具体例としてはペトコール（東ソー（株）製（登録商標））が挙げられる。
The petroleum resin used in the present invention is C5 petroleum resin, C9 petroleum resin, C5C9 petroleum resin or petroleum resin obtained by partially or completely hydrogenating these, and one or more of these are used.
Specific examples of C5 petroleum resin include T-REZ (TonenGeneral Sekiyu), specific examples of C5C9 petroleum resin include Quinton (manufactured by Nippon Zeon Co., Ltd. (registered trademark)), and specific examples of C9 petroleum resin include petol. (Registered trademark) manufactured by Tosoh Corporation.
粘着付与樹脂の配合割合は、スチレンージエン系ブロック共重合体１００質量部に対して、粘着性付与剤が６０〜１４０質量部、好ましくは８０〜１４０重量部である。粘着性付与剤を配合することにより、粘着剤組成物に自着力とタックを付与することができる。粘着性付与剤の量がこの範囲より外れると、自着力が弱くなり、タックが強くなる。 The compounding ratio of the tackifier resin is 60 to 140 parts by weight, preferably 80 to 140 parts by weight of the tackifier with respect to 100 parts by weight of the styrene-diene block copolymer. By blending the tackifier, self-adhesive strength and tack can be imparted to the adhesive composition. When the amount of the tackifier is out of this range, the self-adhesion force becomes weak and the tack becomes strong.
本発明の粘着剤組成物中における粘着性付与剤は、石油樹脂と混合して使用する場合、混合比率はテルペンフェノール樹脂と石油樹脂の質量比が４：１〜１：２、好ましくは３：１〜１：１の範囲である。 When the tackifier in the pressure-sensitive adhesive composition of the present invention is used by mixing with a petroleum resin, the mixing ratio is a mass ratio of terpene phenol resin and petroleum resin of 4: 1 to 1: 2, preferably 3: The range is 1-1: 1.
テルペンフェノール樹脂の比率がこの範囲より多くても、粘着剤組成物としては好ましく使用できる。
しかし、野菜等の結束テープ用途ではタックが低下し、野菜等の被着体に貼りつきにくくなるため好ましくない。
石油樹脂の比率がこの範囲より多くなると、粘着剤組成物のタックが向上しすぎて、野菜等の被着体に貼り付けて剥がした際、被着体を破損させることがあるために好ましくない。
Even if the ratio of the terpene phenol resin is larger than this range, it can be preferably used as the pressure-sensitive adhesive composition.
However, it is not preferable for binding tapes such as vegetables because tack is lowered and it is difficult to stick to adherends such as vegetables.
When the ratio of the petroleum resin exceeds this range, the tackiness of the pressure-sensitive adhesive composition is excessively improved, and it is not preferable because the adherend may be damaged when attached to an adherend such as vegetables and peeled off. .
（充填剤（無機フィラー））
本発明で用いられる無機フィラーとしては、例えば、炭酸カルシウム、亜鉛華（酸化亜鉛）、シリカ、けい酸アルミニウム、タルク、けい藻土、けい砂、軽石粉、スレート粉、雲母粉、アスベスト、アルミニウムゾル、アルミナホワイト、硫酸アルミニウム、硫酸バリウム、リトポン、硫酸カルシウム、二流化モリブデン、グラファイト、ガラス繊維、ガラス球、単結晶チタン酸カリ、カーボン繊維、活性亜鉛華、炭酸亜鉛、酸化マグネシウム、塩基性炭酸マグネシウム、リサージ、鉛丹、鉛白、水酸化カルシウム、活性化水酸化カルシウム、酸化チタン等が挙げられる。
(Filler (inorganic filler))
Examples of the inorganic filler used in the present invention include calcium carbonate, zinc white (zinc oxide), silica, aluminum silicate, talc, diatomaceous earth, silica sand, pumice powder, slate powder, mica powder, asbestos, and aluminum sol. , Alumina white, aluminum sulfate, barium sulfate, lithopone, calcium sulfate, disulfide molybdenum, graphite, glass fiber, glass sphere, single crystal potassium titanate, carbon fiber, activated zinc white, zinc carbonate, magnesium oxide, basic magnesium carbonate Resurge, red lead, lead white, calcium hydroxide, activated calcium hydroxide, titanium oxide and the like.
これらの無機フィラーの中で、炭酸カルシウム、亜鉛華、シリカ、酸化チタンなどが好ましい。これらの充填剤を配合すると、粘着剤に適度の凝集性を付与することができる。無機フィラーの平均粒子径は、１０μｍ以下、好ましくは８μｍ以下である。平均粒子径がこの範囲より大きいと、粘着剤組成物をフィルムに塗工した場合、粘着剤の塗工スジが発生しやすく、外観を損ねるために好ましくない。なお、フィラーの平均粒子径は、ビーカーに水、台所用中性洗剤、炭酸カルシウムを加えて試料とし、超音波で１分間分散処理して、島津製作所製ＳＡＬＤ−２２００を用いて、レーザー回折・散乱法により測定した。測定吸光度範囲の最小値を０．０１、最大値を０．２００として、６４回測定したときの平均値を求めた。 Among these inorganic fillers, calcium carbonate, zinc white, silica, titanium oxide and the like are preferable. When these fillers are blended, appropriate cohesiveness can be imparted to the pressure-sensitive adhesive. The average particle diameter of the inorganic filler is 10 μm or less, preferably 8 μm or less. When the average particle size is larger than this range, when the pressure-sensitive adhesive composition is applied to a film, a pressure-sensitive adhesive coating streaks are likely to occur and the appearance is impaired. The average particle diameter of the filler was determined by adding a sample of water, a neutral kitchen detergent, and calcium carbonate to a beaker, dispersing the sample with ultrasonic waves for 1 minute, and using a SALD-2200 manufactured by Shimadzu Corporation. It was measured by the scattering method. The average value when 64 measurements were taken with the minimum value of the measured absorbance range being 0.01 and the maximum value being 0.200 was determined.
無機フィラーの配合割合は、スチレンージエン系ブロック共重合体１００質量部に対して、１０〜６０質量部、好ましくは２０〜６０重量部である。１０質量部以下では、自着力が小さく、好ましくない。６０質量部を越えると、粘着剤組成物の凝集力が高くなりすぎて粘着加工が困難になり、物性が低下する。 The blending ratio of the inorganic filler is 10 to 60 parts by weight, preferably 20 to 60 parts by weight with respect to 100 parts by weight of the styrene-diene block copolymer. If it is 10 parts by mass or less, the self-adhesion force is small, which is not preferable. If it exceeds 60 parts by mass, the cohesive force of the pressure-sensitive adhesive composition becomes too high, making it difficult to perform pressure-sensitive adhesive processing and lowering the physical properties.
（可塑剤）
本発明における可塑剤としては、例えば、ジブチルフタレート、ジ−ｎ−オクチルフタレート、ビス−２−エチルヘキシルフタレート、ジ−ｎ−デシルフタレート、ジイソデシルフタレート等のフタル酸エステル類、ビス−２−エチルヘキシルアジペート、ジ−ｎ−オクチルアジペート等のアジピン酸エステル類、ビス−２−エチルヘキシルセバケート、ジ−ｎ−ブチルセバケート等のセバシン酸エステル類、ビス−２−エチルヘキシルアゼレート等のアゼライン酸エステル類等の脂肪酸エステル類、塩素化パラフィン等のパラフィン類、ポリプロピレングリコール等のグリコール類、エポキシ化大豆油、エポキシ化アマニ油等のエポキシ系高分子可塑剤、トリオクチルホスフェート、トリフェニルホスフェート等のリン酸エステル類、トリフェニルホスファイト等の亜リン酸エステル類、アジピン酸と１，３−ブチレングリコールとのエステル化物等のエステルオリゴマー類、ポリブテン、ポリイソブチレン、ポリイソプレン、プロセスオイル、ナフテン系オイルなどが挙げられ、これらは単独でまたは混合物で用いられる。好ましくは、ビス−２−エチルヘキシルアジペート、ジ−ｎ−オクチルアジペート等のアジピン酸エステル類やナフテン系オイルがよい。可塑剤の配合量は粘着剤組成物中のスチレンージエン系ブロック共重合体に対して１０質量部以下である。
(Plasticizer)
Examples of the plasticizer in the present invention include dibutyl phthalate, di-n-octyl phthalate, bis-2-ethylhexyl phthalate, di-n-decyl phthalate, diisodecyl phthalate and the like, bis-2-ethylhexyl adipate, Fatty acid esters such as adipic acid esters such as di-n-octyl adipate, sebacic acid esters such as bis-2-ethylhexyl sebacate, di-n-butyl sebacate, and azelaic acid esters such as bis-2-ethylhexyl azelate , Paraffins such as chlorinated paraffin, glycols such as polypropylene glycol, epoxy polymer plasticizers such as epoxidized soybean oil and epoxidized linseed oil, phosphate esters such as trioctyl phosphate and triphenyl phosphate, Phosphites such as phenyl phosphite, ester oligomers such as esterified product of adipic acid and 1,3-butylene glycol, polybutene, polyisobutylene, polyisoprene, process oil, naphthenic oil, etc. Are used alone or in a mixture. Adipic acid esters such as bis-2-ethylhexyl adipate and di-n-octyl adipate and naphthenic oils are preferable. The compounding quantity of a plasticizer is 10 mass parts or less with respect to the styrene-diene type block copolymer in an adhesive composition.
（粘着剤組成物）
本発明における粘着剤組成物は、前記の特定のジブロック率のスチレンージエン系ブロック共重合体と、特定の粘着性付与剤、充填剤及び可塑剤を混合することによって得る。
(Adhesive composition)
The pressure-sensitive adhesive composition in the present invention is obtained by mixing the styrene-diene block copolymer having the specific diblock ratio with a specific tackifier, filler and plasticizer.
従来の公知の製造方法では、スチレンージエン系ブロック共重合体と、粘着性付与剤と無機フィラーを例えばトルエン等の溶剤に溶解させて、粘着剤組成物を得る。得られた粘着剤組成物をフィルム上に塗工し、溶剤を乾燥させて粘着テープを得る。従って得られた粘着テープは数１０〜数１００ｐ．ｐ．ｍ．の残溶剤を含んでいる。 In a conventional known production method, a styrene-diene block copolymer, a tackifier and an inorganic filler are dissolved in a solvent such as toluene to obtain a pressure-sensitive adhesive composition. The obtained pressure-sensitive adhesive composition is coated on a film and the solvent is dried to obtain a pressure-sensitive adhesive tape. Therefore, the obtained adhesive tape has several 10 to several 100 p. p. m. Of residual solvent.
一方、本発明における粘着剤組成物は、溶剤を使用せず、例えば、ニーダールーダー、押出機にて、特定のジブロック率のスチレンージエン系ブロック共重合体と、特定の粘着性付与剤、充填剤及び可塑剤を加熱しながら混合することによって得る。
従って、残溶剤は、検出限界以下である。加熱温度は１３０〜１８０℃が好ましい。この範囲より低い温度であると充分攪拌されない場合があり、一方、これより高い温度だと攪拌中に熱劣化が起こる場合がある。
On the other hand, the pressure-sensitive adhesive composition in the present invention does not use a solvent, for example, a kneader-luder or an extruder, and a specific diblock ratio styrene-diene block copolymer, a specific tackifier, and a filler. And by mixing the plasticizer with heating.
Therefore, the residual solvent is below the detection limit. The heating temperature is preferably 130 to 180 ° C. If the temperature is lower than this range, the mixture may not be sufficiently stirred. On the other hand, if the temperature is higher than this range, thermal deterioration may occur during stirring.
前記粘着剤組成物を得る際、前工程で可塑剤とフィラーを混合し、ペースト状態にして使用しても良い。ペースト状態の混合物を得る方法としては可塑剤とフィラーを混合し、３本ロールミルにより混練する方法がある。
前記の特定のジブロック率のスチレンージエン系ブロック共重合体と、特定の粘着性付与剤、ペースト状混合物を加熱しながら混合することによって得られた粘着剤組成物は、フィラーの２次凝集が無くなり均一な混合物を得ることができるため、塗工の際、スジなどの発生が抑制でき平滑な塗工面を得られ都合が良い。
When obtaining the pressure-sensitive adhesive composition, a plasticizer and a filler may be mixed and used in a paste state in the previous step. As a method for obtaining a paste-like mixture, there is a method in which a plasticizer and a filler are mixed and kneaded by a three-roll mill.
The pressure-sensitive adhesive composition obtained by mixing the styrene-diene block copolymer having the specific diblock ratio, the specific tackifier, and the paste-like mixture with heating eliminates the secondary aggregation of the filler. Since a uniform mixture can be obtained, the occurrence of streaks or the like can be suppressed during coating, and a smooth coated surface can be conveniently obtained.
（合成樹脂製フィルム）
本発明の合成樹脂製フィルムは、材質がポリプロピレン、ポリエチレン、ポリエチレンテレフタレート、ポリスチレンまたはポリ塩化ビニルが挙げられ、いずれも良好な結果を得られる。
(Synthetic resin film)
Examples of the synthetic resin film of the present invention include polypropylene, polyethylene, polyethylene terephthalate, polystyrene, and polyvinyl chloride.
（粘着テープ）
粘着テープは、１００〜２００℃で溶融した粘着剤組成物をＴダイより押出し、合成樹脂フィルムに塗工することにより得られる。塗工速度は１０ｍ／分以上が好ましい。
(Adhesive tape)
The pressure-sensitive adhesive tape is obtained by extruding a pressure-sensitive adhesive composition melted at 100 to 200 ° C. from a T-die and applying it to a synthetic resin film. The coating speed is preferably 10 m / min or more.
粘着層の厚みは５〜５０μｍであり、より好ましくは１０〜４０μｍである。粘着剤厚みが５μｍ未満であると充分な自着力が得られない場合がある。一方、５０μｍを超えると、野菜等の被着体へ貼り付けて剥がした際、被着体を破損させることがある。 The thickness of the adhesive layer is 5 to 50 μm, more preferably 10 to 40 μm. If the pressure-sensitive adhesive thickness is less than 5 μm, sufficient self-adhesive strength may not be obtained. On the other hand, when it exceeds 50 μm, the adherend may be damaged when it is attached to an adherend such as vegetables and peeled off.
このようにして得られた粘着テープの自着力は以下のとおり、測定した。つまり、室温２３±２℃湿度５０±２％の室内にて、粘着テープを長手方向に幅２５ｍｍで長さ２５０ｍｍに短冊状に切り取り、粘着剤面同士を貼り付け、重さが２ｋｇのローラーで５０ｍｍ／ｍｉｎの速さで１往復圧着し試料とした。試料の両端を引張試験機にはさみ、Ｔ型に試験速度３００ｍｍ／ｍｉｎで剥離して測定した。 The self-adhesion force of the pressure-sensitive adhesive tape thus obtained was measured as follows. In other words, in a room with a room temperature of 23 ± 2 ° C and a humidity of 50 ± 2%, the adhesive tape is cut into strips with a width of 25 mm and a length of 250 mm in a longitudinal direction, and the adhesive surfaces are attached to each other with a roller weighing 2 kg. One reciprocal pressure bonding was performed at a speed of 50 mm / min to prepare a sample. Measurement was performed by sandwiching both ends of the sample with a tensile tester and peeling the sample onto a T shape at a test speed of 300 mm / min.
また、プローブタックは、室温２３±２℃湿度５０±２％の室内にて、（株）ユービーエム製のプローブタックテスターＴＡ５００を使用して測定した。測定条件は、押し付け時間を１秒、荷重４００ｇｆ／ｃｍ２、プローブの剥離速度は１０ｍｍ／秒とした。 The probe tack was measured using a probe tack tester TA500 manufactured by UBM Co., Ltd. in a room with a room temperature of 23 ± 2 ° C. and a humidity of 50 ± 2%. The measurement conditions were a pressing time of 1 second, a load of 400 gf / cm 2 , and a probe peeling speed of 10 mm / second.
残溶剤の測定は、ガスクロマトグラフ質量分析計（ＧＣＭＳ）を用いて行った。 The residual solvent was measured using a gas chromatograph mass spectrometer (GCMS).
以下に、表１及び２を参照しつつ、実施例、比較例、参考例を挙げて本発明を詳細に説明する。これらはいずれも例示的なものであって、本発明の内容を限定するものではない。
本実施例で使用した成分を以下に示す。
（Ａ）スチレン−ジエン系ブロック共重合体
（Ａ１）ＳＩＳブロック共重合体（日本ゼオン製「クインタック３４３３Ｎ」、ジブロック率５０％）
（Ａ２）ＳＩＳブロック共重合体（日本ゼオン製「クインタック３４２１」、ジブロック率２５％）
（Ａ３）ＳＩＳブロック共重合体（日本ゼオン製「クインタックＳＬ−１６５」、ジブロック率６０％）
（Ａ４）ＳＩＳブロック共重合体（日本ゼオン製「クインタック３２８０」、ジブロック率１８％）
（Ａ５）ＳＩＳブロック共重合体（日本ゼオン製「クインタック３５２０」、ジグロック率７８％）
（Ｂ）粘着性付与剤
（Ｂ１）テルペンフェノール（住友ベークライト製「ＰＲ−１２６０３」）
（Ｂ２）Ｃ５Ｃ９石油樹脂（日本ゼオン製「クイントンＳ−１９５」）
（Ｂ３）Ｃ５石油樹脂（東燃ゼネラル石油製「Ｔ−ＲＥＺ ＲＣ１００」）
（Ｂ４）Ｃ９石油樹脂（東ソー製「ペトコール１２０」）
（Ｂ５）水添Ｃ９石油樹脂（荒川化学製「アルコンＰ−１１５」）
（Ｃ）充填剤（無機フィラー）
（Ｃ１Ａ）炭酸カルシウム（竹原化学製「ネオライトＳＰ」 平均粒子径０．２μｍ）
（Ｃ１Ｂ）炭酸カルシウム（白石カルシウム製 「ＢＦ−３００」 平均粒子径８μｍ）
（Ｃ２）酸化チタン（堺化学工業「ＴＩＴＯＮＥ Ｒ−１１Ｐ」 平均粒子径０．２μｍ）
（Ｃ３）酸化亜鉛（堺化学工業 酸化亜鉛 平均粒子径１μｍ）
（Ｃ４）硫酸バリウム（竹原化学製「ＳＴ−１」 平均粒子径０．１５μｍ）
（Ｃ５）シリカ（ＤＳＬジャパン製「カープレックス♯８０」 平均粒径５μｍ）
（Ｄ）可塑剤 アジピン酸ジイソノニル（モノサイザーＷ２４２ ＤＩＣ製）
（Ｅ）合成樹脂フィルム
（Ｅ１）ポリプロピレンフィルム（フタムラ化学製 ＦＯＳ−ＢＴ）
（Ｅ２）ポリエチレンフィルム（フタムラ化学製 ＬＬ−ＲＰ２）
（Ｅ３）ポリエチレンテレフタレートフィルム（フタムラ化学製 ＦＥ２００２）
（Ｅ４）ポリスチレンフィルム（大石産業製 スチロファンＳＰＨ）
（Ｅ５）ポリ塩化ビニルフィルム（三菱樹脂製 アルトロン♯２８００）
（実施例１）
スチレンーイソプレンースチレンブロックコポリマー（日本ゼオン製「クインタック３４３３Ｎ」、ジブロック率５０％）１００質量部と、テルペンフェノール樹脂（住友ベークライト製「ＰＲ−１２６０３」）５０質量部と、Ｃ５Ｃ９石油樹脂（日本ゼオン製「クイントンＳ−１９５」）５０質量部と、可塑剤としてアジピン酸ジイソノニル１０質量部と、炭酸カルシウム（竹原化学製「ネオライトＳＰ」、平均粒子径０．２μｍ）４０質量部と、酸化防止剤（イルガノックス１０１０）３質量部とを、１７０℃に加熱されたニーダーにて６０分間混練し、粘着剤組成物を得た。
得られた粘着剤組成物を１７０℃にてメルターで溶解させ、Ｔダイより粘着剤組成物を押し出して、合成樹脂フィルム（ポリプロピレン フタムラ化学製 ＦＯＳ‐ＢＴ）に粘着剤厚みが３０μｍになるように塗工し、粘着テープを得た。
Hereinafter, the present invention will be described in detail with reference to Tables 1 and 2 with reference to Examples, Comparative Examples, and Reference Examples. These are all illustrative and do not limit the contents of the present invention.
The components used in this example are shown below.
(A) Styrene-diene block copolymer (A1) SIS block copolymer ("Quintac 3433N" manufactured by Nippon Zeon, diblock ratio 50%)
(A2) SIS block copolymer ("Quintac 3421" manufactured by Zeon Corporation, diblock rate 25%)
(A3) SIS block copolymer ("Quintac SL-165" manufactured by Zeon Corporation, diblock rate 60%)
(A4) SIS block copolymer (manufactured by Nippon Zeon "Quintac 3280", diblock rate 18%)
(A5) SIS block copolymer (manufactured by Nippon Zeon "Quintac 3520", jiglock rate 78%)
(B) Tackifier (B1) Terpenephenol ("PR-12603" manufactured by Sumitomo Bakelite)
(B2) C5C9 petroleum resin (“Quinton S-195” manufactured by Nippon Zeon)
(B3) C5 petroleum resin ("T-REZ RC100" manufactured by TonenGeneral Sekiyu)
(B4) C9 Petroleum Resin (“Petocol 120” manufactured by Tosoh)
(B5) Hydrogenated C9 petroleum resin ("Arcon P-115" manufactured by Arakawa Chemical)
(C) Filler (inorganic filler)
(C1A) Calcium carbonate (Takehara Chemical “Neolite SP” average particle size 0.2 μm)
(C1B) Calcium carbonate ("BF-300" manufactured by Shiraishi Calcium, average particle diameter of 8 μm)
(C2) Titanium oxide (Sakai Chemical Industry “TITONE R-11P” average particle size 0.2 μm)
(C3) Zinc oxide (Sakai Chemical Industry Zinc Oxide average particle size 1μm)
(C4) Barium sulfate (“ST-1”, average particle diameter of 0.15 μm, manufactured by Takehara Chemical)
(C5) Silica (manufactured by DSL Japan “Carplex # 80” average particle size 5 μm)
(D) Plasticizer diisononyl adipate (manufactured by Monosizer W242 DIC)
(E) Synthetic resin film (E1) Polypropylene film (FOS-BT manufactured by Futamura Chemical)
(E2) Polyethylene film (LL-RP2 manufactured by Futamura Chemical)
(E3) Polyethylene terephthalate film (FE2002 made by Phutamura Chemical)
(E4) Polystyrene film (Styrophane SPH from Oishi Sangyo)
(E5) Polyvinyl chloride film (Mitsubishi Resin Altron # 2800)
Example 1
100 parts by mass of a styrene-isoprene-styrene block copolymer (“Quintac 3433N” manufactured by Zeon Corporation, 50% diblock ratio), 50 parts by mass of a terpene phenol resin (“PR-12603” manufactured by Sumitomo Bakelite), and a C5C9 petroleum resin ( 50 parts by mass of “Quinton S-195” manufactured by ZEON, 10 parts by mass of diisononyl adipate as a plasticizer, 40 parts by mass of calcium carbonate (“Neolite SP” manufactured by Takehara Chemical, average particle size 0.2 μm), and oxidation 3 parts by mass of an inhibitor (Irganox 1010) was kneaded for 60 minutes with a kneader heated to 170 ° C. to obtain an adhesive composition.
The obtained pressure-sensitive adhesive composition was melted with a melter at 170 ° C., and the pressure-sensitive adhesive composition was extruded from a T-die so that the thickness of the pressure-sensitive adhesive was 30 μm on a synthetic resin film (FOS-BT manufactured by Polypropylene Phutamura Chemical). Coating was performed to obtain an adhesive tape.
得られた粘着テープは次のようにして評価した。
（自着力）
室温２３±２℃湿度５０±２％の室内にて、粘着テープを長手方向に幅２５ｍｍで長さ２５０ｍｍに短冊状に切り取り、粘着剤面同士を貼り付け、重さが２ｋｇのローラーで５０ｍｍ／ｍｉｎの速さで１往復圧着し試料とした。試料の両端を引張試験機にはさみ、Ｔ型に試験速度３００ｍｍ／ｍｉｎで剥離して自着力を測定した。
The obtained adhesive tape was evaluated as follows.
(Self-adhesion)
In a room with a room temperature of 23 ± 2 ° C and a humidity of 50 ± 2%, the adhesive tape is cut into strips of 25 mm in width and 250 mm in length, and the adhesive surfaces are attached to each other. One reciprocal pressure bonding was performed at a speed of min to prepare a sample. Both ends of the sample were sandwiched between tensile testers, peeled off from the T-type at a test speed of 300 mm / min, and the self-adhesion force was measured.
（プローブタック）
プローブタックは、室温２３±２℃湿度５０±２％の室内にて、（株）ユービーエム製のプローブタックテスターＴＡ５００を使用して測定した。測定条件は、押し付け時間を１秒、荷重４００ｇｆ／ｃｍ２、プローブの剥離速度は１０ｍｍ／秒とした。
(Probe tack)
The probe tack was measured in a room with a room temperature of 23 ± 2 ° C. and a humidity of 50 ± 2% using a probe tack tester TA500 manufactured by UBM. The measurement conditions were a pressing time of 1 second, a load of 400 gf / cm 2 , and a probe peeling speed of 10 mm / second.
（残溶剤）
残溶剤の測定は、ガスクロマトグラフ質量分析計（ＧＣＭＳ）を用いて行い、下記のとおりとした。ＧＣＭＳは、Ａｇｌｉｅｎｔ ７８９０Ａおよび５９７５Ｃ ＭＳＤを使用し、カラムは ＤＢ−１を使用した。試料の前処理手順は次の通りとした。
（前処理手順）
（１）テープ試料を約４ｇ精秤し、フタ付き試験管に入れた。
（２）モノクロロベンゼンを２０ｍＬ加えて、振動させ、２４ｈｒｓ放置した。
（３）抽出液をガラス製パスツールピペットで採取して、オートサンプラバイアル瓶に注入し、測定に供した。
表１〜３に、実施例１〜３１、比較例１〜７、参考例１の粘着剤組成物等の配合等を示す。
(Residual solvent)
The residual solvent was measured using a gas chromatograph mass spectrometer (GCMS) as follows. GCMS used Agilent 7890A and 5975C MSD and the column used DB-1. The sample pretreatment procedure was as follows.
(Pre-processing procedure)
(1) About 4 g of the tape sample was precisely weighed and placed in a test tube with a lid.
(2) 20 mL of monochlorobenzene was added, vibrated and left for 24 hrs.
(3) The extract was collected with a glass Pasteur pipette, poured into an autosampler vial, and used for measurement.
Tables 1 to 3 show the compositions of the pressure-sensitive adhesive compositions of Examples 1 to 31, Comparative Examples 1 to 7, and Reference Example 1 and the like.
実施例３１は、実施例１において前工程でアジピン酸ジイソノニル１０質量部と炭酸カルシウム（竹原化学工業製「ネオライトＳＰ」、平均粒子径０．２μｍ）４０質量部を混合し、３本ロールミルにより混練することでペーストを得た。その後、スチレンーイソプレンースチレンブロックコポリマー（日本ゼオン製「クインタック３４３３Ｎ」、ジブロック率５０％）１００質量部と、テルペンフェノール樹脂（住友ベークライト製「ＰＲ−１２６０３」）７０質量部と、Ｃ５Ｃ９石油樹脂（日本ゼオン製「クイントンＳ−１９５」）４０質量部と、酸化防止剤（イルガノックス１０１０）３質量部と、前記で得られたペースト５０質量部とを、１７０℃に加熱されたニーダーにて６０分間混練し、粘着剤組成物を得た。それ以外は実施例１と同様にして粘着テープを得た。 In Example 31, 10 parts by mass of diisononyl adipate and 40 parts by mass of calcium carbonate (“Neolite SP” manufactured by Takehara Chemical Industry Co., Ltd., average particle size 0.2 μm) were mixed in the previous step in Example 1 and kneaded by a three roll mill. A paste was obtained. Thereafter, 100 parts by mass of a styrene-isoprene-styrene block copolymer (“Quintac 3433N” manufactured by Nippon Zeon Co., Ltd., 50% diblock), 70 parts by mass of a terpene phenol resin (“PR-12603” manufactured by Sumitomo Bakelite), and C5C9 petroleum 40 parts by mass of resin (“Quinton S-195” manufactured by Nippon Zeon), 3 parts by mass of antioxidant (Irganox 1010), and 50 parts by mass of the paste obtained above were added to a kneader heated to 170 ° C. And kneaded for 60 minutes to obtain an adhesive composition. Other than that was carried out similarly to Example 1, and obtained the adhesive tape.
表１〜３に示すように、スチレンージエン系ブロック共重合体を使用した粘着剤組成物において、スチレンージエン系共重合体のジブロック率が特定の範囲内であり且つ粘着性付与剤としてテルペンフェノール樹脂を使用しており且つ充填剤として無機フィラーが特定の範囲内である全ての実施例では自着力が６Ｎ／ｃｍ以上であり、且つプローブタックが５０Ｎ／ｃｍ２以下であった。従って、生野菜類などの各種物品を結束するための粘着テープとして用いた際、自着力が大きいため輸送時等にバラケがおこらず、結束する物品（野菜）からの剥離が良好であると考えられる。また、残溶剤も検出限界以下であった。 As shown in Tables 1 to 3, in the pressure-sensitive adhesive composition using the styrene-diene block copolymer, the diblock ratio of the styrene-diene copolymer is within a specific range, and a terpene phenol resin is used as a tackifier. In all of the examples that were used and the inorganic filler was in a specific range as a filler, the self-adhesion force was 6 N / cm or more and the probe tack was 50 N / cm 2 or less. Therefore, when used as a pressure-sensitive adhesive tape for bundling various items such as raw vegetables, it is considered that the self-adhesion force is large, so that there will be no looseness during transportation, and the peeling from the bundling items (vegetables) will be good. It is done. The residual solvent was also below the detection limit.
比較例１、２はスチレンージエン系のジブロック率が範囲から外れるため、自着力が低い結果となった。
比較例３は粘着性付与剤にテルペンフェノールを使用しなかったので、自着力が低い結果となった。
比較例４は可塑剤の量が、範囲からよりも過大であるため、プローブタックの値が大きくなった。
比較例５はフィラーの添加量が範囲より多いため、硬くなりすぎて混練できず、粘着剤が得られなかった。
比較例６は粘着性付与剤の量を範囲より少なくしたため、十分な自着力が得られなかった。
比較例７は粘着性付与剤の量を範囲より多くしたため、タックが大きすぎた。
参考例１は溶剤に溶解させて作成した粘着剤組成物を用いた粘着テープであるため、残溶剤が多かった。
In Comparative Examples 1 and 2, the styrene-diene-based diblock ratio was out of the range, and thus the self-adhesion force was low.
Since the comparative example 3 did not use terpene phenol for a tackifier, it resulted in a low self-adhesion force.
In Comparative Example 4, since the amount of the plasticizer was excessive from the range, the probe tack value was large.
In Comparative Example 5, since the amount of filler added was larger than the range, it was too hard to knead and an adhesive could not be obtained.
In Comparative Example 6, since the amount of the tackifier was less than the range, sufficient self-adhesive strength could not be obtained.
In Comparative Example 7, since the amount of the tackifier was larger than the range, the tack was too large.
Since Reference Example 1 was an adhesive tape using an adhesive composition prepared by dissolving in a solvent, there were many residual solvents.
本発明は、特定のジブロック率のスチレンージエン系ブロック共重合体と、特定の粘着性付与剤、可塑剤及び無機フィラーを含む粘着剤組成物は、合成樹脂製フィルムに塗布することで、自着力が高く、粘着剤面のプローブタックが低く残溶剤が殆ど存在しない粘着テープを提供する。 In the present invention, a styrene-diene block copolymer having a specific diblock ratio and a pressure-sensitive adhesive composition containing a specific tackifier, a plasticizer, and an inorganic filler are applied to a synthetic resin film, thereby self-adhesion. The pressure-sensitive adhesive tape has a low probe tack on the adhesive surface and almost no residual solvent.
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