JP2012179888A - Polyester film for substrate-less double-sided adhesive sheet - Google Patents
Polyester film for substrate-less double-sided adhesive sheet Download PDFInfo
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- JP2012179888A JP2012179888A JP2011069055A JP2011069055A JP2012179888A JP 2012179888 A JP2012179888 A JP 2012179888A JP 2011069055 A JP2011069055 A JP 2011069055A JP 2011069055 A JP2011069055 A JP 2011069055A JP 2012179888 A JP2012179888 A JP 2012179888A
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- polyester film
- release
- peeling force
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- 229920006267 polyester film Polymers 0.000 title claims abstract description 41
- 239000000853 adhesive Substances 0.000 title abstract description 16
- 230000001070 adhesive effect Effects 0.000 title abstract description 16
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229920002050 silicone resin Polymers 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 11
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 8
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 6
- 125000003342 alkenyl group Chemical group 0.000 claims abstract description 5
- 125000000524 functional group Chemical group 0.000 claims abstract description 4
- 230000005012 migration Effects 0.000 claims description 12
- 238000013508 migration Methods 0.000 claims description 12
- 230000003287 optical effect Effects 0.000 abstract description 5
- 239000004973 liquid crystal related substance Substances 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 36
- 239000010410 layer Substances 0.000 description 30
- -1 polyethylene terephthalate Polymers 0.000 description 23
- 239000002245 particle Substances 0.000 description 20
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 18
- 239000003795 chemical substances by application Substances 0.000 description 16
- 238000000576 coating method Methods 0.000 description 16
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 15
- 239000011248 coating agent Substances 0.000 description 14
- 229920002545 silicone oil Polymers 0.000 description 13
- 238000001035 drying Methods 0.000 description 9
- 238000011156 evaluation Methods 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 229920000728 polyester Polymers 0.000 description 9
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000011247 coating layer Substances 0.000 description 5
- 239000004721 Polyphenylene oxide Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 239000012046 mixed solvent Substances 0.000 description 4
- 229920000570 polyether Polymers 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229920002799 BoPET Polymers 0.000 description 3
- 239000003522 acrylic cement Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 150000002009 diols Chemical class 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229920001187 thermosetting polymer Polymers 0.000 description 3
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 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
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 239000012790 adhesive layer Substances 0.000 description 2
- 239000002390 adhesive tape Substances 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 125000003710 aryl alkyl group Chemical group 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
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 2
- 238000001723 curing Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 125000005388 dimethylhydrogensiloxy group Chemical group 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 238000007756 gravure coating Methods 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- 239000011146 organic particle Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920001843 polymethylhydrosiloxane Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- PXGZQGDTEZPERC-UHFFFAOYSA-N 1,4-cyclohexanedicarboxylic acid Chemical compound OC(=O)C1CCC(C(O)=O)CC1 PXGZQGDTEZPERC-UHFFFAOYSA-N 0.000 description 1
- CEBKHWWANWSNTI-UHFFFAOYSA-N 2-methylbut-3-yn-2-ol Chemical compound CC(C)(O)C#C CEBKHWWANWSNTI-UHFFFAOYSA-N 0.000 description 1
- NECRQCBKTGZNMH-UHFFFAOYSA-N 3,5-dimethylhex-1-yn-3-ol Chemical compound CC(C)CC(C)(O)C#C NECRQCBKTGZNMH-UHFFFAOYSA-N 0.000 description 1
- 229940090248 4-hydroxybenzoic acid Drugs 0.000 description 1
- KAUQJMHLAFIZDU-UHFFFAOYSA-N 6-Hydroxy-2-naphthoic acid Chemical compound C1=C(O)C=CC2=CC(C(=O)O)=CC=C21 KAUQJMHLAFIZDU-UHFFFAOYSA-N 0.000 description 1
- GZVHEAJQGPRDLQ-UHFFFAOYSA-N 6-phenyl-1,3,5-triazine-2,4-diamine Chemical compound NC1=NC(N)=NC(C=2C=CC=CC=2)=N1 GZVHEAJQGPRDLQ-UHFFFAOYSA-N 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229920001807 Urea-formaldehyde Polymers 0.000 description 1
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 238000006757 chemical reactions by type Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 150000001991 dicarboxylic acids Chemical class 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229920005645 diorganopolysiloxane polymer Polymers 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 230000032050 esterification Effects 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 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
- 238000000691 measurement method Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- RXOHFPCZGPKIRD-UHFFFAOYSA-N naphthalene-2,6-dicarboxylic acid Chemical compound C1=C(C(O)=O)C=CC2=CC(C(=O)O)=CC=C21 RXOHFPCZGPKIRD-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 150000002894 organic compounds Chemical group 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 150000003058 platinum compounds Chemical class 0.000 description 1
- 229920003216 poly(methylphenylsiloxane) Polymers 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002683 reaction inhibitor Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007763 reverse roll coating Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000003017 thermal stabilizer Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Laminated Bodies (AREA)
- Adhesive Tapes (AREA)
- Coating Of Shaped Articles Made Of Macromolecular Substances (AREA)
Abstract
Description
本発明は、光学用途向けとして好適な基材レス両面粘着シート用ポリエステルフィルムに関するものである。 The present invention relates to a polyester film for a base-less double-sided pressure-sensitive adhesive sheet suitable for optical applications.
従来、物体間を面接着する粘着シートは種々知られており、粘着シートの1つとして基材レス両面粘着シートが知られている。基材レス両面粘着シートは、粘着剤層の両面に剥離力の相対的に低い軽剥離シートと、剥離力の相対的に高い重剥離シートが積層されて構成され、両面の剥離シートを除去した後には、支持基材を有さない粘着剤層のみとなる両面粘着シートである。基材レス両面粘着シートは、まず軽剥離シートが剥がされ、露出された粘着剤層の一方の面が物体面に接着され、その接着後、さらに重剥離シートが剥がされ、露出された粘着剤層の他方の面が、異なる物体面に接着され、これにより物体間が面接着される。 Conventionally, various pressure-sensitive adhesive sheets for surface bonding between objects are known, and a base-less double-sided pressure-sensitive adhesive sheet is known as one of pressure-sensitive adhesive sheets. The substrate-less double-sided pressure-sensitive adhesive sheet is configured by laminating a light release sheet having a relatively low peeling force and a heavy release sheet having a relatively high peeling force on both sides of the pressure-sensitive adhesive layer, and removing the double-sided release sheet. The latter is a double-sided pressure-sensitive adhesive sheet that only has a pressure-sensitive adhesive layer that does not have a supporting substrate. The substrate-less double-sided PSA sheet is first peeled off from the light release sheet, and one side of the exposed PSA layer is bonded to the object surface. The other side of the layer is bonded to a different object surface, thereby surface bonding between the objects.
近年、基材レス両面粘着シートは、その用途が広がりつつあり、各種光学用途の部材等にも用いられている。例えば、LCDの部材として、基材レス両面粘着剤シートの剥離力の軽い方の離型フィルムを剥がして、その面に偏光板を貼り合わせて、その反対面側に剥離力の重い離型フィルムを用いることがある。 In recent years, the use of a baseless double-sided pressure-sensitive adhesive sheet has been spreading, and is also used for members for various optical applications. For example, as the LCD member, peel off the release film with the lighter peeling force of the base-less double-sided pressure-sensitive adhesive sheet, paste the polarizing plate on the surface, and release the heavy release force on the opposite side. May be used.
生産上の作業性から、ある程度高速域での加工が考えられるが、軽剥離の離型フィルムにおいて、軽い剥離力を達成するのはもちろんだが、それを達成しつつ、加工速度を上げても、できるだけ重剥離の離型フィルムとの剥離力差が縮まらないことを同時に達成することは非常に難しい。もし、重剥離の離型フィルムとの剥離力差が縮まったならば、剥離工程において、両面のフィルムが同時に剥がれる、また、剥離力差が小さくなるために粘着剤も一緒に剥がれる等の問題が起こり、加工性、生産性に不具合をきたすことになる。 In terms of workability in production, processing in a high speed range can be considered to some extent, but in the release film of light release, of course, to achieve a light release force, It is very difficult to simultaneously achieve that the difference in peel force from the release film that is as heavy as possible is not reduced. If the peel force difference with the heavy release film is reduced, there will be problems such as the film on both sides being peeled off at the same time in the peeling process, and the adhesive being peeled off together because the peel force difference is small. This will cause problems in workability and productivity.
本発明は、上記実情に鑑みなされたものであって、その解決課題は、基材レス両面粘着シートを光学用途、例えば、タッチパネル、液晶偏向板、位相差板等において使用する際、剥離速度依存性を最小限に抑えることを可能にし、生産性、コストなどの問題を解決した、安価な基材レス両面粘着シート用ポリエステルフィルムを提供することにある。 The present invention has been made in view of the above circumstances, and the problem to be solved is that the substrate-less double-sided pressure-sensitive adhesive sheet depends on the peeling rate when used in optical applications, for example, touch panels, liquid crystal deflecting plates, retardation plates, and the like. It is an object of the present invention to provide an inexpensive polyester film for a double-sided pressure-sensitive adhesive sheet that can minimize productivity and solve problems such as productivity and cost.
本発明者は、上記実情に鑑み鋭意検討した結果、特定の構成を有するポリエステルフィルムによれば、上記課題を容易に解決できることを見いだし、本発明を完成するに至った。 As a result of intensive studies in view of the above circumstances, the present inventor has found that the above problem can be easily solved by a polyester film having a specific configuration, and has completed the present invention.
すなわち、本発明の要旨は、アルケニル基およびアルキル基を官能基として有し、移行成分を5〜20重量%含むシリコーン樹脂と、白金系触媒とを含有するシリコーン系離型層を有するポリエステルフィルムであり、当該離型層の300mm/分速度域での低速剥離力が10〜20mN/cmの範囲であり、かつ、10000mm/分速度域での高速剥離力が前記低速剥離力の2.5倍以下であることを特徴とする基材レス両面粘着シート用ポリエステルフィルムに存する。 That is, the gist of the present invention is a polyester film having a silicone release layer containing a silicone resin having an alkenyl group and an alkyl group as functional groups and containing 5 to 20% by weight of a migration component and a platinum catalyst. Yes, the release layer has a low-speed peel force in the range of 300 mm / min and a speed of 10-20 mN / cm, and a high-speed peel force in the range of 10,000 mm / min is 2.5 times the low-speed peel force. It exists in the polyester film for base-material-less double-sided adhesive sheets characterized by the following.
本発明によれば、軽剥離で剥離速度依存性が小さい離型ポリエステルフィルムを提供することができるため、その工業的価値は高い。 According to the present invention, it is possible to provide a release polyester film that is lightly peeled and has a small peel rate dependency, and therefore its industrial value is high.
本発明でいうポリエステルフィルムとは、いわゆる押出法に従い押出口金から溶融押出されたシートを延伸したフィルムである。 The polyester film referred to in the present invention is a film obtained by stretching a sheet melt-extruded from an extrusion die according to a so-called extrusion method.
上記のフィルムを構成するポリエステルとは、ジカルボン酸と、ジオールとからあるいはヒドロキシカルボン酸から重縮合によって得られるエステル基を含むポリマーを指す。
ジカルボン酸としては、テレフタル酸、イソフタル酸、アジピン酸、アゼライン酸、セバシン酸、2,6−ナフタレンジカルボン酸、1,4−シクロヘキサンジカルボン酸等を、ジオールとしては、エチレングリコール、1,4−ブタンジオール、ジエチレングリコール、トリエチレングリコール、ネオペンチルグリコール、1,4−シクロヘキサンジメタノール、ポリエチレングリコール等を、ヒドロキシカルボン酸としては、p−ヒドロキシ安息香酸、6−ヒドロキシ−2−ナフトエ酸等をそれぞれ例示することができる。かかるポリマーの代表的なものとして、ポリエチレンテレフタレートやポリエチレン−2、6−ナフタレート等が例示される。
The polyester constituting the film refers to a polymer containing an ester group obtained by polycondensation from dicarboxylic acid and diol or from hydroxycarboxylic acid.
Examples of dicarboxylic acids include terephthalic acid, isophthalic acid, adipic acid, azelaic acid, sebacic acid, 2,6-naphthalenedicarboxylic acid, 1,4-cyclohexanedicarboxylic acid, and diols include ethylene glycol and 1,4-butane. Examples include diol, diethylene glycol, triethylene glycol, neopentyl glycol, 1,4-cyclohexanedimethanol, polyethylene glycol and the like, and examples of hydroxycarboxylic acid include p-hydroxybenzoic acid and 6-hydroxy-2-naphthoic acid. be able to. Typical examples of such a polymer include polyethylene terephthalate and polyethylene-2,6-naphthalate.
本発明のフィルム中には、易滑性の付与および各工程での傷発生防止を主たる目的として、粒子を配合することが好ましい。配合する粒子の種類は、易滑性付与可能な粒子であれば特に限定されるものではなく、具体例としては、例えば、シリカ、炭酸カルシウム、炭酸マグネシウム、炭酸バリウム、硫酸カルシウム、リン酸カルシウム、リン酸マグネシウム、カオリン、酸化アルミニウム、酸化チタン等の粒子が挙げられる。また、特公昭59−5216号公報、特開昭59−217755号公報等に記載されているような耐熱性有機粒子を用いてもよい。この他の耐熱性有機粒子の例として、熱硬化性尿素樹脂、熱硬化性フェノール樹脂、熱硬化性エポキシ樹脂、ベンゾグアナミン樹脂等が挙げられる。さらに、ポリエステル製造工程中、触媒等の金属化合物の一部を沈殿、微分散させた析出粒子を用いることもできる。 In the film of the present invention, it is preferable to blend particles mainly for the purpose of imparting slipperiness and preventing the occurrence of scratches in each step. The kind of the particle to be blended is not particularly limited as long as it is a particle capable of imparting slipperiness. Specific examples thereof include silica, calcium carbonate, magnesium carbonate, barium carbonate, calcium sulfate, calcium phosphate, and phosphoric acid. Examples of the particles include magnesium, kaolin, aluminum oxide, and titanium oxide. Further, heat-resistant organic particles as described in JP-B-59-5216, JP-A-59-217755 and the like may be used. Examples of other heat-resistant organic particles include thermosetting urea resins, thermosetting phenol resins, thermosetting epoxy resins, benzoguanamine resins, and the like. Furthermore, precipitated particles obtained by precipitating and finely dispersing a part of a metal compound such as a catalyst during the polyester production process can also be used.
一方、使用する粒子の形状に関しても特に限定されるわけではなく、球状、塊状、棒状、扁平状等のいずれを用いてもよい。また、その硬度、比重、色等についても特に制限はない。これら一連の粒子は、必要に応じて2種類以上を併用してもよい。 On the other hand, the shape of the particles to be used is not particularly limited, and any of a spherical shape, a block shape, a rod shape, a flat shape, and the like may be used. Moreover, there is no restriction | limiting in particular also about the hardness, specific gravity, a color. These series of particles may be used in combination of two or more as required.
また、用いる粒子の平均粒径は、通常0.01〜3μm、好ましくは0.1〜2μmの範囲である。平均粒径が0.01μm未満の場合には、易滑性を十分に付与できない場合がある。一方、3μmを超える場合には、フィルムの製膜時に、その粒子の凝集物のために透明性が低下することがある他に、破断などを起こし易くなり、生産性の面で問題になることがある。 Moreover, the average particle diameter of the particle | grains to be used is 0.01-3 micrometers normally, Preferably it is the range of 0.1-2 micrometers. When the average particle size is less than 0.01 μm, the slipperiness may not be sufficiently imparted. On the other hand, when the thickness exceeds 3 μm, transparency may be lowered due to the aggregate of the particles when the film is formed, and it is easy to cause breakage, which causes a problem in terms of productivity. There is.
さらにポリエステル中の粒子含有量は、通常0.001〜5重量%、好ましくは0.005〜3重量%の範囲である。粒子含有量が0.001重量%未満の場合には、フィルムの易滑性が不十分な場合があり、一方、5重量%を超えて添加する場合には、フィルムの透明性が不十分な場合がある。 Furthermore, the content of particles in the polyester is usually in the range of 0.001 to 5% by weight, preferably 0.005 to 3% by weight. When the particle content is less than 0.001% by weight, the slipperiness of the film may be insufficient. On the other hand, when the content exceeds 5% by weight, the transparency of the film is insufficient. There is a case.
ポリエステル層中に粒子を添加する方法としては、特に限定されるものではなく、従来公知の方法を採用しうる。例えば、各層を構成するポリエステルを製造する任意の段階において添加することができるが、好ましくはエステル化もしくはエステル交換反応終了後、添加するのが良い。 The method for adding particles to the polyester layer is not particularly limited, and a conventionally known method can be adopted. For example, it can be added at any stage for producing the polyester constituting each layer, but it is preferably added after completion of esterification or transesterification.
また、ベント付き混練押出機を用い、エチレングリコールまたは水などに分散させた粒子のスラリーとポリエステル原料とをブレンドする方法、または、混練押出機を用い、乾燥させた粒子とポリエステル原料とをブレンドする方法などによって行われる。 Also, a method of blending a slurry of particles dispersed in ethylene glycol or water with a vented kneading extruder and a polyester raw material, or a blending of dried particles and a polyester raw material using a kneading extruder. It is done by methods.
なお、本発明におけるポリエステルフィルム中には、上述の粒子以外に必要に応じて従来公知の酸化防止剤、帯電防止剤、熱安定剤、潤滑剤、染料、顔料等を添加することができる。 In addition to the above-mentioned particles, conventionally known antioxidants, antistatic agents, thermal stabilizers, lubricants, dyes, pigments, and the like can be added to the polyester film in the present invention as necessary.
本発明におけるポリエステルフィルムの厚みは、フィルムとして製膜可能な範囲であれば特に限定されるものではないが、通常10〜350μm、好ましくは15〜100μmの範囲である。 Although the thickness of the polyester film in this invention will not be specifically limited if it is a range which can be formed into a film as a film, Usually, 10-350 micrometers, Preferably it is the range of 15-100 micrometers.
次に本発明におけるポリエステルフィルムの製造例について具体的に説明するが、以下の製造例に何ら限定されるものではない。すなわち、先に述べたポリエステル原料を使用し、ダイから押し出された溶融シートを冷却ロールで冷却固化して未延伸シートを得る方法が好ましい。この場合、シートの平面性を向上させるためシートと回転冷却ドラムとの密着性を高めることが好ましく、静電印加密着法および/または液体塗布密着法が好ましく採用される。次に得られた未延伸シートは二軸方向に延伸される。その場合、まず、前記の未延伸シートを一方向にロールまたはテンター方式の延伸機により延伸する。延伸温度は、通常90〜140℃、好ましくは95〜120℃であり、延伸倍率は通常2.5〜7倍、好ましくは3.0〜6倍である。次いで、一段目の延伸方向と直交する方向に延伸するが、その場合、延伸温度は通常90〜170℃であり、延伸倍率は通常3.0〜7倍、好ましくは3.5〜6倍である。そして、引き続き180〜270℃の温度で緊張下または30%以内の弛緩下で熱処理を行い、二軸配向フィルムを得る。上記の延伸においては、一方向の延伸を2段階以上で行う方法を採用することもできる。その場合、最終的に二方向の延伸倍率がそれぞれ上記範囲となるように行うのが好ましい。 Next, although the manufacture example of the polyester film in this invention is demonstrated concretely, it is not limited to the following manufacture examples at all. That is, a method of using the polyester raw material described above and cooling and solidifying a molten sheet extruded from a die with a cooling roll to obtain an unstretched sheet is preferable. In this case, in order to improve the flatness of the sheet, it is preferable to improve the adhesion between the sheet and the rotary cooling drum, and an electrostatic application adhesion method and / or a liquid application adhesion method is preferably employed. Next, the obtained unstretched sheet is stretched in the biaxial direction. In that case, first, the unstretched sheet is stretched in one direction by a roll or a tenter type stretching machine. The stretching temperature is usually 90 to 140 ° C., preferably 95 to 120 ° C., and the stretching ratio is usually 2.5 to 7 times, preferably 3.0 to 6 times. Next, the film is stretched in the direction perpendicular to the first stretching direction. In that case, the stretching temperature is usually 90 to 170 ° C., and the stretching ratio is usually 3.0 to 7 times, preferably 3.5 to 6 times. is there. Subsequently, heat treatment is performed at a temperature of 180 to 270 ° C. under tension or under relaxation within 30% to obtain a biaxially oriented film. In the above-described stretching, a method in which stretching in one direction is performed in two or more stages can be employed. In that case, it is preferable to carry out so that the draw ratios in the two directions finally fall within the above ranges.
また、本発明のポリエステルフィルム製造に関しては、同時二軸延伸法を採用することもできる。同時二軸延伸法は、前記の未延伸シートを通常90〜140℃、好ましくは80〜110℃で温度コントロールされた状態で機械方向および幅方向に同時に延伸し配向させる方法であり、延伸倍率としては、面積倍率で4〜50倍、好ましくは7〜35倍、さらに好ましくは10〜25倍である。そして、引き続き、170〜250℃の温度で緊張下または30%以内の弛緩下で熱処理を行い、延伸配向フィルムを得る。上述の延伸方式を採用する同時二軸延伸装置に関しては、スクリュー方式、パンタグラフ方式、リニアー駆動方式等、従来公知の延伸方式を採用することができる。 For the production of the polyester film of the present invention, a simultaneous biaxial stretching method can also be employed. The simultaneous biaxial stretching method is a method in which the unstretched sheet is usually stretched and oriented in the machine direction and the width direction at 90 to 140 ° C., preferably 80 to 110 ° C., and the stretching ratio is as follows. Is 4 to 50 times, preferably 7 to 35 times, and more preferably 10 to 25 times in terms of area magnification. Subsequently, heat treatment is performed at a temperature of 170 to 250 ° C. under tension or under relaxation within 30% to obtain a stretched oriented film. With respect to the simultaneous biaxial stretching apparatus that employs the above-described stretching method, a conventionally known stretching method such as a screw method, a pantograph method, or a linear driving method can be employed.
ポリエステルフィルムの表面に塗布層を形成する方法は、特に制限されないが、ポリエステルフィルムを製造する工程中で塗布液を塗布する方法が好適に採用される。具体的には、未延伸シート表面に塗布液を塗布して乾燥する方法、一軸延伸フィルム表面に塗布液を塗布して乾燥する方法、二軸延伸フィルム表面に塗布液を塗布して乾燥する方法等が挙げられる。これらの中では、未延伸フィルムまたは一軸延伸フィルム表面に塗布液を塗布後、フィルムに熱処理を行う過程で同時に塗布層を乾燥硬化する方法が経済的である。また、塗布層を形成する方法として、必要に応じ、前述の塗布方法の幾つかを併用した方法も採用し得る。具体的には、未延伸シート表面に第一層を塗布して乾燥し、その後、一軸方向に延伸後、第二層を塗布して乾燥する方法等が挙げられる。ポリエステルフィルムの表面に塗布液を塗布する方法としては、原崎勇次著、槙書店、1979年発行、「コーティング方式」に示されるリバースロールコーター、グラビアコーター、ロッドコーター、エアドクターコーター等を使用することができる。 Although the method in particular of forming a coating layer on the surface of a polyester film is not restrict | limited, The method of apply | coating a coating liquid in the process of manufacturing a polyester film is employ | adopted suitably. Specifically, a method of applying and drying a coating solution on the surface of an unstretched sheet, a method of applying and drying a coating solution on the surface of a uniaxially stretched film, and a method of applying and drying a coating solution on the surface of a biaxially stretched film Etc. Among these, it is economical to apply a coating solution to the surface of an unstretched film or a uniaxially stretched film, and then simultaneously dry and cure the coating layer in the process of heat treatment on the film. Moreover, as a method for forming the coating layer, a method in which some of the above-described coating methods are used in combination can be adopted as necessary. Specifically, a method of applying a first layer on the surface of an unstretched sheet and drying, then stretching in a uniaxial direction, and then applying and drying a second layer can be used. Use the reverse roll coater, gravure coater, rod coater, air doctor coater, etc. shown in “Coating Method” by Yuji Harasaki, Tsuji Shoten, published in 1979, as a method of applying the coating solution to the surface of the polyester film. Can do.
本発明において得られたポリエステルフィルムの片方の最外層に形成する離型層硬化型シリコーン樹脂の種類としては、付加型・縮合型・紫外線硬化型・電子線硬化型・無溶剤型等何れの硬化反応タイプでも用いることができる。 The type of release layer curable silicone resin to be formed on the outermost layer of one of the polyester films obtained in the present invention is any of addition type, condensation type, ultraviolet curable type, electron beam curable type, solventless type, etc. The reaction type can also be used.
本発明において使用する、アルケニル基およびアルキル基を官能基として有するシリコーン樹脂の例としては以下のようなものが挙げられる。まず、アルケニル基を含む硬化型シリコーン樹脂は、ジオルガノポリシロキサンとして、分子鎖両末端トリメチルシロキシ基封鎖ジメチルシロキサン・メチルヘキセニルシロキサン共重合体(ジメチルシロキサン単位96モル%、メチルヘキセニルシロキサン単位4モル%、分子鎖両末端ジメチルビニルシロキシ基封鎖ジメチルシロキサン・メチルヘキセニルシロキサン共重合体(ジメチルシロキサン単位97モル%、メチルヘキセニルシロキサン単位3モル%)、分子鎖両末端ジメチルヘキセニルシロキシ基封鎖ジメチルシロキサン・メチルヘキセニルシロキサン共重合体(ジメチルシロキサン単位95モル%、メチルヘキセニルシロキサン単位5モル%)が挙げられる。次に、アルキル基を含む硬化型シリコーン樹脂は、オルガノハイドロジェンポリシロキサンとして、分子鎖両末端トリメチルシロキシ基封鎖メチルハイドロジェンポリシロキサン、分子鎖両末端トリメチルシロキシ基封鎖ジメチルシロキサン・メチルハイドロジェンシロキサン共重合体、分子鎖両末端ジメチルハイドロジェンシロキシ基封鎖メチルハイドロジェンポリシロキサン、分子鎖両末端ジメチルハイドロジェンシロキシ基封鎖ジメチルシロキサン・メチルハイドロジェンシロキサン共重合体が挙げられる。 Examples of the silicone resin having an alkenyl group and an alkyl group as functional groups used in the present invention include the following. First, a curable silicone resin containing an alkenyl group is a diorganopolysiloxane having a trimethylsiloxy group-blocked dimethylsiloxane / methylhexenylsiloxane copolymer (96 mol% dimethylsiloxane unit, 4 mol% methylhexenylsiloxane unit). , Dimethylvinylsiloxy group-blocked dimethylsiloxane / methylhexenylsiloxane copolymer (97 mol% dimethylsiloxane unit, 3 mol% methylhexenylsiloxane unit), dimethylsiloxane / methylhexenyl blocked with dimethylhexenylsiloxy group blocked at both ends of the molecular chain Siloxane copolymers (95 mol% of dimethylsiloxane units and 5 mol% of methylhexenylsiloxane units) can be mentioned. Genpolysiloxanes include trimethylsiloxy group-capped methylhydrogen polysiloxane with both molecular chains, trimethylsiloxy group-capped dimethylsiloxane / methylhydrogensiloxane copolymer with both molecular chains, and dimethylhydrogensiloxy group-capped methylhydro with molecular chains. Genpolysiloxane, dimethylhydrogensiloxy group-blocked dimethylsiloxane / methylhydrogensiloxane copolymer having both molecular chain ends.
本発明において移行性を達成するためにシリコーンオイルを添加してもよい。シリコーンオイルはストレートシリコーンオイル、変性シリコーンオイルと称されるシリコーンオイルで、以下のようなものが挙げられる。ストレートシリコーンとしては、ジメチルシリコーンオイル、メチルフェニルシリコーンオイル、メチルハイドロジェンシリコーンオイル等が挙げられる。また、変性シリコーンオイルとしては、側鎖型タイプのポリエーテル変性、アラルキル変性、フロロアルキル変性、長鎖アルキル変性、高級脂肪酸エステル変性、高級脂肪酸アミド変性、ポリエーテル・長鎖アルキル変性・アラルキル変性、フェニル変性、両末端型のポリエーテル変性、ポリエーテル・メトキシ変性などが挙げられる。
これらシリコーンオイルは、移行成分としてシリコーン樹脂中に0.1〜5.0重量%含有されることが好ましい。ストレートシリコーンオイル、変性シリコーンオイル共に、非反応性の無官能オイルである。
In the present invention, silicone oil may be added in order to achieve migration. The silicone oil is a silicone oil called a straight silicone oil or a modified silicone oil, and examples thereof include the following. Examples of the straight silicone include dimethyl silicone oil, methylphenyl silicone oil, methyl hydrogen silicone oil, and the like. Further, as modified silicone oil, side chain type polyether modified, aralkyl modified, fluoroalkyl modified, long chain alkyl modified, higher fatty acid ester modified, higher fatty acid amide modified, polyether / long chain alkyl modified / aralkyl modified, Examples include phenyl modification, polyether modification at both ends, and polyether / methoxy modification.
These silicone oils are preferably contained in the silicone resin in an amount of 0.1 to 5.0% by weight as a migration component. Both straight silicone oil and modified silicone oil are non-reactive, non-functional oils.
本発明において使用するシリコーン樹脂に含まれる移行成分は、5〜20重量%の範囲であり、好ましくは10〜13重量%である。移行成分の含有量が5%より低いと速度依存性が高くなり、20重量%を超えると、硬化性が著しく低下し、密着性も悪化する不具合がある。 The migration component contained in the silicone resin used in the present invention is in the range of 5 to 20% by weight, preferably 10 to 13% by weight. If the content of the transition component is lower than 5%, the speed dependency becomes high, and if it exceeds 20% by weight, the curability is remarkably lowered and the adhesion is also deteriorated.
本発明において日東電工株式会社製No.31Bテープによる残留接着率が65%〜90%が好ましく、より好ましくは、70%〜85%である。残留接着率が65%より低いと、移行性が高く、粘着剤加工時にロール汚れや粘着剤面に移行して、粘着剥離力低下などが生じてしまう。また、残留接着率が90%以上となると、速度依存性を小さく抑えることができない。 In the present invention, Nitto Denko Corporation No. The residual adhesion rate with 31B tape is preferably 65% to 90%, more preferably 70% to 85%. When the residual adhesion rate is lower than 65%, the transferability is high, and the adhesive moves to roll dirt or the adhesive surface during the adhesive processing, resulting in a decrease in adhesive peeling force. Further, when the residual adhesion rate is 90% or more, the speed dependency cannot be reduced.
シリコーン系樹脂塗剤の具体例を挙げると、信越化学工業(株)製KS−774、KS−775、KS−778、KS−779H、KS−847H、KS−856、X−62−2422、X−62−2461、ダウ・コーニング・アジア(株)製DKQ3−202、DKQ3−203、DKQ3−204、DKQ3−205、DKQ3−210、東芝シリコーン(株)製YSR−3022、TPR−6700、TPR−6720、TPR−6721、東レ・ダウ・コーニング(株)製LTC300B、LTC303E、LTC310、LTC314、SRX357、BY24−749、SD7333、BY24−179、SP7015、SP7259、SD7220、SD7226、SD7229等が挙げられる。さらに離型層の剥離性等を調整するために剥離コントロール剤を併用してもよい。また、上述のとおり、離型層中にアミノ基を有するシラン化合物を添加することもある。 Specific examples of the silicone resin coating agent include KS-774, KS-775, KS-778, KS-779H, KS-847H, KS-856, X-62-2422, X manufactured by Shin-Etsu Chemical Co., Ltd. -62-2461, DKQ3-202, DKQ3-203, DKQ3-204, DKQ3-205, DKQ3-210, manufactured by Dow Corning Asia Co., Ltd. YSR-3022, TPR-6700, TPR-, manufactured by Toshiba Silicone Co., Ltd. 6720, TPR-6721, Toray Dow Corning Co., Ltd. LTC300B, LTC303E, LTC310, LTC314, SRX357, BY24-749, SD7333, BY24-179, SP7015, SP7259, SD7220, SD7226, SD7229, and the like. Further, a release control agent may be used in combination to adjust the release property of the release layer. Further, as described above, a silane compound having an amino group may be added to the release layer.
本発明において、ポリエステルフィルムに離型層を設ける方法としては、リバースロールコート、グラビアコート、バーコート、ドクターブレードコート等、従来公知の塗工方式を用いることができる。本発明における離型層の塗布量は、通常0.01〜1g/m2の範囲である。 In the present invention, as a method for providing a release layer on the polyester film, a conventionally known coating method such as reverse roll coating, gravure coating, bar coating, doctor blade coating, or the like can be used. The application amount of the release layer in the present invention is usually in the range of 0.01 to 1 g / m 2 .
本発明において、離型層が設けられていない面には、接着層、帯電防止層、オリゴマー析出防止層等の塗布層を設けてもよく、また、ポリエステルフィルムにはコロナ処理、プラズマ処理等の表面処理を施してもよい。 In the present invention, a coating layer such as an adhesive layer, an antistatic layer and an oligomer precipitation preventing layer may be provided on the surface where the release layer is not provided, and the polyester film may be subjected to corona treatment, plasma treatment, etc. A surface treatment may be applied.
本発明におけるポリエステルフィルムでは、離型層をきれいかつ頑丈にするため、付加型の反応を促進する白金系触媒を用いる。本成分としては、塩化白金酸、塩化白金酸のアルコール溶液、塩化白金酸とオレフィンとの錯体、塩化白金酸とアルケニルシロキサンとの錯体等の白金系化合物、白金黒、白金担持シリカ、白金担持活性炭が例示される。離型層中の白金系触媒含有量は、通常0.3〜3.0重量%、好ましくは0.5〜2.0重量%の範囲が良い。離型層中の白金系触媒含有量が0.3重量%よりも低い場合、剥離力の不具合や、塗布層での硬化反応が不十分になるため、面状悪化などの不具合を生じる場合があり、一方、離型層中の白金系触媒含有量が3.0重量%を超える場合には、コストがかかる、また、反応性が高まり、ゲル異物が発生する等の工程不具合を生じてしまうことがある。 In the polyester film in the present invention, a platinum-based catalyst that promotes an addition-type reaction is used to make the release layer clean and strong. As this component, chloroplatinic acid, alcohol solution of chloroplatinic acid, a complex of chloroplatinic acid and olefin, a platinum compound such as a complex of chloroplatinic acid and alkenylsiloxane, platinum black, platinum-supported silica, platinum-supported activated carbon Is exemplified. The platinum-based catalyst content in the release layer is usually 0.3 to 3.0% by weight, preferably 0.5 to 2.0% by weight. When the platinum-based catalyst content in the release layer is lower than 0.3% by weight, there may be problems such as deterioration of the surface condition due to insufficient peeling force and insufficient curing reaction in the coating layer. On the other hand, when the platinum-based catalyst content in the release layer exceeds 3.0% by weight, the cost is increased, and the process becomes defective due to increased reactivity and generation of gel foreign matter. Sometimes.
また、付加型の反応は非常に反応性が高いため、場合によっては、反応抑制剤として、アセチレンアルコールを添加することがある。その成分は炭素−炭素3重結合と水酸基を有する有機化合物であるが、好ましくは、3−メチル−1−ブチン−3−オール、3,5−ジメチル−1−ヘキシン−3−オールおよびフェニルブチノールからなる群から選択される化合物である。 In addition, since the addition type reaction is very reactive, acetylene alcohol may be added as a reaction inhibitor in some cases. The component is an organic compound having a carbon-carbon triple bond and a hydroxyl group, and preferably 3-methyl-1-butyn-3-ol, 3,5-dimethyl-1-hexyn-3-ol and phenylbuty It is a compound selected from the group consisting of nor.
本発明における、剥離力とは、両面粘着テープ(日東電工製「No.31B」)を離型層面に貼り付け、室温にて1時間放置した後に、基材フィルムと剥離角度180°、任意の引張速度でテープを剥離したときに引張試験機で測定した値を言う。本発明において特定の剥離力を調整する方法は、離型層中の組成を選択することにより達成することができるが、その他の手段も採用でき、主にシリコーン離型層の離型剤の種類を、所望の剥離力に応じて変更することが好ましく、さらには、剥離力は用いる離型剤の塗布量に大きく依存するため、その離型剤の塗布量を調整する方法がさらに好ましい。 In the present invention, the peeling force refers to a double-sided pressure-sensitive adhesive tape (“No. 31B” manufactured by Nitto Denko) attached to the release layer surface and left at room temperature for 1 hour, and then the substrate film and the peeling angle of 180 °. The value measured with a tensile tester when the tape is peeled off at the tensile speed. The method for adjusting the specific peeling force in the present invention can be achieved by selecting the composition in the release layer, but other means can also be adopted, mainly the type of release agent for the silicone release layer. Is preferably changed according to the desired peeling force, and furthermore, since the peeling force largely depends on the application amount of the release agent to be used, a method of adjusting the application amount of the release agent is more preferable.
本発明におけるポリエステルフィルムの剥離力の値については、300mm/分速度域での低速剥離力が10〜20mN/cmの範囲である。当該剥離力が10mN/cm未満の場合、剥離力が軽くなりすぎて本来剥離する必要がない場面においても容易に剥離する不具合を生じる。剥離力が20mN/cmを超える場合、剥離力の重い方の離型フィルムとの剥離力差が小さくなり、剥離工程で不具合を生じたり、剥離力の重い方の離型フィルムの選定幅が狭くなったりする等の問題がある。 About the value of the peeling force of the polyester film in this invention, the low speed peeling force in a 300 mm / min speed area is the range of 10-20 mN / cm. When the peeling force is less than 10 mN / cm, the peeling force becomes too light, and the problem of peeling easily occurs even in a scene where it is not necessary to peel off. If the peel force exceeds 20 mN / cm, the difference in peel force between the release film with the greater peel force will be small, causing problems in the peel process, and the selection range for the release film with the greater peel force will be narrow. There are problems such as becoming.
さらに、加工性を考慮に入れた10000mm/分速度域での高速剥離力が、上記低速剥離力の2.5倍以下である。当該剥離力の比が2.5倍よりも大きい場合、剥離力が重い方の離型フィルムとの剥離力差が小さくなり、剥離工程で剥離が上手くできなかったり、粘着剤ごと剥がれてしまったりする。 Furthermore, the high speed peeling force in the 10,000 mm / min speed range in consideration of workability is 2.5 times or less of the above low speed peeling force. If the peel force ratio is larger than 2.5 times, the peel force difference between the release film and the heavier peel force will be small, and the peel process will not be successful, or the adhesive may be peeled off. To do.
以下、本発明を実施例によりさらに詳細に説明するが、本発明はその要旨を越えない限り、以下の実施例に限定されるものではない。また、本発明で用いた測定法および評価方法は次のとおりである。 EXAMPLES Hereinafter, although an Example demonstrates this invention further in detail, this invention is not limited to a following example, unless the summary is exceeded. The measurement method and evaluation method used in the present invention are as follows.
(1)平均粒径(d50:μm)の測定
遠心沈降式粒度分布測定装置(株式会社島津製作所社製SA−CP3型)を使用して測定した等価球形分布における積算(重量基準)50%の値を平均粒径とした。
(1) Measurement of average particle diameter (d50: μm) 50% integrated (weight basis) in equivalent spherical distribution measured using centrifugal sedimentation type particle size distribution measuring device (SA-CP3 type manufactured by Shimadzu Corporation) The value was defined as the average particle size.
(2)移行成分量測定
トルエンで固形分濃度4重量%に希釈したシリコーン樹脂15gに対して白金触媒0.02重量%0.004gを添加し、攪拌後、テフロン(登録商標)製のシートで作成した箱に入れ、150℃1時間熱硬化する(サンプル1)。移行成分を添加する場合(後述の比較例2に該当する)は、シリコーン樹脂の固形分に対して30重量%添加する。サンプル1を1日トルエンに浸漬し、取り出したサンプルを、120℃30分乾燥し、室温になるまで、放冷する(サンプル2)。下記式より以降成分量を算出した。
移行成分量(重量%)=(サンプル1の重量−サンプル2の重量)÷サンプル1の重量×100
(2) Measurement of amount of migrating component To 15 g of silicone resin diluted with toluene to a solid content concentration of 4% by weight, 0.02% by weight of platinum catalyst is added and 0.004 g is stirred, and then a Teflon (registered trademark) sheet is used. Place in the created box and heat cure at 150 ° C. for 1 hour (Sample 1). When adding a migration component (corresponding to Comparative Example 2 described later), 30% by weight is added to the solid content of the silicone resin. Sample 1 is immersed in toluene for 1 day, and the sample taken out is dried at 120 ° C. for 30 minutes and allowed to cool to room temperature (sample 2). The component amount was calculated from the following formula.
Migration component amount (% by weight) = (weight of sample 1−weight of sample 2) ÷ weight of sample 1 × 100
(3)離型フィルムの移行性評価接着率
試料フィルムをA4大に切り取り、離型面に75μm厚の2軸延伸PETフィルム(三菱化学ポリエステルフィルム株式会社製:ダイアホイルT100−75)を重ねて温度60℃、圧力1MPaの条件で2時間プレスする。この離型面に押し当てた75μm厚フィルムを移行性評価フィルムとする。未処理のPETフィルムにも同様にして75μm厚2軸延伸PETフィルム(同)を押し当て、基準フィルムとする。それぞれのフィルムの押し当てた面に粘着テープ(日東電工(株)製「No.31B」)を貼り付けた後、50mm×300mmのサイズにカットし、室温にて1時間放置後の剥離力を測定した。剥離力は(株)島津製作所製「Ezgraph」を使用し、引張速度0.3(m/min)の条件下、180°剥離を行った。
移行性評価接着率(%)=(移行性評価フィルムの剥離力÷基準フィルムの剥離力)×100
移行性の大きなフィルムでは押し当てたフィルムに多くのシリコーンが付着するため、粘着テープの剥離力が小さくなり、移行性評価接着率(%)も低下する。
(3) Transferability Evaluation Adhesion Rate of Release Film Sample film was cut to A4 size, and 75 μm thick biaxially stretched PET film (Mitsubishi Chemical Polyester Film Co., Ltd .: Diafoil T100-75) was layered on the release surface. Press for 2 hours under conditions of a temperature of 60 ° C. and a pressure of 1 MPa. A 75 μm-thick film pressed against this release surface is used as a migration evaluation film. Similarly, a 75 μm-thick biaxially stretched PET film (same as above) is pressed against an untreated PET film as a reference film. Adhesive tape (“No. 31B” manufactured by Nitto Denko Corporation) is applied to the pressed surface of each film, then cut to a size of 50 mm × 300 mm, and the peel strength after standing for 1 hour at room temperature. It was measured. The peeling force was “Ezgraph” manufactured by Shimadzu Corporation, and 180 ° peeling was performed under the condition of a tensile speed of 0.3 (m / min).
Transferability evaluation adhesion rate (%) = (Peeling force of transferability evaluation film ÷ Peeling force of reference film) × 100
In a film having a high migration property, a large amount of silicone adheres to the pressed film, so that the peeling force of the pressure-sensitive adhesive tape is reduced, and the migration evaluation adhesion rate (%) is also reduced.
(4)離型フィルムの剥離力(F)の評価
試料フィルムの離型層表面に両面粘着テープ(日東電工製「No.31B」)の片面を貼り付けた後、50mm×300mmのサイズにカットした後、室温にて1時間放置後の剥離力を測定する。剥離力は、引張試験機((株)インテスコ製「インテスコモデル2001型」)を使用し、引張速度300mm/分、さらに、10000mm/分の条件下、180°剥離を行った。次のような基準で判断する。
(4) Evaluation of peel force (F) of release film Affixed with one side of double-sided adhesive tape (Nitto Denko "No. 31B") on the release layer surface of the sample film, then cut to a size of 50mm x 300mm After that, the peel strength after standing for 1 hour at room temperature is measured. For the peeling force, a tensile tester (“Intesco model 2001 type” manufactured by Intesco Co., Ltd.) was used, and 180 ° peeling was performed under the conditions of a tensile speed of 300 mm / min and further 10,000 mm / min. Judgment is based on the following criteria.
<300mm/分での剥離力>
○:10〜20mN/cmの範囲
×:10mN/cmより小さい、もしくは、20mN/cmより大きい
<Peeling force at 300 mm / min>
○: Range of 10 to 20 mN / cm ×: Less than 10 mN / cm or greater than 20 mN / cm
<10000mm/分での剥離力と300mm/分での剥離力の比較>
下式にて求めた値で判断した。
(10000mm/分剥離力(mN/cm))÷(300mm/分剥離力(mN/cm))
○:2.5以下
×:2.5より大きい
<Comparison of peel force at 10,000 mm / min and peel force at 300 mm / min>
Judgment was made based on the value obtained by the following equation.
(10000 mm / min peeling force (mN / cm)) / (300 mm / min peeling force (mN / cm))
○: 2.5 or less ×: More than 2.5
(5)離型特性
粘着層を有する積層フィルムより離型フィルムを剥がした時の状況より、離型特性を評価した。
○:離型フィルムがきれいに剥がれ、粘着剤が離型層に付着する現象が見られない
△:離型フィルムは剥がれるが、速い速度で剥離した場合に粘着剤が離型層に付着する ×:離型フィルムに粘着剤が付着する、上手く剥がれない。
(5) Release characteristics The release characteristics were evaluated from the situation when the release film was peeled off from the laminated film having the adhesive layer.
○: The release film peels cleanly, and the phenomenon that the adhesive adheres to the release layer is not observed. Δ: The release film peels off, but the adhesive adheres to the release layer when peeled at a high speed. Adhesive adheres to the release film and does not peel off well.
(6)総合評価
製膜性、生産性、検査特性全てを考慮に入れた評価を行う。次のような基準で判断する。
○:生産しても十分に製品として供給できる
△:生産性が良い、かつ、不具合の頻度が少ない
×:生産性が悪い。不具合が多発する。
(6) Comprehensive evaluation An evaluation that takes into consideration all the film-forming properties, productivity, and inspection characteristics. Judgment is based on the following criteria.
○: Even if it is produced, it can be sufficiently supplied as a product. Δ: Productivity is good and the frequency of defects is low. ×: Productivity is poor. Many troubles occur.
実施例1
<ポリエステルフィルムの製造>
先に述べたポリエステルを原料として、ベント付き押出機に供給し、290℃で溶融押出した後、静電印加密着法を用いて表面温度を40℃に設定した冷却ロール上で冷却固化して厚さ約550μmの無定形フィルムを得た。
このフィルムを85℃で縦方向に3.7倍延伸し、100℃で横方向に3.9倍延伸し、210℃で熱処理して、厚さ38μmの二軸延伸ポリエステルフィルムを得た
Example 1
<Manufacture of polyester film>
The polyester described above is used as a raw material, supplied to an extruder with a vent, melt-extruded at 290 ° C, and then cooled and solidified on a cooling roll set at a surface temperature of 40 ° C using an electrostatic application adhesion method. An amorphous film having a thickness of about 550 μm was obtained.
This film was stretched 3.7 times in the longitudinal direction at 85 ° C., stretched 3.9 times in the transverse direction at 100 ° C., and heat treated at 210 ° C. to obtain a biaxially stretched polyester film having a thickness of 38 μm.
得られたポリエステルフィルムに、下記に示す離型剤組成−Aからなる離型剤を塗布量(乾燥後)が0.12g/m2になるようにリバースグラビアコート方式により塗布し、ドライヤー温度120℃、ライン速度30m/分の条件でロール状の離型ポリエステルフィルムを得た。得られた離型ポリエステルフィルムは、300mm/分速度域での剥離力が14mN/cm離型フィルムで、かつ、10000mm/分速度域での剥離力が32mN/cmであった。 A release agent composed of release agent composition-A shown below was applied to the obtained polyester film by a reverse gravure coating method so that the coating amount (after drying) was 0.12 g / m 2 , and the dryer temperature was 120. A roll-shaped release polyester film was obtained under the conditions of ° C and a line speed of 30 m / min. The obtained release polyester film had a release force of 14 mN / cm at a speed of 300 mm / min and a release force of 32 mN / cm at a speed of 10,000 mm / min.
<離型剤組成−A>
硬化型シリコーン樹脂(LTC303E:東レ・ダウコーニング製) 20部 付加型白金触媒(SRX212:東レ・ダウコーニング製) 0.2部
MEK/トルエン/n−ヘプタン混合溶媒(混合比率は1:1:1)
離型剤組成−Aの移行性分量:15重量%
<Releasing agent composition-A>
Curable silicone resin (LTC303E: manufactured by Toray Dow Corning) 20 parts Addition type platinum catalyst (SRX212: manufactured by Toray Dow Corning) 0.2 parts MEK / toluene / n-heptane mixed solvent (mixing ratio is 1: 1: 1) )
Release agent composition-A transferable amount: 15% by weight
得られたポリエステルフィルムは、下記方法で偏向板を作成し、剥離特性の評価を行った。得られた離型フィルムは偏光板きれいに剥がれ、粘着剤が離型層に付着する現象が見られなかった。 For the obtained polyester film, a polarizing plate was prepared by the following method, and the peeling characteristics were evaluated. The obtained release film was peeled off cleanly, and the phenomenon that the adhesive adhered to the release layer was not observed.
<離型フィルム付き偏光板の製造>
偏光板に下記に示すアクリル粘着剤を、乾燥後の厚みが25μmとなるように塗布し、130℃の乾燥炉内を30秒で通過させた後、離型フィルムを貼り合わせ、粘着剤を介して離型フィルムと偏光フィルムが密着された離型フィルム付き偏光板を作成した。フィルムの貼り合せ方向は、離型フィルムの幅方向が、偏光フィルムの配向軸と平行となるように行った。
・アクリル粘着剤塗布液
アクリル粘着剤(オリバインBPS429−4:東洋インキ製) 100部
硬化剤(BPS8515:東洋インキ製) 3部
MEK/トルエン混合溶媒(混合比率は1:1) 50部
<Manufacture of polarizing plate with release film>
The acrylic adhesive shown below is applied to the polarizing plate so that the thickness after drying is 25 μm, and after passing through a 130 ° C. drying oven in 30 seconds, the release film is bonded, and the adhesive is interposed. Thus, a polarizing plate with a release film in which the release film and the polarizing film were adhered to each other was prepared. The laminating direction of the film was performed so that the width direction of the release film was parallel to the orientation axis of the polarizing film.
Acrylic adhesive coating solution Acrylic adhesive (Olivein BPS429-4: manufactured by Toyo Ink) 100 parts Curing agent (BPS8515: manufactured by Toyo Ink) 3 parts MEK / toluene mixed solvent (mixing ratio is 1: 1) 50 parts
実施例2〜4:
実施例1において、ポリエステルフィルム製造時の塗離型剤塗布量(乾燥後)を変更する以外は実施例1と同様にして製造し、ポリエステルフィルムを得た。得られた結果をまとめて下記表1に示す。
Examples 2-4:
In Example 1, it manufactured like Example 1 except changing the coating amount (after drying) of the release agent at the time of polyester film manufacture, and obtained the polyester film. The obtained results are summarized in Table 1 below.
実施例5:
実施例2において、離型剤組成−Aにシリコーンオイル(AL−1)3部を添加したものを塗布する以外は実施例2と同様にして製造し、ポリエステルフィルムを得た。得られた結果をまとめて下記表1に示す。
Example 5:
In Example 2, it manufactured like Example 2 except having apply | coated what added 3 parts of silicone oil (AL-1) to mold release composition-A, and obtained the polyester film. The obtained results are summarized in Table 1 below.
比較例1:
離型剤組成を下記のとおり変更する以外は、実施例1と同様にして製造し、ポリエステルフィルムを得た。
<離型剤組成−B>
硬化型シリコーン樹脂(KS−847H:信越化学製) 20部
付加型白金触媒(PL−50T:信越化学製) 0.2部
MEK/トルエン/n−ヘプタン混合溶媒(混合比率は1:1:1)
離型剤組成−Bの移行性分量:5重量%
Comparative Example 1:
A polyester film was obtained in the same manner as in Example 1 except that the release agent composition was changed as follows.
<Releasing agent composition-B>
Curable silicone resin (KS-847H: manufactured by Shin-Etsu Chemical Co., Ltd.) 20 parts Addition type platinum catalyst (PL-50T: manufactured by Shin-Etsu Chemical Co., Ltd.) 0.2 part MEK / toluene / n-heptane mixed solvent (mixing ratio is 1: 1: 1) )
Release agent composition-B migration amount: 5% by weight
比較例2:
離型剤組成を下記のとおり変更する以外は、実施例1と同様にして製造し、ポリエステルフィルムを得た。得られた結果をまとめて下記表2に示す。
<離型剤組成−C>
硬化型シリコーン樹脂(LTC303E:東レ・ダウコーニング製) 20部
シリコーンオイル(KS−64−100cs) 0.18部
付加型白金触媒(SRX212:東レ・ダウコーニング製) 0.2部
MEK/トルエン/n−ヘプタン混合溶媒(混合比率は1:1:1)
離型剤組成−Cの移行性分量:23重量%
Comparative Example 2:
A polyester film was obtained in the same manner as in Example 1 except that the release agent composition was changed as follows. The results obtained are summarized in Table 2 below.
<Releasing agent composition-C>
Curable silicone resin (LTC303E: manufactured by Toray Dow Corning) 20 parts Silicone oil (KS-64-100cs) 0.18 parts Addition type platinum catalyst (SRX212: manufactured by Toray Dow Corning) 0.2 parts MEK / toluene / n -Heptane mixed solvent (mixing ratio is 1: 1: 1)
Release agent composition-C migration amount: 23% by weight
比較例3:
実施例1において、<離型組成−A>で、塗布量を0.25g/m2に変更する以外は実施例1と同様にして製造し、ポリエステルフィルムを得た。得られた結果をまとめて下記表2に示す。
Comparative Example 3:
In Example 1, it was manufactured in the same manner as in Example 1 except that <mold release composition-A> and the coating amount was changed to 0.25 g / m 2 to obtain a polyester film. The results obtained are summarized in Table 2 below.
比較例4:
比較例1において、<離型組成−C>で、塗布量を0.08g/m2に変更する以外は比較例1と同様にして製造し、ポリエステルフィルムを得た。得られた結果をまとめて下記表2に示す。
Comparative Example 4:
In Comparative Example 1, a polyester film was obtained in the same manner as in Comparative Example 1 except that <mold release composition-C> and the coating amount was changed to 0.08 g / m 2 . The results obtained are summarized in Table 2 below.
本発明のポリエステルフィルムは、需要が大きい光学用途における基材レス両面粘着シート用分野で、生産性がよく、剥離速度依存性が小さい離型ポリエステルフィルムとして好適に利用できる。 The polyester film of the present invention can be suitably used as a release polyester film having good productivity and low release rate dependency in the field of substrate-less double-sided pressure-sensitive adhesive sheets in optical applications where demand is great.
Claims (1)
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2011069055A JP2012179888A (en) | 2011-02-09 | 2011-03-28 | Polyester film for substrate-less double-sided adhesive sheet |
KR1020137011397A KR101707863B1 (en) | 2010-12-27 | 2011-12-19 | Mold release film |
CN201180057701.3A CN103229080B (en) | 2010-12-27 | 2011-12-19 | Mold release film |
PCT/JP2011/079373 WO2012090762A1 (en) | 2010-12-27 | 2011-12-19 | Mold release film |
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2011026004 | 2011-02-09 | ||
JP2011026004 | 2011-02-09 | ||
JP2011069055A JP2012179888A (en) | 2011-02-09 | 2011-03-28 | Polyester film for substrate-less double-sided adhesive sheet |
Publications (1)
Publication Number | Publication Date |
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JP2012179888A true JP2012179888A (en) | 2012-09-20 |
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ID=47011520
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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JP2011069055A Withdrawn JP2012179888A (en) | 2010-12-27 | 2011-03-28 | Polyester film for substrate-less double-sided adhesive sheet |
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JP (1) | JP2012179888A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2015208863A (en) * | 2014-04-24 | 2015-11-24 | 三菱樹脂株式会社 | Polyester film |
KR20170099980A (en) | 2015-03-23 | 2017-09-01 | 미쯔비시 케미컬 주식회사 | Release film |
WO2024070440A1 (en) * | 2022-09-29 | 2024-04-04 | 住友化学株式会社 | Optical laminate |
-
2011
- 2011-03-28 JP JP2011069055A patent/JP2012179888A/en not_active Withdrawn
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2015208863A (en) * | 2014-04-24 | 2015-11-24 | 三菱樹脂株式会社 | Polyester film |
KR20170099980A (en) | 2015-03-23 | 2017-09-01 | 미쯔비시 케미컬 주식회사 | Release film |
WO2024070440A1 (en) * | 2022-09-29 | 2024-04-04 | 住友化学株式会社 | Optical laminate |
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