JP5357064B2 - Optical film - Google Patents
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- JP5357064B2 JP5357064B2 JP2010000063A JP2010000063A JP5357064B2 JP 5357064 B2 JP5357064 B2 JP 5357064B2 JP 2010000063 A JP2010000063 A JP 2010000063A JP 2010000063 A JP2010000063 A JP 2010000063A JP 5357064 B2 JP5357064 B2 JP 5357064B2
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- 239000012788 optical film Substances 0.000 title claims abstract description 32
- 239000004094 surface-active agent Substances 0.000 claims abstract description 78
- 239000010408 film Substances 0.000 claims abstract description 45
- 229920005596 polymer binder Polymers 0.000 claims abstract description 30
- 239000002491 polymer binding agent Substances 0.000 claims abstract description 30
- 125000001165 hydrophobic group Chemical group 0.000 claims abstract description 14
- 239000012790 adhesive layer Substances 0.000 claims abstract description 13
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical group CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 12
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 12
- -1 polyethylene terephthalate Polymers 0.000 claims abstract description 11
- 125000006353 oxyethylene group Chemical group 0.000 claims abstract description 9
- 229920001577 copolymer Polymers 0.000 claims abstract description 8
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 5
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 5
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 5
- 239000010410 layer Substances 0.000 claims description 45
- 125000004432 carbon atom Chemical group C* 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 abstract description 30
- 238000000576 coating method Methods 0.000 abstract description 30
- 229920000728 polyester Polymers 0.000 description 54
- 239000000203 mixture Substances 0.000 description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 36
- 239000007788 liquid Substances 0.000 description 19
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 18
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 18
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 16
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 15
- 238000000034 method Methods 0.000 description 13
- 238000006243 chemical reaction Methods 0.000 description 12
- 230000003247 decreasing effect Effects 0.000 description 10
- HLZKNKRTKFSKGZ-UHFFFAOYSA-N tetradecan-1-ol Chemical compound CCCCCCCCCCCCCCO HLZKNKRTKFSKGZ-UHFFFAOYSA-N 0.000 description 10
- 238000011156 evaluation Methods 0.000 description 9
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 8
- 239000008199 coating composition Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- 239000011230 binding agent Substances 0.000 description 5
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 5
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 5
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 5
- 238000006467 substitution reaction Methods 0.000 description 5
- 239000002216 antistatic agent Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 230000018044 dehydration Effects 0.000 description 4
- 238000006297 dehydration reaction Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 229920001519 homopolymer Polymers 0.000 description 3
- 229920001225 polyester resin Polymers 0.000 description 3
- 239000004645 polyester resin Substances 0.000 description 3
- BBMCTIGTTCKYKF-UHFFFAOYSA-N 1-heptanol Chemical compound CCCCCCCO BBMCTIGTTCKYKF-UHFFFAOYSA-N 0.000 description 2
- 125000003504 2-oxazolinyl group Chemical group O1C(=NCC1)* 0.000 description 2
- LPIQIQPLUVLISR-UHFFFAOYSA-N 2-prop-1-en-2-yl-4,5-dihydro-1,3-oxazole Chemical compound CC(=C)C1=NCCO1 LPIQIQPLUVLISR-UHFFFAOYSA-N 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 2
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 2
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- VNGOYPQMJFJDLV-UHFFFAOYSA-N dimethyl benzene-1,3-dicarboxylate Chemical compound COC(=O)C1=CC=CC(C(=O)OC)=C1 VNGOYPQMJFJDLV-UHFFFAOYSA-N 0.000 description 2
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 230000009477 glass transition Effects 0.000 description 2
- 238000009775 high-speed stirring Methods 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- REIUXOLGHVXAEO-UHFFFAOYSA-N pentadecan-1-ol Chemical compound CCCCCCCCCCCCCCCO REIUXOLGHVXAEO-UHFFFAOYSA-N 0.000 description 2
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 229920006267 polyester film Polymers 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005809 transesterification reaction Methods 0.000 description 2
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 description 1
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- MMINFSMURORWKH-UHFFFAOYSA-N 3,6-dioxabicyclo[6.2.2]dodeca-1(10),8,11-triene-2,7-dione Chemical group O=C1OCCOC(=O)C2=CC=C1C=C2 MMINFSMURORWKH-UHFFFAOYSA-N 0.000 description 1
- 239000004214 Fast Green FCF Substances 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- GYUVMLBYMPKZAZ-UHFFFAOYSA-N dimethyl naphthalene-2,6-dicarboxylate Chemical compound C1=C(C(=O)OC)C=CC2=CC(C(=O)OC)=CC=C21 GYUVMLBYMPKZAZ-UHFFFAOYSA-N 0.000 description 1
- 238000009998 heat setting Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- KYTZHLUVELPASH-UHFFFAOYSA-N naphthalene-1,2-dicarboxylic acid Chemical compound C1=CC=CC2=C(C(O)=O)C(C(=O)O)=CC=C21 KYTZHLUVELPASH-UHFFFAOYSA-N 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
- 239000003960 organic solvent Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- Laminated Bodies (AREA)
Abstract
Description
本発明は、光学用フィルムに関する。詳しくは、表示装置のタッチパネル基材や保護フィルム等、光を透過する態様で用いる部材として使用される光学用フィルムに関する。 The present invention relates to an optical film. In detail, it is related with the film for optics used as a member used in the aspect which permeate | transmits light, such as the touchscreen base material of a display apparatus, and a protective film.
光学用フィルムとして二軸延伸ポリエステルフィルムが一般的に用いられており、フィルムを製膜した後、ハードコート層や粘着剤層といった加工層が設けられる。
このため、二軸延伸ポリエステルフィルムと加工層との密着性をよくするために、フィルム表面には易接着層が設けられる。易接着層はポリエステルのエマルジョンをコーティングすることにより塗設されるが、コーティングの際に、ロールによるせん断応力でエマルションが凝集し、しばしば異物が発生する。そうなると、凝集異物を含む易接着層の上にハードコート層や粘着剤層を設けても異物が残ってしまい、その光学フィルムを用いた表示装置の表示品質を低下させることになる。
A biaxially stretched polyester film is generally used as an optical film, and after the film is formed, processed layers such as a hard coat layer and an adhesive layer are provided.
For this reason, in order to improve the adhesiveness of a biaxially stretched polyester film and a process layer, an easily bonding layer is provided in the film surface. The easy-adhesion layer is applied by coating an emulsion of polyester. During coating, the emulsion aggregates due to the shear stress of the roll, and foreign matter is often generated. Then, even if a hard coat layer or a pressure-sensitive adhesive layer is provided on the easy-adhesion layer containing aggregated foreign substances, the foreign substances remain, and the display quality of the display device using the optical film is deteriorated.
本発明は、易接着層を設けるコーティングの際に発生する異物を低減した光学用フィルムを提供することを課題とする。 This invention makes it a subject to provide the film for optics which reduced the foreign material which generate | occur | produces in the coating which provides an easily bonding layer.
すなわち本発明は、ポリエチレンテレフタレート二軸延伸フィルムおよびその少なくとも片面に設けられた厚み１０〜３００ｎｍの易接着層からなる光学用フィルムであって、易接着層は高分子バインダーおよび界面活性剤を含有し、易接着層における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー１００重量部に対して界面活性剤０．５〜１０重量部であり、易接着層における界面活性剤の含有率は易接着層の重量を基準に０．５〜６重量％であり、界面活性剤は疎水基と親水基とからなり、疎水基は炭素数１３〜１５の直鎖炭化水素であり、親水基はオキシエチレンとオキシプロピレンの共重合体からなり、オキシエチレンの親水基における割合が３０〜５０モル％であり、界面活性剤の重量平均分子量が１２００〜１６００であることを特徴とする光学用フィルムである。 That is, the present invention is an optical film comprising a polyethylene terephthalate biaxially stretched film and an easy-adhesion layer having a thickness of 10 to 300 nm provided on at least one surface thereof, and the easy-adhesion layer contains a polymer binder and a surfactant. The ratio of the content of the polymer binder and the surfactant in the easy adhesion layer is 0.5 to 10 parts by weight of the surfactant with respect to 100 parts by weight of the polymer binder, and the content of the surfactant in the easy adhesion layer The ratio is 0.5 to 6% by weight based on the weight of the easy-adhesion layer, the surfactant is composed of a hydrophobic group and a hydrophilic group, and the hydrophobic group is a linear hydrocarbon having 13 to 15 carbon atoms, and is hydrophilic. The group consists of a copolymer of oxyethylene and oxypropylene, the proportion of oxyethylene in the hydrophilic group is 30 to 50 mol%, and the weight average molecular weight of the surfactant is 1200 to An optical film, which is a 600.
本発明によれば、易接着層を設けるコーティングの際に発生する異物を低減した光学用フィルムを提供することができる。 ADVANTAGE OF THE INVENTION According to this invention, the film for optics which reduced the foreign material which generate | occur | produces in the case of the coating which provides an easily bonding layer can be provided.
以下、本発明を詳細に説明する。 Hereinafter, the present invention will be described in detail.
［ポリエチレンテレフタレート二軸延伸フィルム］
本発明におけるポリエチレンテレフタレート二軸延伸フィルムは、ポリエチレンテレフタレートからなる二軸延伸フィルムである。
本発明におけるポリエチレンテレフタレートは、エチレンテレフタレート単位を、全繰返し単位を基準に９５％以上、好ましくは９８％以上の繰り返し単位としてなるポリエステルである。これは、ホモポリマーであってもよく、共重合ポリマーであってもよい。共重合ポリマーである場合、共重合成分として、例えば、イソフタル酸、ナフタレンジカルボン酸、ジエチレングリコールを用いることができる。ポリエチレンテレフタレートとして最も好ましいものは、ポリエチレンテレフタレートホモポリマーである。
光学用フィルムとしての機械的特性を得るために二軸延伸フィルムの厚みは、好ましくは３０〜２５０μｍ、さらに好ましくは７０〜２２５μｍである。
[Polyethylene terephthalate biaxially stretched film]
The polyethylene terephthalate biaxially stretched film in the present invention is a biaxially stretched film made of polyethylene terephthalate.
The polyethylene terephthalate in the present invention is a polyester having ethylene terephthalate units as 95% or more, preferably 98% or more repeating units based on all repeating units. This may be a homopolymer or a copolymer. In the case of a copolymer, for example, isophthalic acid, naphthalene dicarboxylic acid, or diethylene glycol can be used as the copolymer component. Most preferred as polyethylene terephthalate is a polyethylene terephthalate homopolymer.
In order to obtain mechanical properties as an optical film, the thickness of the biaxially stretched film is preferably 30 to 250 μm, more preferably 70 to 225 μm.
［易接着層］
本発明の光学用フィルムは、ポリエチレンテレフタレート二軸延伸フィルムの片面または両面に易接着層を備える。易接着層の厚みは１０〜３００ｎｍ、好ましくは５０〜１２０ｎｍである。塗布層の厚みがこの範囲にないと、本発明の光学用フィルムのうえにハードコート層を設けたときに密着性が不足したり、干渉斑が生じたりするので、光学用フィルムとして不適である。
[Easily adhesive layer]
The optical film of the present invention includes an easy-adhesion layer on one side or both sides of a polyethylene terephthalate biaxially stretched film. The thickness of the easy adhesion layer is 10 to 300 nm, preferably 50 to 120 nm. If the thickness of the coating layer is not within this range, adhesion is insufficient or interference spots occur when a hard coat layer is provided on the optical film of the present invention, which is not suitable as an optical film. .
［高分子バインダー］
易接着層の高分子バインダーは、易接着層の表面にハードコート層を設ける場合にハードコート層との良好な接着性を得る観点から、ポリエステル樹脂およびオキサゾリン基とポリアルキレンオキシド鎖とを有するアクリル樹脂の混合物であることが好ましい。この高分子バインダーは、水に可溶性または分散性のものが好ましいが、多少の有機溶剤を含有する水に可溶なものも好ましく用いることができる。高分子バインダーのポリエステル樹脂のガラス転移点は、好ましくは４０〜１００℃、さらに好ましくは６０〜８０℃である。この範囲であれば、優れた接着性、耐傷性、耐ブロッキング性および塗布外観を得ることができる。
[Polymer binder]
The polymer binder of the easy adhesion layer is an acrylic resin having a polyester resin and an oxazoline group and a polyalkylene oxide chain from the viewpoint of obtaining good adhesion to the hard coat layer when a hard coat layer is provided on the surface of the easy adhesion layer. A mixture of resins is preferred. This polymer binder is preferably soluble or dispersible in water, but water-soluble one containing some organic solvent can also be preferably used. The glass transition point of the polyester resin of the polymer binder is preferably 40 to 100 ° C, more preferably 60 to 80 ° C. If it is this range, the outstanding adhesiveness, scratch resistance, blocking resistance, and application | coating external appearance can be obtained.
この場合、高分子バインダーを構成するポリエステル樹脂の塗布層中での含有割合は、好ましくは５〜９５重量％、さらに好ましくは５０〜９０重量％である。高分子バインダーを構成するオキサゾリン基とポリアルキレンオキシド鎖とを有するアクリル樹脂の、塗布層中での含有割合は、好ましくは５〜９５重量％、さらに好ましくは１０〜５０重量％である。高分子バインダーがこの範囲の組成であることで、ハードコート層との良好な接着性を得るとともに、フィルムへの特に良好な密着性を得ることができる。 In this case, the content ratio of the polyester resin constituting the polymer binder in the coating layer is preferably 5 to 95% by weight, more preferably 50 to 90% by weight. The content ratio in the coating layer of the acrylic resin having an oxazoline group and a polyalkylene oxide chain constituting the polymer binder is preferably 5 to 95% by weight, more preferably 10 to 50% by weight. When the polymer binder has a composition within this range, good adhesion to the hard coat layer can be obtained, and particularly good adhesion to the film can be obtained.
［界面活性剤］
本発明における界面活性剤は親水基と疎水基からなり、疎水基は炭素数が１３〜１５の直鎖炭化水素であり、かつ親水基はオキシエチレンとオキシプロピレンの共重合体からなり、オキシエチレンの親水基における割合が３０〜５０モル％である界面活性剤である。
易接着層における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー１００重量部に対して界面活性剤０．５〜１０重量部、好ましくは１〜３重量部である。界面活性剤の量が０．５重量部未満であるとポリエステルバインダーの水分散性が悪化する。他方、１０重量部を越えると余剰の界面活性剤自身が凝集を促進する作用を持つ。
易接着層における界面活性剤の含有率は易接着層の重量を基準に０．５〜６重量％である。０．５重量％未満であると、ポリエステルバインダーの水分散性が悪化する。他方、６重量％を超えるとロールコーターで塗布する時のロールとフィルムとのせん断応力によってポリエステルバインダーを凝集させてしまう。
[Surfactant]
The surfactant in the present invention is composed of a hydrophilic group and a hydrophobic group, the hydrophobic group is a linear hydrocarbon having 13 to 15 carbon atoms, and the hydrophilic group is composed of a copolymer of oxyethylene and oxypropylene. Is a surfactant having a ratio of 30 to 50 mol% in the hydrophilic group.
The ratio of the content of the polymer binder and the surfactant in the easy-adhesion layer is 0.5 to 10 parts by weight, preferably 1 to 3 parts by weight, based on 100 parts by weight of the polymer binder. When the amount of the surfactant is less than 0.5 parts by weight, the water dispersibility of the polyester binder is deteriorated. On the other hand, when it exceeds 10 parts by weight, the surplus surfactant itself has an action of promoting aggregation.
The content of the surfactant in the easy adhesion layer is 0.5 to 6% by weight based on the weight of the easy adhesion layer. If it is less than 0.5% by weight, the water dispersibility of the polyester binder deteriorates. On the other hand, if it exceeds 6% by weight, the polyester binder will be agglomerated by the shear stress between the roll and the film when applied by a roll coater.
界面活性剤は疎水基と親水基とからなる。疎水基は炭素数１３〜１５の直鎖炭化水素である。疎水基の炭素数が１３未満であると易接着層をコーティングするときに高分子バインダーが凝集する、１５を超えると表面張力が下がりコーティングの斑になる。親水基はオキシエチレンとオキシプロピレンの共重合体からなる。オキシエチレンの親水基における割合が３０〜５０モル％である。３０モル％未満であると水分散がうまくいかない、５０モル％を超えるとコーティングするときに高分子バインダーが凝集する。
界面活性剤の分子量は１２００〜１６００である。界面活性剤の分子量がこの範囲から外れると、ポリエステルバインダーの水分散性が悪化する。また、ロールコーターで塗布する時のロールとフィルムとのせん断応力によってポリエステルバインダーを凝集させてしまう。
The surfactant consists of a hydrophobic group and a hydrophilic group. The hydrophobic group is a straight chain hydrocarbon having 13 to 15 carbon atoms. When the number of carbon atoms of the hydrophobic group is less than 13, the polymer binder aggregates when coating the easy-adhesion layer. When the number of the hydrophobic group exceeds 15, the surface tension decreases and the coating becomes uneven. The hydrophilic group consists of a copolymer of oxyethylene and oxypropylene. The ratio in the hydrophilic group of oxyethylene is 30-50 mol%. If it is less than 30 mol%, water dispersion will not be successful, and if it exceeds 50 mol%, the polymer binder will aggregate when coating.
The molecular weight of the surfactant is 1200-1600. When the molecular weight of the surfactant is out of this range, the water dispersibility of the polyester binder deteriorates. In addition, the polyester binder is agglomerated by the shear stress between the roll and the film when applied by a roll coater.
［帯電防止剤］
易接着層は、加工時の剥離帯電による異物の付着を防止するために、帯電防止剤を含有していることが好ましい。易接着層が耐電防止剤を含有する場合、易接着層の重量を基準として、好ましくは２〜５重量％である。この範囲で含有することにより、接着性および密着性を損なうことなく、異物の付着を防止する帯電防止性を付与することができる。
[Antistatic agent]
The easy-adhesion layer preferably contains an antistatic agent in order to prevent adhesion of foreign matters due to peeling charging during processing. When an easily bonding layer contains an antistatic agent, it is preferably 2 to 5% by weight based on the weight of the easily bonding layer. By containing in this range, the antistatic property which prevents adhesion of a foreign material can be provided, without impairing adhesiveness and adhesiveness.
［異物］
本発明の光学用フィルムにおいては、易接着層における、凸部の大きさの最大径が２０μｍ以上かつ凸部の高さが１μｍ以上の異物が３個以下／１００ｍ２であることが好ましい。異物が３個／１００ｍ２を超えると、光学用基材を製造する際の歩留まりが低下して好ましくない。
[Foreign matter]
In the optical film of the present invention, it is preferable that in the easy-adhesive layer, there are 3 or less / 100 m 2 of foreign matter having a maximum diameter of the protrusions of 20 μm or more and a height of the protrusions of 1 μm or more. If the number of foreign matters exceeds 3/100 m 2 , the yield in producing an optical substrate is lowered, which is not preferable.
［製造方法］
本発明に用いる界面活性剤は、テトラデカノールもしくはペンタデカノールに触媒として水酸化ナトリウムを加え、攪拌しながら１５０〜１８０℃まで加熱し、これにエチレンオキサイドとプロピレンオキサイドを加えることで製造することができる。
本発明の光学用フィルムを製造するためには、コーティング速度を遅くすることができる同時二軸延伸法にて延伸することが肝要である。以下、ポリエステルの融点をＴｍ、ガラス転移温度をＴｇと略記する。
[Production method]
The surfactant used in the present invention is manufactured by adding sodium hydroxide as a catalyst to tetradecanol or pentadecanol, heating to 150 to 180 ° C. with stirring, and adding ethylene oxide and propylene oxide thereto. Can do.
In order to produce the optical film of the present invention, it is important to stretch the film by a simultaneous biaxial stretching method that can reduce the coating speed. Hereinafter, the melting point of polyester is abbreviated as Tm, and the glass transition temperature is abbreviated as Tg.
本発明の光学用フィルムは、まず、ポリエステルを溶融し、シート状に押出し、冷却ドラムで冷却して未延伸フィルムとし、未延伸フィルムの少なくとも片面に易接着層の塗液を塗布したあと、二軸方向に同時に延伸し、熱固定し、熱弛緩処理することによって得ることができる。具体的には、ポリエステルを、（Ｔｍ＋１０℃）〜（Ｔｍ＋３０℃）の温度で溶融し、押出して未延伸フィルムとし、未延伸フィルムの少なくとも片面に易接着層をロールコーターで積層したあと、同時に二軸方向に、Ｔｇ〜（Ｔｇ＋１０℃）の温度で縦方向に３．０〜３．４倍、横方向に３．４〜４．０倍の倍率で延伸する。得られた延伸フィルムを、（Ｔｇ＋６０）〜Ｔｍの温度で熱固定する。例えばポリエステルが、ポリエチレンテレフタレートホモポリマーである場合、２３０〜２４０℃の温度で、１〜６０秒の時間熱固定処理するのが好ましい。 The optical film of the present invention is obtained by first melting a polyester, extruding it into a sheet, cooling it with a cooling drum to form an unstretched film, applying an easy-adhesion layer coating liquid on at least one side of the unstretched film, It can be obtained by simultaneously stretching in the axial direction, heat setting, and heat relaxation treatment. Specifically, the polyester is melted at a temperature of (Tm + 10 ° C.) to (Tm + 30 ° C.), extruded to be an unstretched film, and an easy-adhesion layer is laminated on at least one side of the unstretched film with a roll coater. In the axial direction, the film is stretched at a temperature of Tg to (Tg + 10 ° C.) at a magnification of 3.0 to 3.4 times in the longitudinal direction and 3.4 to 4.0 times in the transverse direction. The obtained stretched film is heat-set at a temperature of (Tg + 60) to Tm. For example, when polyester is a polyethylene terephthalate homopolymer, it is preferable to heat-set at a temperature of 230 to 240 ° C. for 1 to 60 seconds.
易接着層の塗布は、以下の方法で行うことができる。走行するフィルムの速度は１０ｍ／ｍｉｎとし、８０線のグラビアロールを２０ｍ／ｍｉｎの回転速度で塗液を汲み上げ、ドクターブレードによってグラビアロール上の塗液を一定量となるように掻き落とし、フィルムに塗布する。もしくは、８０線のグラビアロールを１５ｍ／ｍｉｎの回転速度で塗液を汲み上げ、ドクターブレードによってグラビアロール上の塗液を一定量となるように掻き落とし、２５ｍ／ｍｉｎで回転するゴムロールに転写させ、フィルムに塗布する。 Application | coating of an easily bonding layer can be performed with the following method. The speed of the traveling film is 10 m / min, the 80-line gravure roll is pumped up at a rotational speed of 20 m / min, and the coating liquid on the gravure roll is scraped off to a certain amount by a doctor blade. Apply. Alternatively, an 80-line gravure roll is pumped up at a rotation speed of 15 m / min, the doctor liquid is scraped off to a constant amount by a doctor blade, and transferred to a rubber roll rotating at 25 m / min, Apply to film.
以下、実施例により本発明を具体的に説明する。
フィルムの評価および実施例で用いた界面活性剤の合成は、以下の方法で行った。
Hereinafter, the present invention will be described specifically by way of examples.
Evaluation of the film and synthesis of the surfactant used in the examples were performed by the following methods.
（１）異物の個数
以下に説明する光学欠点検出装置により、巾１ｍ、長さ１００ｍのフィルムロールについて、光学的に最大径が２０μｍ以上の大きさと認識される光学欠点を異物として検出した。巻取り機の繰出し側と巻取り側の間に、パナソニック社製三波長形蛍光灯ラピッドスタータ形４０Ｗの蛍光灯を巾１０ｍｍのスリットでマスキングした光源をフィルムの上方５ｃｍの位置に設置し、フィルムロールをシワが入らないように、この巻取り機で巻き返し、この際に、繰出したフィルムへ光源と受光器とを結ぶ直線と測定対象のフィルム面の垂直方向とのなす角度が１２度になるようにフィルムに光線を入射し、フィルムに光線があたる位置に光学欠点が存在すると受光器のＣＣＤイメージセンサカメラで電気信号に変換し、光学欠点のある位置と無い位置での電機信号のシグナル強度変化により異物を認識し、異物のフィルム上での長手方向および横手方向の位置情報を記録した。この方法による異物の検出を、フィルムの繰出し速度５ｍ毎分でフィルムの長手方向１００ｍについて実施して、フィルムの１００ｍ２あたりに存在する異物の個数と位置情報を検出した。
異物の高さ測定は、位置情報を基に異物を含む領域を適切な大きさにサンプリングし、オリンパス社製レーザー顕微鏡ＬＥＸＴ ＯＬＳ４０００で異物の高さを測定した。
最終的に、凸部の大きさの最大径が２０μｍ以上かつ凸部の高さが１μｍ以上の異物の数を算出した。
(1) Number of Foreign Objects Optical defects that are optically recognized as having a maximum diameter of 20 μm or more were detected as foreign objects on a film roll having a width of 1 m and a length of 100 m using an optical defect detection apparatus described below. Between the unwinding side and the winding side of the winder, a light source obtained by masking a three-wavelength fluorescent lamp rapid starter type 40W made by Panasonic with a slit with a width of 10 mm is placed at a position 5 cm above the film. The roll is rewound by this winder so as not to be wrinkled. At this time, the angle formed by the straight line connecting the light source and the light receiver to the fed film and the vertical direction of the film surface to be measured is 12 degrees. When a light beam is incident on the film and there is an optical defect at the position where the light beam hits the film, it is converted into an electrical signal by the CCD image sensor camera of the receiver, and the signal strength of the electrical signal at the position where there is no optical defect The foreign matter was recognized by the change, and the positional information of the foreign matter on the film in the longitudinal direction and the lateral direction was recorded. The detection of foreign matters by this method was carried out in the longitudinal direction of the film at 100 m at a film feeding speed of 5 m per minute, and the number and position information of foreign matters existing per 100 m 2 of the film were detected.
The height of the foreign material was measured by sampling an area including the foreign material to an appropriate size based on the position information, and measuring the height of the foreign material using a laser microscope LEXT OLS4000 manufactured by Olympus.
Finally, the number of foreign matters having a maximum diameter of the convex portion of 20 μm or more and a height of the convex portion of 1 μm or more was calculated.
（２）界面活性剤の重量平均分子量
界面活性剤の重量平均分子量は、大塚電子社製ＤＬＳ−８０００で測定して求めた。
(2) Weight average molecular weight of surfactant The weight average molecular weight of the surfactant was determined by measuring with DLS-8000 manufactured by Otsuka Electronics Co., Ltd.
（３）界面活性剤の疎水基の炭素数
疎水基の炭素数は、ＢＲＵＫＥＲ社製核磁気共鳴装置ＡＶＡＮＣＥで１Ｈ−ＮＭＲの測定チャートから読み取った。
(3) Carbon number of hydrophobic group of surfactant The carbon number of the hydrophobic group was read from a measurement chart of 1 H-NMR with a nuclear magnetic resonance apparatus AVANCE manufactured by BRUKER.
（４）易接着層の厚み
易接着層の膜厚は、フィルムサンプルの断面を日立社製電界放出形透過電子顕微鏡 ＨＦ−３３００で観察し、実際の膜厚を測定した。
(4) Thickness of easy-adhesion layer The film thickness of the easy-adhesion layer was measured by observing the cross section of the film sample with a field emission transmission electron microscope HF-3300 manufactured by Hitachi, Ltd.
（５）界面活性剤の合成
界面活性剤Ａ〜Ｆを特許３１８７８４６号公報（特願平１０−５２１２２６号）に記載の方法に準拠して、以下の方法にて作成した。「部」は重量部を意味する。
(5) Synthesis of Surfactant Surfactants A to F were prepared by the following method based on the method described in Japanese Patent No. 318784 (Japanese Patent Application No. 10-521226). “Parts” means parts by weight.
界面活性剤Ａ
エチレンオキサイド用とプロピレンオキサイド用の２つ計量槽の付いた５リットルの回転攪拌式オートクレーブ中に、テトラデカノールを１４３部、水酸化カリウムを３．０部仕込み、窒素置換を行った後１１０℃に昇温して、４０ＴＯＲＲで１時間脱水を行った。次に１５０℃に昇温し、エチレンオキサイドを３．５ｋｇ/ｃｍ２の圧力で２８８部オートクレーブ中に導入し、圧力が低下して一定になるまで反応させた後、１２０℃に冷却してプロピレンオキサイド５６９部をオートクレーブ中に３．５ｋｇ/ｃｍ２の圧力で導入し、エチレンオキサイドの場合と同様に圧力が低下し一定になるまで反応させた。反応終了後、温度を低下させて合成したサンプルを抜き出し、約１０００部の目的の界面活性剤Ａを得た。
Surfactant A
143 parts of tetradecanol and 3.0 parts of potassium hydroxide were charged into a 5-liter rotary stirring autoclave equipped with two measuring tanks for ethylene oxide and propylene oxide, and after nitrogen substitution, the temperature was changed to 110 ° C. The temperature was raised to 40 torr and dehydration was performed for 1 hour. Next, the temperature is raised to 150 ° C., 288 parts of ethylene oxide is introduced into the autoclave at a pressure of 3.5 kg / cm 2 , reacted until the pressure decreases and becomes constant, and then cooled to 120 ° C. to propylene. 569 parts of oxide was introduced into the autoclave at a pressure of 3.5 kg / cm 2 , and the reaction was continued until the pressure decreased and became constant as in the case of ethylene oxide. After completion of the reaction, the synthesized sample was extracted by lowering the temperature to obtain about 1000 parts of the desired surfactant A.
界面活性剤Ｂ
エチレンオキサイド用とプロピレンオキサイド用の２つ計量槽の付いた５リットルの回転攪拌式オートクレーブ中に、トリデカノールを１５４部、水酸化カリウムを３．０部仕込み、窒素置換を行った後１１０℃に昇温して、４０ＴＯＲＲで１時間脱水を行った。次に１５０℃に昇温し、エチレンオキサイドを３．５ｋｇ/ｃｍ２の圧力で２０８部オートクレーブ中に導入し、圧力が低下して一定になるまで反応させた後、１２０℃に冷却してプロピレンオキサイド６３９部をオートクレーブ中に３．５ｋｇ/ｃｍ２の圧力で導入し、エチレンオキサイドの場合と同様に圧力が低下し一定になるまで反応させた。反応終了後、温度を低下させて合成したサンプルを抜き出し、約１０００部の目的の界面活性剤Ｂを得た。
Surfactant B
154 parts of tridecanol and 3.0 parts of potassium hydroxide were charged into a 5-liter rotary stirring autoclave equipped with two measuring tanks for ethylene oxide and propylene oxide. Warmed and dehydrated at 40 TORR for 1 hour. Next, the temperature was raised to 150 ° C., 208 parts of autoclave was introduced into the autoclave at a pressure of 3.5 kg / cm 2 , and the reaction was continued until the pressure decreased and became constant. 639 parts of oxide was introduced into the autoclave at a pressure of 3.5 kg / cm 2 and reacted until the pressure decreased and became constant in the same manner as in the case of ethylene oxide. After completion of the reaction, the synthesized sample was extracted at a reduced temperature to obtain about 1000 parts of the desired surfactant B.
界面活性剤Ｃ
エチレンオキサイド用とプロピレンオキサイド用の２つ計量槽の付いた５リットルの回転攪拌式オートクレーブ中に、テトラデカノールを３０６部、水酸化カリウムを３．０部仕込み、窒素置換を行った後１１０℃に昇温して、４０ＴＯＲＲで１時間脱水を行った。次に１５０℃に昇温し、エチレンオキサイドを３．５ｋｇ/ｃｍ２の圧力で２３３部オートクレーブ中に導入し、圧力が低下して一定になるまで反応させた後、１２０℃に冷却してプロピレンオキサイド４６１部をオートクレーブ中に３．５ｋｇ/ｃｍ２の圧力で導入し、エチレンオキサイドの場合と同様に圧力が低下し一定になるまで反応させた。反応終了後、温度を低下させて合成したサンプルを抜き出し、約１０００部の目的の界面活性剤Ｃを得た。
Surfactant C
Into a 5 liter rotary stirring autoclave equipped with two measuring tanks for ethylene oxide and propylene oxide, 306 parts of tetradecanol and 3.0 parts of potassium hydroxide were charged, and after nitrogen substitution, 110 ° C. The temperature was raised to 40 torr and dehydration was performed for 1 hour. Next, the temperature was raised to 150 ° C., ethylene oxide was introduced into the 233 parts autoclave at a pressure of 3.5 kg / cm 2 , reacted until the pressure decreased and became constant, and then cooled to 120 ° C. to propylene. 461 parts of oxide were introduced into the autoclave at a pressure of 3.5 kg / cm 2 and reacted until the pressure decreased and became constant in the same manner as in the case of ethylene oxide. After completion of the reaction, the synthesized sample was extracted at a reduced temperature, and about 1000 parts of the desired surfactant C was obtained.
界面活性剤Ｄ
エチレンオキサイド用とプロピレンオキサイド用の２つ計量槽の付いた５リットルの回転攪拌式オートクレーブ中に、ヘプタノールを７７部、水酸化カリウムを３．０部仕込み、窒素置換を行った後１１０℃に昇温して、４０ＴＯＲＲで１時間脱水を行った。次に１５０℃に昇温し、エチレンオキサイドを３．５ｋｇ/ｃｍ２の圧力で３１０部オートクレーブ中に導入し、圧力が低下して一定になるまで反応させた後、１２０℃に冷却してプロピレンオキサイド６１３部をオートクレーブ中に３．５ｋｇ/ｃｍ２の圧力で導入し、エチレンオキサイドの場合と同様に圧力が低下し一定になるまで反応させた。反応終了後、温度を低下させて合成したサンプルを抜き出し、約１０００部の目的の界面活性剤Ｄを得た。
Surfactant D
77 parts of heptanol and 3.0 parts of potassium hydroxide were charged into a 5-liter rotary stirring autoclave equipped with two measuring tanks for ethylene oxide and propylene oxide, and the temperature was raised to 110 ° C. after nitrogen substitution. Warmed and dehydrated at 40 TORR for 1 hour. Next, the temperature was raised to 150 ° C., ethylene oxide was introduced into 310 parts autoclave at a pressure of 3.5 kg / cm 2 , reacted until the pressure decreased and became constant, and then cooled to 120 ° C. to propylene. 613 parts of oxide was introduced into the autoclave at a pressure of 3.5 kg / cm 2 and reacted until the pressure decreased and became constant in the same manner as in the case of ethylene oxide. After completion of the reaction, a sample synthesized at a reduced temperature was extracted to obtain about 1000 parts of the desired surfactant D.
界面活性剤Ｅ
エチレンオキサイド用とプロピレンオキサイド用の２つ計量槽の付いた５リットルの回転攪拌式オートクレーブ中に、テトラデカノールを１４３部、水酸化カリウムを３．０部仕込み、窒素置換を行った後１１０℃に昇温して、４０ＴＯＲＲで１時間脱水を行った。次に１５０℃に昇温し、エチレンオキサイドを３．５ｋｇ/ｃｍ２の圧力で６７部オートクレーブ中に導入し、圧力が低下して一定になるまで反応させた後、１２０℃に冷却してプロピレンオキサイド７９１部をオートクレーブ中に３．５ｋｇ/ｃｍ２の圧力で導入し、エチレンオキサイドの場合と同様に圧力が低下し一定になるまで反応させた。反応終了後、温度を低下させて合成したサンプルを抜き出し、約１０００部の目的の界面活性剤Ｅを得た。
Surfactant E
143 parts of tetradecanol and 3.0 parts of potassium hydroxide were charged into a 5-liter rotary stirring autoclave equipped with two measuring tanks for ethylene oxide and propylene oxide, and after nitrogen substitution, the temperature was changed to 110 ° C. The temperature was raised to 40 torr and dehydration was performed for 1 hour. Next, the temperature is raised to 150 ° C., ethylene oxide is introduced into 67 parts of an autoclave at a pressure of 3.5 kg / cm 2 , reacted until the pressure decreases and becomes constant, and then cooled to 120 ° C. to propylene. 791 parts of oxide were introduced into the autoclave at a pressure of 3.5 kg / cm 2 and reacted until the pressure decreased and became constant in the same manner as in the case of ethylene oxide. After completion of the reaction, the synthesized sample was extracted by lowering the temperature, and about 1000 parts of the desired surfactant E was obtained.
界面活性剤Ｆ
エチレンオキサイド用とプロピレンオキサイド用の２つ計量槽の付いた５リットルの回転攪拌式オートクレーブ中に、テトラデカノールを１４３部、水酸化カリウムを３．０部仕込み、窒素置換を行った後１１０℃に昇温して、４０ＴＯＲＲで１時間脱水を行った。次に１５０℃に昇温し、エチレンオキサイドを３．５ｋｇ/ｃｍ２の圧力で６４５部オートクレーブ中に導入し、圧力が低下して一定になるまで反応させた後、１２０℃に冷却してプロピレンオキサイド２１３部をオートクレーブ中に３．５ｋｇ/ｃｍ２の圧力で導入し、エチレンオキサイドの場合と同様に圧力が低下し一定になるまで反応させた。反応終了後、温度を低下させて合成したサンプルを抜き出し、約１０００部の目的の界面活性剤Ｆを得た。
得られた界面活性剤ＡからＦの詳細を表１に示す。
Surfactant F
143 parts of tetradecanol and 3.0 parts of potassium hydroxide were charged into a 5-liter rotary stirring autoclave equipped with two measuring tanks for ethylene oxide and propylene oxide, and after nitrogen substitution, the temperature was changed to 110 ° C. The temperature was raised to 40 torr and dehydration was performed for 1 hour. Next, the temperature was raised to 150 ° C., ethylene oxide was introduced into the 645 parts autoclave at a pressure of 3.5 kg / cm 2 , reacted until the pressure decreased and became constant, and then cooled to 120 ° C. to propylene. 213 parts of oxide was introduced into the autoclave at a pressure of 3.5 kg / cm 2 , and the reaction was continued until the pressure decreased and became constant as in the case of ethylene oxide. After completion of the reaction, the synthesized sample was extracted by lowering the temperature, and about 1000 parts of the desired surfactant F was obtained.
Details of the obtained surfactants A to F are shown in Table 1.
［実施例１］
溶融ポリエチレンテレフタレート（［η］＝０．６３ｄｌ／ｇ、Ｔｇ＝７８℃）をダイより押出し、常法により冷却ドラムで冷却して未延伸フィルムとし、次いでその両面に表１に示す塗剤組成１の濃度１０重量％の水性塗液をロールコーターで均一に塗布して塗布フィルムを得た。この水性塗液における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー１００重量部に対して界面活性剤５重量部であり、塗布フィルムを、引き続いて９５℃で乾燥し、１２０℃で縦方向に３．３倍、横方向に３．７倍の延伸倍率で縦横方向を同時に延伸し、２４０℃で熱固定し、厚さ１００μｍの光学用フィルムを得た。この光学用フィルムの易接着層における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー１００重量部に対して界面活性剤４重量部であり、易接着層における界面活性剤の含有率は易接着層の重量を基準に４重量％である。評価結果を表２に示す。
[Example 1]
Molten polyethylene terephthalate ([η] = 0.63 dl / g, Tg = 78 ° C.) is extruded from a die, cooled with a cooling drum by a conventional method to form an unstretched film, and then a coating composition 1 shown in Table 1 on both sides thereof An aqueous coating solution having a concentration of 10% by weight was uniformly applied by a roll coater to obtain a coated film. The ratio of the content of the polymer binder and the surfactant in this aqueous coating liquid is 5 parts by weight of the surfactant with respect to 100 parts by weight of the polymer binder, and the coated film is subsequently dried at 95 ° C. The film was stretched at the same time in the longitudinal and transverse directions at a stretching ratio of 3.3 times in the longitudinal direction and 3.7 times in the transverse direction, and heat-set at 240 ° C. to obtain an optical film having a thickness of 100 μm. The ratio of the content of the polymer binder and the surfactant in the easy-adhesion layer of the optical film is 4 parts by weight of the surfactant with respect to 100 parts by weight of the polymer binder. The rate is 4% by weight based on the weight of the easily adhesive layer. The evaluation results are shown in Table 2.
［実施例２］
水性塗液を表２に示す塗剤組成２の濃度１０重量％の水性塗液に変更すること以外は実施例１と同様にして厚さ１００μｍの光学用フィルムを得た。この光学用フィルムの易接着層における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー１００重量部に対して界面活性剤４重量部であり、易接着層における界面活性剤の含有率は易接着層の重量を基準に４重量％である。評価結果を表２に示す。
[Example 2]
An optical film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the aqueous coating liquid was changed to an aqueous coating liquid having a concentration of 10% by weight of the coating composition 2 shown in Table 2. The ratio of the content of the polymer binder and the surfactant in the easy-adhesion layer of the optical film is 4 parts by weight of the surfactant with respect to 100 parts by weight of the polymer binder. The rate is 4% by weight based on the weight of the easily adhesive layer. The evaluation results are shown in Table 2.
［比較例１］
水性塗液を表２に示す塗剤組成３の濃度１０重量％の水性塗液に変更すること以外は実施例１と同様にして厚さ１００μｍの光学用フィルムを得た。この光学用フィルムの易接着層における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー１００重量部に対して界面活性剤０．４重量部である。評価結果を表２に示す。
[Comparative Example 1]
An optical film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the aqueous coating liquid was changed to an aqueous coating liquid having a concentration of 10% by weight of the coating composition 3 shown in Table 2. The ratio of the content of the polymer binder and the surfactant in the easy-adhesion layer of this optical film is 0.4 parts by weight of the surfactant with respect to 100 parts by weight of the polymer binder. The evaluation results are shown in Table 2.
［比較例２］
水性塗液を表２に示す塗剤組成４の濃度１０重量％の水性塗液に変更すること以外は実施例１と同様にして厚さ１００μｍの光学用フィルムを得た。この光学用フィルムの易接着層における高分子バインダーと界面活性剤の含有量の比は、高分子バインダー１００重量部に対して界面活性剤２０重量部である。評価結果を表２に示す。
[Comparative Example 2]
An optical film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the aqueous coating liquid was changed to an aqueous coating liquid having a concentration of 10% by weight of the coating composition 4 shown in Table 2. The ratio of the content of the polymer binder and the surfactant in the easy-adhesion layer of the optical film is 20 parts by weight of the surfactant with respect to 100 parts by weight of the polymer binder. The evaluation results are shown in Table 2.
［比較例３］
水性塗液を表２に示す塗剤組成５の濃度１０重量％の水性塗液に変更すること以外は実施例１と同様にして厚さ１００μｍの光学用フィルムを得た。評価結果を表２に示す。
[Comparative Example 3]
An optical film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the aqueous coating liquid was changed to an aqueous coating liquid having a concentration of 10% by weight of the coating composition 5 shown in Table 2. The evaluation results are shown in Table 2.
［比較例４］
水性塗液を表２に示す塗剤組成６の濃度１０重量％の水性塗液に変更すること以外は実施例１と同様にして厚さ１００μｍの光学用フィルムを得た。評価結果を表２に示す。
[Comparative Example 4]
An optical film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the aqueous coating liquid was changed to an aqueous coating liquid having a concentration of 10% by weight of the coating composition 6 shown in Table 2. The evaluation results are shown in Table 2.
［比較例５］
水性塗液を表２に示す塗剤組成７の濃度１０重量％の水性塗液に変更すること以外は実施例１と同様にして厚さ１００μｍの光学用フィルムを得た。評価結果を表２に示す。
[Comparative Example 5]
An optical film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the aqueous coating liquid was changed to an aqueous coating liquid having a concentration of 10% by weight of the coating composition 7 shown in Table 2. The evaluation results are shown in Table 2.
［比較例６］
水性塗液を表２に示す塗剤組成８の濃度１０重量％の水性塗液に変更すること以外は実施例１と同様にして厚さ１００μｍの光学用フィルムを得た。評価結果を表２に示す。
[Comparative Example 6]
An optical film having a thickness of 100 μm was obtained in the same manner as in Example 1 except that the aqueous coating liquid was changed to an aqueous coating liquid having a concentration of 10% by weight of the coating composition 8 shown in Table 2. The evaluation results are shown in Table 2.
なお、表２の塗液組成の成分は次のとおりである。「部」は重量部を意味する。 In addition, the component of the coating liquid composition of Table 2 is as follows. “Parts” means parts by weight.
水分散性ポリエステル組成物１
水分散性ポリエステル組成物１は、水分散性ポリエステル１と界面活性剤Ａとの混合物である。
水分散性ポリエステル１は、ジカルボン酸成分が２，６−ナフタレンジカルボン酸７５モル％／イソフタル酸２０モル％／５−ナトリウムスルホイソフタル酸５モル％、グリコール成分がエチレングリコール９０モル％／ジエチレングリコール１０モル％で構成されている（Ｔｇ＝８０℃、平均分子量１５０００）。なお、この水分散性ポリエステル１は、下記の方法で製造した。すなわち、２，６−ナフタレンジカルボン酸ジメチル５１部、イソフタル酸ジメチル１１部、５−ナトリウムスルホイソフタル酸ジメチル４部、エチレングリコール３１部、ジエチレングリコール２部を反応器に仕込み、これにテトラブトキシチタン０．０５部を添加して窒素雰囲気下で温度を２３０℃にコントロールして加熱し、生成するメタノールを留去させてエステル交換反応を行った。次いで攪拌器のモータートルクの高い重合釜で反応系の温度を徐々に２５５℃まで上昇させ系内を１ｍｍＨｇの減圧にして重縮合反応を行い、固有粘度が０．５６の水分散性ポリエステル１を得た。この水分散性ポリエステル１の２５部をテトラヒドロフラン７５部に溶解させ、得られた溶液に界面活性剤Ａを１部添加し、１００００回転／分の高速攪拌下で水７５部を滴下して乳白色の分散体を得、次いでこの分散体を２０ｍｍＨｇの減圧下で蒸留し、テトラヒドロフランを留去した。
Water dispersible polyester composition 1
The water dispersible polyester composition 1 is a mixture of the water dispersible polyester 1 and the surfactant A.
The water dispersible polyester 1 has a dicarboxylic acid component of 75 mol% of 2,6-naphthalenedicarboxylic acid / 20 mol% of isophthalic acid / 5 mol% of 5-sodium sulfoisophthalic acid, and a glycol component of 90 mol% of ethylene glycol / 10 mol of diethylene glycol. % (Tg = 80 ° C., average molecular weight 15000). The water dispersible polyester 1 was produced by the following method. That is, 51 parts of dimethyl 2,6-naphthalenedicarboxylate, 11 parts of dimethyl isophthalate, 4 parts of dimethyl 5-sodium sulfoisophthalate, 31 parts of ethylene glycol and 2 parts of diethylene glycol were charged into a reactor. 05 parts were added, the temperature was controlled at 230 ° C. in a nitrogen atmosphere, and the resulting methanol was distilled off to conduct a transesterification reaction. Next, the temperature of the reaction system is gradually raised to 255 ° C. in a polymerization kettle with high motor torque of a stirrer, and the inside of the system is reduced to 1 mmHg to carry out a polycondensation reaction, and water dispersible polyester 1 having an intrinsic viscosity of 0.56 is obtained. Obtained. 25 parts of this water-dispersible polyester 1 was dissolved in 75 parts of tetrahydrofuran, 1 part of surfactant A was added to the resulting solution, and 75 parts of water was added dropwise under high-speed stirring at 10,000 rpm to give a milky white color. A dispersion was obtained, and then the dispersion was distilled under a reduced pressure of 20 mmHg to distill off the tetrahydrofuran.
水分散性ポリエステル組成物２
水分散性ポリエステル組成物２は、水分散性ポリエステル２と界面活性剤Ｂとの混合物である。
水分散性ポリエステル２は、ジカルボン酸成分がテレフタルジカルボン酸９７モル％／イソフタル酸１モル％／５−ナトリウムスルホイソフタル酸２モル％、グリコール成分がエチレングリコール９０モル％／ジエチレングリコール１０モル％で構成されている（Ｔｇ＝８０℃、平均分子量１５０００）。なお、この水分散性ポリエステル２は、下記の方法で製造した。すなわち、テレフタル酸ジメチル６２部、イソフタル酸ジメチル１部、５−ナトリウムスルホイソフタル酸ジメチル４部、エチレングリコール３１部、ジエチレングリコール２部を反応器に仕込み、これにテトラブトキシチタン０．０５部を添加して窒素雰囲気下で温度を２３０℃にコントロールして加熱し、生成するメタノールを留去させてエステル交換反応を行った。次いで攪拌器のモータートルクの高い重合釜で反応系の温度を徐々に２５５℃まで上昇させ系内を１ｍｍＨｇの減圧にして重縮合反応を行い、固有粘度が０．５６の水分散性ポリエステル２を得た。この水分散性ポリエステル２の２５部をテトラヒドロフラン７５部に溶解させ、得られた溶液に界面活性剤Ｂを１部添加し、１００００回転／分の高速攪拌下で水７５部を滴下して乳白色の分散体を得、次いでこの分散体を２０ｍｍＨｇの減圧下で蒸留し、テトラヒドロフランを留去した。
Water dispersible polyester composition 2
The water dispersible polyester composition 2 is a mixture of the water dispersible polyester 2 and the surfactant B.
In the water dispersible polyester 2, the dicarboxylic acid component is composed of 97 mol% terephthaldicarboxylic acid / 1 mol% isophthalic acid / 5 mol% 5-sodium sulfoisophthalic acid, and the glycol component is composed of 90 mol% ethylene glycol / 10 mol% diethylene glycol. (Tg = 80 ° C., average molecular weight 15000). This water-dispersible polyester 2 was produced by the following method. That is, 62 parts of dimethyl terephthalate, 1 part of dimethyl isophthalate, 4 parts of dimethyl 5-sodium sulfoisophthalate, 31 parts of ethylene glycol and 2 parts of diethylene glycol were charged into the reactor, and 0.05 part of tetrabutoxy titanium was added thereto. Then, the temperature was controlled at 230 ° C. in a nitrogen atmosphere, and the produced methanol was distilled off to conduct a transesterification reaction. Next, the temperature of the reaction system is gradually raised to 255 ° C. in a polymerization kettle with high motor torque of the stirrer, and the inside of the system is depressurized to 1 mmHg to carry out a polycondensation reaction. Obtained. 25 parts of this water-dispersible polyester 2 was dissolved in 75 parts of tetrahydrofuran, 1 part of surfactant B was added to the resulting solution, and 75 parts of water was added dropwise under high-speed stirring at 10,000 rpm to give a milky white color. A dispersion was obtained, and then the dispersion was distilled under a reduced pressure of 20 mmHg to distill off the tetrahydrofuran.
水分散性ポリエステル組成物３
水分散性ポリエステル組成物３は、水分散性ポリエステル１と界面活性剤Ａとの混合物である。界面活性剤Ａの添加量を０．１部に変更する以外は水分散性ポリエステル組成物１と同様にして、水分散性ポリエステル組成物３を得た。
Water dispersible polyester composition 3
The water dispersible polyester composition 3 is a mixture of the water dispersible polyester 1 and the surfactant A. A water-dispersible polyester composition 3 was obtained in the same manner as the water-dispersible polyester composition 1 except that the addition amount of the surfactant A was changed to 0.1 part.
水分散性ポリエステル組成物４
水分散性ポリエステル組成物４は、水分散性ポリエステル１と界面活性剤Ａとの混合物である。界面活性剤Ａの添加量を５部に変更する以外は水分散性ポリエステル組成物１と同様にして、水分散性ポリエステル組成物４を得た。
Water dispersible polyester composition 4
The water dispersible polyester composition 4 is a mixture of the water dispersible polyester 1 and the surfactant A. A water-dispersible polyester composition 4 was obtained in the same manner as the water-dispersible polyester composition 1 except that the addition amount of the surfactant A was changed to 5 parts.
水分散性ポリエステル組成物５
水分散性ポリエステル組成物５は、水分散性ポリエステル１と界面活性剤Ｃとの混合物である。界面活性剤Ａの代わりに界面活性剤Ｃを用いた以外は水分散性ポリエステル組成物１と同様にして、水分散性ポリエステル組成物５を得た。
Water dispersible polyester composition 5
The water dispersible polyester composition 5 is a mixture of the water dispersible polyester 1 and the surfactant C. A water-dispersible polyester composition 5 was obtained in the same manner as the water-dispersible polyester composition 1 except that the surfactant C was used instead of the surfactant A.
水分散性ポリエステル組成物６
水分散性ポリエステル組成物５は、水分散性ポリエステル１と界面活性剤Ｄとの混合物である。界面活性剤Ａの代わりに界面活性剤Ｄを用いた以外は水分散性ポリエステル組成物１と同様にして、水分散性ポリエステル組成物６を得た。
Water dispersible polyester composition 6
The water dispersible polyester composition 5 is a mixture of the water dispersible polyester 1 and the surfactant D. A water-dispersible polyester composition 6 was obtained in the same manner as the water-dispersible polyester composition 1 except that the surfactant D was used instead of the surfactant A.
水分散性ポリエステル組成物７
水分散性ポリエステル組成物５は、水分散性ポリエステル１と界面活性剤Ｅとの混合物である。界面活性剤Ａの代わりに界面活性剤Ｅを用いた以外は水分散性ポリエステル組成物１と同様にして、水分散性ポリエステル組成物７を得た。
Water dispersible polyester composition 7
The water dispersible polyester composition 5 is a mixture of the water dispersible polyester 1 and the surfactant E. A water-dispersible polyester composition 7 was obtained in the same manner as the water-dispersible polyester composition 1 except that the surfactant E was used instead of the surfactant A.
水分散性ポリエステル組成物８
水分散性ポリエステル組成物８は、水分散性ポリエステル１と界面活性剤Ｆとの混合物である。界面活性剤Ａの代わりに界面活性剤Ｆを用いた以外は水分散性ポリエステル組成物１と同様にして、水分散性ポリエステル組成物８を得た。
Water dispersible polyester composition 8
The water dispersible polyester composition 8 is a mixture of the water dispersible polyester 1 and the surfactant F. A water-dispersible polyester composition 8 was obtained in the same manner as the water-dispersible polyester composition 1 except that the surfactant F was used instead of the surfactant A.
架橋剤
メチルメタクリレート１０モル％／２−イソプロペニル−２−オキサゾリン７０モル％／ポリエチレンオキシド（ｎ＝１０）メタクリレート５モル％／アクリルアミド１５モル％で構成されている（Ｔｇ＝１００℃）。なお、架橋剤は、特開昭６３−３７１６７号公報の製造例１〜３に記載の方法に準じて下記の通り製造した。すなわち、四つ口フラスコに、イオン交換水３０２部を仕込んで窒素気流中で６０℃まで昇温させ、次いで重合開始剤として過硫酸アンモニウム０．５部、亜硫酸水素ナトリウム０．２部を添加し、メタクリル酸メチル７．８部、２−イソプロペニル−２−オキサゾリン５２．８部、ポリエチレンオキシド（ｎ＝１０）メタクリル酸２０．４部、アクリルアミド６．６部の混合物を３時間にわたり、液温が６０〜７０℃になるよう調整しながら滴下した。滴下終了後も同温度範囲に２時間保持しつつ、撹拌下に反応を継続させ、次いで冷却して固形分が２５％の架橋剤の水分散体を得た。
The crosslinking agent is composed of 10 mol% of methyl methacrylate / 2 mol of 2-isopropenyl-2-oxazoline / 5 mol% of polyethylene oxide (n = 10) methacrylate / 15 mol% of acrylamide (Tg = 100 ° C.). The crosslinking agent was produced as follows according to the method described in Production Examples 1 to 3 of JP-A No. 63-37167. That is, 302 parts of ion-exchanged water was charged into a four-necked flask and the temperature was raised to 60 ° C. in a nitrogen stream, then 0.5 parts of ammonium persulfate and 0.2 parts of sodium bisulfite were added as a polymerization initiator, A mixture of methyl methacrylate (7.8 parts), 2-isopropenyl-2-oxazoline (52.8 parts), polyethylene oxide (n = 10) methacrylic acid (20.4 parts) and acrylamide (6.6 parts) was stirred for 3 hours. The solution was added dropwise while adjusting to 60 to 70 ° C. After the completion of dropping, the reaction was continued under stirring while maintaining the same temperature range for 2 hours, and then cooled to obtain an aqueous dispersion of a crosslinking agent having a solid content of 25%.
添加剤
帯電防止剤（複合資材株式会社製 商品名エレカットＬ）
Additives Antistatic agent (trade name ELECUT L manufactured by Composite Materials Co., Ltd.)
本発明の光学用フィルムは、タッチパネルの基材フィルムとして好適に用いることができる。また、液晶表示面に貼付ける表面保護フィルムとして好適に用いることができる。
本発明の光学用フィルムは、少なくとも片面にハードコート層を設ける加工を施したあと、透明導電層や粘着層を設ける加工を施し製品サイズに裁断することで、タッチパネルの基材フィルムや表面保護フィルム等の光学部材に加工することができる。
The optical film of the present invention can be suitably used as a base film for a touch panel. Moreover, it can use suitably as a surface protection film stuck on a liquid crystal display surface.
The optical film of the present invention has a process of providing a hard coat layer on at least one side, and then a process of providing a transparent conductive layer or an adhesive layer and cutting it into a product size. It can process into optical members, such as.
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Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2010000063A JP5357064B2 (en) | 2010-01-04 | 2010-01-04 | Optical film |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2010000063A JP5357064B2 (en) | 2010-01-04 | 2010-01-04 | Optical film |
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| Publication Number | Publication Date |
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| JP2011136539A JP2011136539A (en) | 2011-07-14 |
| JP5357064B2 true JP5357064B2 (en) | 2013-12-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| JP2010000063A Expired - Fee Related JP5357064B2 (en) | 2010-01-04 | 2010-01-04 | Optical film |
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| US11551584B2 (en) | 2019-10-28 | 2023-01-10 | Skc Co., Ltd. | Polyester film and flexible display apparatus comprising same |
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| JPH0227393B2 (en) * | 1981-12-04 | 1990-06-15 | Nippon Oils & Fats Co Ltd | MIZUKEIJUNKATSUYUSOSEIBUTSU |
| JP5084143B2 (en) * | 2005-02-14 | 2012-11-28 | 株式会社Ａｄｅｋａ | Light stabilizer emulsion composition |
| JP2008183760A (en) * | 2007-01-29 | 2008-08-14 | Teijin Dupont Films Japan Ltd | Easily adhesive polyester film for optics |
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| JP2011136539A (en) | 2011-07-14 |
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