JP2013067764A - 光学フィルム用粘着剤層の製造方法、光学フィルム用粘着剤層、粘着型光学フィルムおよび画像表示装置 - Google Patents
光学フィルム用粘着剤層の製造方法、光学フィルム用粘着剤層、粘着型光学フィルムおよび画像表示装置 Download PDFInfo
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- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
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- 125000005670 ethenylalkyl group Chemical group 0.000 description 1
- DECIPOUIJURFOJ-UHFFFAOYSA-N ethoxyquin Chemical compound N1C(C)(C)C=C(C)C2=CC(OCC)=CC=C21 DECIPOUIJURFOJ-UHFFFAOYSA-N 0.000 description 1
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- IPZIVCLZBFDXTA-UHFFFAOYSA-N ethyl n-prop-2-enoylcarbamate Chemical compound CCOC(=O)NC(=O)C=C IPZIVCLZBFDXTA-UHFFFAOYSA-N 0.000 description 1
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- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
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- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 1
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- 150000002513 isocyanates Chemical class 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000003475 lamination Methods 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
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- RBQRWNWVPQDTJJ-UHFFFAOYSA-N methacryloyloxyethyl isocyanate Chemical compound CC(=C)C(=O)OCCN=C=O RBQRWNWVPQDTJJ-UHFFFAOYSA-N 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- RZRNAYUHWVFMIP-UHFFFAOYSA-N monoelaidin Natural products CCCCCCCCC=CCCCCCCCC(=O)OCC(O)CO RZRNAYUHWVFMIP-UHFFFAOYSA-N 0.000 description 1
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 description 1
- ZQXSMRAEXCEDJD-UHFFFAOYSA-N n-ethenylformamide Chemical class C=CNC=O ZQXSMRAEXCEDJD-UHFFFAOYSA-N 0.000 description 1
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- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
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- 125000004433 nitrogen atom Chemical group N* 0.000 description 1
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- JFNLZVQOOSMTJK-KNVOCYPGSA-N norbornene Chemical compound C1[C@@H]2CC[C@H]1C=C2 JFNLZVQOOSMTJK-KNVOCYPGSA-N 0.000 description 1
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- ANISOHQJBAQUQP-UHFFFAOYSA-N octyl prop-2-enoate Chemical compound CCCCCCCCOC(=O)C=C ANISOHQJBAQUQP-UHFFFAOYSA-N 0.000 description 1
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- OVEJEPOXQQLXEI-UHFFFAOYSA-N pent-4-enyl(tripropoxy)silane Chemical compound CCCO[Si](OCCC)(OCCC)CCCC=C OVEJEPOXQQLXEI-UHFFFAOYSA-N 0.000 description 1
- WDQCVPOQABDJJO-UHFFFAOYSA-N pent-4-enyl-tri(propan-2-yloxy)silane Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)CCCC=C WDQCVPOQABDJJO-UHFFFAOYSA-N 0.000 description 1
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- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
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- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
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- 229920006254 polymer film Polymers 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920000306 polymethylpentene Polymers 0.000 description 1
- 239000011116 polymethylpentene Substances 0.000 description 1
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 description 1
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 1
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 229920006264 polyurethane film Polymers 0.000 description 1
- 229920002717 polyvinylpyridine Polymers 0.000 description 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- AAYRWMCIKCRHIN-UHFFFAOYSA-N propane-1-sulfonic acid;prop-2-enamide Chemical compound NC(=O)C=C.CCCS(O)(=O)=O AAYRWMCIKCRHIN-UHFFFAOYSA-N 0.000 description 1
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012966 redox initiator Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000001846 repelling effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- 229940001584 sodium metabisulfite Drugs 0.000 description 1
- 235000010262 sodium metabisulphite Nutrition 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- OGRPJZFGZFQRHZ-UHFFFAOYSA-M sodium;4-octoxy-4-oxo-3-sulfobutanoate Chemical compound [Na+].CCCCCCCCOC(=O)C(S(O)(=O)=O)CC([O-])=O OGRPJZFGZFQRHZ-UHFFFAOYSA-M 0.000 description 1
- HIEHAIZHJZLEPQ-UHFFFAOYSA-M sodium;naphthalene-1-sulfonate Chemical compound [Na+].C1=CC=C2C(S(=O)(=O)[O-])=CC=CC2=C1 HIEHAIZHJZLEPQ-UHFFFAOYSA-M 0.000 description 1
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- 235000019337 sorbitan trioleate Nutrition 0.000 description 1
- 229960000391 sorbitan trioleate Drugs 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- SGCFZHOZKKQIBU-UHFFFAOYSA-N tributoxy(ethenyl)silane Chemical compound CCCCO[Si](OCCCC)(OCCCC)C=C SGCFZHOZKKQIBU-UHFFFAOYSA-N 0.000 description 1
- AYYIWCRQXLDMJG-UHFFFAOYSA-N tributoxy(pent-4-enyl)silane Chemical compound CCCCO[Si](CCCC=C)(OCCCC)OCCCC AYYIWCRQXLDMJG-UHFFFAOYSA-N 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- UMFJXASDGBJDEB-UHFFFAOYSA-N triethoxy(prop-2-enyl)silane Chemical compound CCO[Si](CC=C)(OCC)OCC UMFJXASDGBJDEB-UHFFFAOYSA-N 0.000 description 1
- WDUXKFKVDQRWJN-UHFFFAOYSA-N triethoxysilylmethyl prop-2-enoate Chemical compound CCO[Si](OCC)(OCC)COC(=O)C=C WDUXKFKVDQRWJN-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- SYYDEXILBJXXIA-UHFFFAOYSA-N trimethoxy(pent-4-enyl)silane Chemical compound CO[Si](OC)(OC)CCCC=C SYYDEXILBJXXIA-UHFFFAOYSA-N 0.000 description 1
- LFRDHGNFBLIJIY-UHFFFAOYSA-N trimethoxy(prop-2-enyl)silane Chemical compound CO[Si](OC)(OC)CC=C LFRDHGNFBLIJIY-UHFFFAOYSA-N 0.000 description 1
- JPPHEZSCZWYTOP-UHFFFAOYSA-N trimethoxysilylmethyl prop-2-enoate Chemical compound CO[Si](OC)(OC)COC(=O)C=C JPPHEZSCZWYTOP-UHFFFAOYSA-N 0.000 description 1
- 125000006617 triphenylamine group Chemical group 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 239000004034 viscosity adjusting agent Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 229960001763 zinc sulfate Drugs 0.000 description 1
- 229910000368 zinc sulfate Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/08—Homopolymers or copolymers of acrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/312—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier parameters being the characterizing feature
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/14—Layer or component removable to expose adhesive
- Y10T428/1476—Release layer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Devices For Indicating Variable Information By Combining Individual Elements (AREA)
- Polarising Elements (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
- Laminated Bodies (AREA)
Abstract
【解決手段】水分散型の(メタ)アクリル系重合体を含有する水分散液を含有する水分散型粘着剤を離型フィルムに塗工する工程(1)および塗工された水分散型粘着剤を乾燥する工程(2)を有する光学フィルム用粘着剤層の製造方法であって、前記水分散型粘着剤は、せん断速度4000(1/s)における粘度が0.01〜0.1Pa・sであり、前記離型フィルム上に形成される前記光学フィルム用粘着剤層の表面の表面粗さ(Ra)が10〜40nmであり、かつ、前記光学フィルム用粘着剤層のヘイズが1%以下である。
【選択図】なし
Description
前記水分散型粘着剤は、せん断速度4000(1/s)における粘度が0.01〜0.1Pa・sであり、
前記離型フィルム上に形成される前記光学フィルム用粘着剤層の表面の表面粗さ(Ra)が10〜40nmであり、かつ、
前記光学フィルム用粘着剤層の厚さが23μmの場合のヘイズが1%以下であることを特徴とする光学フィルム用粘着剤層の製造方法、に関する。
(一般式(1)中、R1は、水素原子またはメチル基を示し、R2は炭素数1〜4のアルキレン基、mは2以上の整数を示し、M1およびM2は、それぞれ独立に、水素原子またはカチオンを示す。)で表されるリン酸基またはその塩を示す。)で表されるリン酸基含有モノマーが挙げられる。
水分散型粘着剤の粘度(Pa・s)は、HAAKE社製Rheowinを用いて次の条件で測定した。
コーン:直径35mm
測定温度:30℃
せん断条件:0.1〜14000(1/s)を20秒間かけて測定。得られたデータから近似値を算出し、せん断速度(1/s)=4000の値を粘度として示した。
(メタ)アクリル系重合体の体積平均粒子径は、調製した水分散型の(メタ)アクリル系重合体を含有する水分散液を、蒸留水により固形分濃度が約1重量%となるように希釈したものを用いて下記装置にて測定した。
装置:ベックマンコールター製のLS13 320 PIDSモード
分散質の屈折率:1.48 ポリn−ブチルアクリレートを使用
分散媒の屈折率:1.333
(モノマーエマルションを調製)
容器に、原料モノマーとして、アクリル酸ブチル880部、アクリル酸50部、メタクリル酸シクロへキシル50部、モノ[ポリ(プロピレンオキシド)メタクリレート]リン酸エステル(プロピレンオキシドの平均重合度約5.0)20部、および3−メタクリロイルオキシプロピル−トリエトキシシラン(信越化学工業(株)製,KBM−503)0.3部を加えて混合し、モノマー成分を調製した。次いで、調製したモノマー成分400部に、反応性乳化剤であるアクアロンHS−10(第一工業製薬(株)製)4部、イオン交換水268部を加え、ホモミキサーを用い、5分間、6000rpmで攪拌し、強制乳化してモノマーエマルションを調製した。
次に、冷却管、窒素導入管、温度計、滴下ロートおよび攪拌羽根を備えた反応容器に、上記で調製したモノマーエマルションのなかの136部、反応性乳化剤であるアクアロンHS−10(第一工業製薬(株)製)8部およびイオン交換水308部を仕込み、次いで、反応容器を十分窒素置換した後、過硫酸アンモニウム0.1部を添加して、65℃で1時間重合した。次いで、過硫酸アンモニウム0.3部を加え、残りのモノマーエマルション536部を、反応容器に3時間かけて滴下し、その後、3時間重合した。さらにその後、窒素置換しながら、75℃で3時間重合し、固形分濃度40%の水分散型の(メタ)アクリル系重合体を含有する水分散液(エマルション)を得た。次いで、上記水分散液を室温まで冷却した後、これに、濃度10%のアンモニア水を添加してpHを8に調整して、水分散型アクリル系粘着剤を得た(固形分濃度38%)。当該水分散型アクリル系粘着剤の粘度は0.066Pa・s、体積平均粒子径は88nmであった。
上記水分散型アクリル系粘着剤を、乾燥後の厚みが23μmとなるように、離型フィルム(三菱化学ポリエステル(株)製,ダイアホイルMRF−38,ポリエチレンテレフタレート基材)上に、リップコーターにより、塗工速度20m/minで塗工した後、熱風循環式オーブン(風速10m/s)により乾燥温度100℃で1分間の第一乾燥工程と、熱風循環式オーブン(風速20m/s)により乾燥温度130℃で1分間の第二乾燥工程を施して、粘着剤層を形成した。当該粘着剤層を偏光板(日東電工(株)製,製品名VEGQ)と貼り合せて、2種類の粘着型偏光板を作成した。
実施例1の(粘着剤層の形成および粘着型偏光板の作成)において、塗工速度を50m/minに変えたこと以外は、実施例1と同様にして粘着剤層を形成した。また、実施例1と同様にして、粘着型偏光板を作成した。
実施例1の(粘着剤層の形成および粘着型偏光板の作成)において、第一乾燥工程の乾燥温度を80℃に変えたこと以外は、実施例1と同様にして粘着剤層を形成した。また、実施例1と同様にして、粘着型偏光板を作成した。
実施例1の(粘着剤層の形成および粘着型偏光板の作成)において、第一乾燥工程の乾燥温度を60℃に変えたこと、塗工速度を25m/minに変えたこと以外は、実施例1と同様にして粘着剤層を形成した。また、実施例1と同様にして、粘着型偏光板を作成した。
実施例1の(水分散型アクリル系粘着剤の調製)において、濃度10%のアンモニア水を添加してpHを7に調整したこと以外は、実施例1と同様にして、水分散型アクリル系粘着剤を得た(固形分濃度38%)。当該水分散型アクリル系粘着剤の粘度は0.044Pa・s、体積平均粒子径は86nmであった。また、当該水分散型アクリル系粘着剤を用いたこと以外は、実施例1と同様にして粘着剤層を形成した。また、実施例1と同様にして、粘着型偏光板を作成した。
実施例1の(モノマーエマルションを調製)において、アクリル酸の配合部数を50部から10部に変えたこと、実施例1の(水分散型アクリル系粘着剤の調製)において、得られる水分散型アクリル系粘着剤の固形分濃度が50%になるように調整したこと以外は、実施例1と同様にして、水分散型アクリル系粘着剤を得た。当該水分散型アクリル系粘着剤の粘度は0.070Pa・s、体積平均粒子径は130nmであった。また、当該水分散型アクリル系粘着剤を用いたこと以外は、実施例1と同様にして粘着剤層を形成した。また、実施例1と同様にして、粘着型偏光板を作成した。
実施例1の(水分散型アクリル系粘着剤の調製)において、濃度10%のアンモニア水を添加してpHを6.8に調整したこと以外は、実施例1と同様にして、水分散型アクリル系粘着剤を得た(固形分濃度38%)。当該水分散型アクリル系粘着剤の粘度は0.020Pa・s、体積平均粒子径は88nmであった。また、当該水分散型アクリル系粘着剤を用いたこと以外は、実施例1と同様にして粘着剤層を形成した。また、実施例1と同様にして、粘着型偏光板を作成した。
(モノマーエマルションを調製)
容器に、原料モノマーとして、アクリル酸−2−エチルヘキシル80部、メタクリル酸メチル20部、ドデシルメルカプタン0.1部、N−メチロールアクリルアミド0.1部およびアクリル酸2部、ポリオキシエチレンアルキルフェニルエーテル硫酸ナトリウム(花王(株)製の商品名レベノールWZ)1.5部および水27部を加えてモノマーエマルションを調製した。
次に、還流冷却器、温度計および撹拌器を備えた反応器に水33部を仕込み、反応器内を窒素乾燥した後、80℃に昇温し、過硫酸アンモニウム0.5部を加え、次いで前記モノマーエマルションの全量の0.2重量%を加え、重合を開始した。重合の開始確認後、79〜81℃でモノマーエマルションの残部(全量の99.8重量%)を連続的に4時間で滴下した。モノマーエマルションの連続滴下終了後、10重量%の過硫酸アンモニウム水溶液1.0部を加え、さらに80℃に2時間保ち反応を終了した。上記により得たアクリル系共重合体のエマルションを25重量%のアンモニア水で中和し、アクリル系増粘剤(東亜合成(株)製のB−300)を添加することにより水分散型アクリル系粘着剤組成物を得た。当該水分散型アクリル系粘着剤組成物の粘度は0.150Pa・s、体積平均粒子径は1020nmであった。
実施例1において、水分散型アクリル系粘着剤として、上記で得られた水分散型アクリル系粘着剤を用いたこと以外は、実施例1と同様にして粘着剤層を形成した。また、実施例1と同様にして、粘着型偏光板を作成した。
(溶剤型アクリル系粘着剤の調製)
冷却管、窒素導入管、温度計および攪拌機を備えた反応容器に、アクリル酸ブチル96.5部、アクリル酸3部、2−ヒドロキシエチルアクリレート0.5部、2,2´−アゾビスイソブチロニトリル0.15部および酢酸エチル100部を仕込み、十分窒素置換した後、窒素気流下で撹拌しながら、60℃で8時間反応して重量平均分子量165万のアクリル系重合体溶液を得た。上記アクリル系重合体溶液の固形分100部に対して、イソシアネート系架橋剤(日本ポリウレタン工業(株)製,コロネートL)0.5部を配合して、固形分12%の溶剤型アクリル系粘着剤を得た。当該溶剤型アクリル系粘着剤の粘度は0.21Pa・sであった。
実施例1において、水分散型アクリル系粘着剤の代わりに、上記溶剤型アクリル系粘着剤を用いたこと以外は、実施例1と同様にして粘着剤層を形成した。また、実施例1と同様にして、粘着型偏光板を作成した。
比較例2の(粘着剤層の形成および粘着型偏光板の作成)において、塗工速度を10m/minに変えたこと以外は、比較例2と同様にして粘着剤層を形成した。また、実施例1と同様にして、粘着型偏光板を作成した。
実施例1の(水分散型アクリル系粘着剤の調製)において、得られる水分散型アクリル系粘着剤の固形分濃度が20%になるように調整し、かつ、ウレタン会合系増粘剤のアデカノールUH541(株式会社ADEKA製)を水分散型アクリル系粘着剤の固形分100部に対して2重量部添加したこと以外は、実施例1と同様にして、水分散型アクリル系粘着剤を得た。当該水分散型アクリル系粘着剤の粘度は0.23Pa・s、体積平均粒子径は92nmであった。また、当該水分散型アクリル系粘着剤を用いたこと以外は、実施例1と同様にして粘着剤層を形成した。また、実施例1と同様にして、粘着型偏光板を作成した。
各例で得られた、離型フィルムに設けた厚さ23μmの粘着剤層を、スライドガラス板(マイクロスライドガラス,マツナミガラス製,厚さ1.3mm)上に貼着させたものについて、ヘイズメーター(HM−150型,(株)村上色彩技術研究所社製)にてヘイズ値を測定した。なお、ヘイズ測定の際は、離形フィルムを剥離して測定した。
粘着剤層の表面について、富士写真光機社製の「レーザー干渉計F601」を用いて富士スキャン法によりφ60mmの視野の表面粗さRa(凹凸)を測定した(単位nm)。粘着剤層の表面の測定は、離型フィルム(三菱化学ポリエステル(株)製,ダイアホイルMRF−38,ポリエチレンテレフタレート基材)上に形成した厚さ23μm(乾燥後)の粘着剤層の表面について行なった。離型フィルムを剥離した状態で測定すると、剥離時に粘着剤層表面が乱れ、平滑性に影響を与えるためである。なお、粘着剤層を設けた離型フィルムの表面のRaは6nmである。
得られた粘着型偏光板から離型フィルムを剥離して、粘着剤層側をガラス基板に貼り合せたものをサンプルとした。当該サンプルについて、蛍光灯下で、目視にて下記基準により正面及び斜め45°の2方向から視認性の観察を行った。
○:視認性に影響するムラなし。
△:多少のムラが確認できる。
×:視認性に問題あり。
Claims (15)
- 水分散型の(メタ)アクリル系重合体を含有する水分散液を含有する水分散型粘着剤を離型フィルムに塗工する工程(1)および塗工された水分散型粘着剤を乾燥する工程(2)を有する光学フィルム用粘着剤層の製造方法であって、
前記水分散型粘着剤は、せん断速度4000(1/s)における粘度が0.01〜0.1Pa・sであり、
前記離型フィルム上に形成される前記光学フィルム用粘着剤層の表面の表面粗さ(Ra)が10〜40nmであり、かつ、
前記光学フィルム用粘着剤層の厚さが23μmの場合のヘイズが、1%以下であることを特徴とする光学フィルム用粘着剤層の製造方法。 - 前記乾燥工程(2)は、温度40〜110℃の第一乾燥工程(21)と、温度100〜160℃の第二乾燥工程(22)を有することを特徴とする請求項1記載の光学フィルム用粘着剤層の製造方法。
- 前記水分散型粘着剤の(メタ)アクリル系重合体の体積平均粒子径が180nm以下であることを特徴とする請求項1または2記載の光学フィルム用粘着剤層の製造方法。
- 塗工工程(1)の塗工速度は、10〜100m/min、であることを特徴とする請求項1〜3のいずれかに記載の光学フィルム用粘着剤層の製造方法。
- 前記水分散型粘着剤は、固形分濃度が5〜45重量%の水分散液であることを特徴とする請求項1〜4のいずれかに記載の光学フィルム用粘着剤層の製造方法。
- 前記(メタ)アクリル系重合体が、総モノマー単位に対して、(メタ)アクリル酸アルキルエステル60〜99.9重量%およびカルボキシル基含有モノマー0.1〜10重量%をモノマー単位として含有することを特徴とする請求項1〜5のいずれかに記載の光学フィルム用粘着剤層の製造方法。
- 前記(メタ)アクリル系重合体が、モノマー単位として、さらに、リン酸基含有モノマーを含有することを特徴とする請求項6記載の光学フィルム用粘着剤層の製造方法。
- 前記リン酸基含有モノマーの割合が、(メタ)アクリル系重合体の総モノマー単位の0.1〜20重量%であることを特徴とする請求項7記載の光学フィルム用粘着剤層の製造方法。
- 前記(メタ)アクリル系重合体が、モノマー単位として、さらに、アルコキシシリル基含有モノマーを含有することを特徴とする請求項6〜8のいずれかに記載の光学フィルム用粘着剤層の製造方法。
- 前記アルコキシシリル基含有モノマーの割合が、(メタ)アクリル系重合体の総モノマー単位の0.001〜1重量%であることを特徴とする請求項9記載の光学フィルム用粘着剤層の製造方法。
- (メタ)アクリル酸アルキルエステル60〜99.9重量%に係るモノマー単位が、アクリル酸アルキルエステル60〜99.8重量%およびメタクリル酸アルキルエステル0.1〜39.9重量%に係るモノマー単位であることを特徴とする請求項6〜10のいずれかに記載の光学フィルム用粘着剤層の製造方法。
- アクリル酸アルキルエステルが、炭素数が3〜9のアクリル酸アルキルエステルであり、メタクリル酸アルキルエステルが、メタクリル酸メチル、メタクリル酸エチルおよびメタクリル酸シクロヘキシルから選ばれるいずれか少なくとも1つであることを特徴とする請求項11記載の光学フィルム用粘着剤層の製造方法。
- 請求項1〜12のいずれかに記載の製造方法により得られたものであることを特徴とする光学フィルム用粘着剤層。
- 光学フィルムの少なくとも片側に、請求項1〜13のいずれかに記載の光学フィルム用粘着剤層が積層されていることを特徴とする粘着型光学フィルム。
- 請求項14記載の粘着型光学フィルムを少なくとも1枚用いていることを特徴とする画像表示装置。
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JP2015209430A (ja) * | 2014-04-23 | 2015-11-24 | 東亞合成株式会社 | プラスチック製フィルム又はシート用活性エネルギー線硬化型粘接着剤組成物及び積層体の製造方法 |
JP2017206679A (ja) * | 2016-04-20 | 2017-11-24 | 東山フイルム株式会社 | 透明粘着層付き基材フィルム、透明粘着層付き透明導電性フィルム、およびタッチパネル |
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JP6344812B2 (ja) * | 2012-12-28 | 2018-06-20 | 日東電工株式会社 | 透明導電層用水分散型粘着剤組成物、透明導電層用粘着剤層、粘着剤層付き光学フィルム、及び、液晶表示装置 |
KR101821801B1 (ko) * | 2015-06-18 | 2018-01-25 | 삼성에스디아이 주식회사 | 편광판, 그의 제조방법 및 이를 포함하는 광학표시장치 |
FR3039455B1 (fr) * | 2015-07-31 | 2020-10-09 | Adhex Tech | Membrane permeable auto-adhesive et procede de fabrication d'une telle membrane permeable auto-adhesive |
EP3755753B1 (de) | 2018-02-21 | 2022-07-27 | Basf Se | Verfahren zur herstellung von mit klebstoff beschichteten artikeln |
CN113369095B (zh) * | 2021-06-18 | 2023-03-21 | 业成科技(成都)有限公司 | 免框胶式胶合结构的制作方法 |
CN115044087A (zh) * | 2022-08-15 | 2022-09-13 | 江苏康辉新材料科技有限公司 | 一种低雾度光学膜及其制备方法和应用 |
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US20130078407A1 (en) | 2013-03-28 |
JP5893881B2 (ja) | 2016-03-23 |
TW201323566A (zh) | 2013-06-16 |
KR101426146B1 (ko) | 2014-07-31 |
CN103013362A (zh) | 2013-04-03 |
KR20130033324A (ko) | 2013-04-03 |
US9181458B2 (en) | 2015-11-10 |
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