JP6530745B2 - フッ素含有アクリル樹脂からなるコーティング層を基材フィルムに積層させたフィルム - Google Patents
フッ素含有アクリル樹脂からなるコーティング層を基材フィルムに積層させたフィルム Download PDFInfo
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- JP6530745B2 JP6530745B2 JP2016519113A JP2016519113A JP6530745B2 JP 6530745 B2 JP6530745 B2 JP 6530745B2 JP 2016519113 A JP2016519113 A JP 2016519113A JP 2016519113 A JP2016519113 A JP 2016519113A JP 6530745 B2 JP6530745 B2 JP 6530745B2
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- film
- fluorine
- acrylic resin
- resin
- methacrylate
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- 229920000178 Acrylic resin Polymers 0.000 title claims description 121
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- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 title claims description 97
- 239000011247 coating layer Substances 0.000 title claims description 16
- 239000000758 substrate Substances 0.000 title claims description 14
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- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 claims description 16
- 239000000155 melt Substances 0.000 claims description 15
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- 125000004432 carbon atom Chemical group C* 0.000 claims description 10
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 7
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- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 42
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- -1 2- ( Trifluoromethyl) ethyl Chemical group 0.000 description 35
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- QTKPMCIBUROOGY-UHFFFAOYSA-N 2,2,2-trifluoroethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(F)(F)F QTKPMCIBUROOGY-UHFFFAOYSA-N 0.000 description 10
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 10
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- FRIBMENBGGCKPD-UHFFFAOYSA-N 3-(2,3-dimethoxyphenyl)prop-2-enal Chemical compound COC1=CC=CC(C=CC=O)=C1OC FRIBMENBGGCKPD-UHFFFAOYSA-N 0.000 description 8
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
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- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 8
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- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 8
- 229940048053 acrylate Drugs 0.000 description 8
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- 239000010419 fine particle Substances 0.000 description 8
- 239000004816 latex Substances 0.000 description 8
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- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 7
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- AVTLBBWTUPQRAY-UHFFFAOYSA-N 2-(2-cyanobutan-2-yldiazenyl)-2-methylbutanenitrile Chemical compound CCC(C)(C#N)N=NC(C)(CC)C#N AVTLBBWTUPQRAY-UHFFFAOYSA-N 0.000 description 6
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 6
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 description 6
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 6
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- 238000009826 distribution Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- FBCQUCJYYPMKRO-UHFFFAOYSA-N prop-2-enyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC=C FBCQUCJYYPMKRO-UHFFFAOYSA-N 0.000 description 5
- 238000010526 radical polymerization reaction Methods 0.000 description 5
- XWGJFPHUCFXLBL-UHFFFAOYSA-M rongalite Chemical compound [Na+].OCS([O-])=O XWGJFPHUCFXLBL-UHFFFAOYSA-M 0.000 description 5
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 5
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 description 4
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000000149 argon plasma sintering Methods 0.000 description 4
- 238000013329 compounding Methods 0.000 description 4
- 235000019329 dioctyl sodium sulphosuccinate Nutrition 0.000 description 4
- YHAIUSTWZPMYGG-UHFFFAOYSA-L disodium;2,2-dioctyl-3-sulfobutanedioate Chemical compound [Na+].[Na+].CCCCCCCCC(C([O-])=O)(C(C([O-])=O)S(O)(=O)=O)CCCCCCCC YHAIUSTWZPMYGG-UHFFFAOYSA-L 0.000 description 4
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- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 4
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- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 3
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 3
- VCYCUECVHJJFIQ-UHFFFAOYSA-N 2-[3-(benzotriazol-2-yl)-4-hydroxyphenyl]ethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCC1=CC=C(O)C(N2N=C3C=CC=CC3=N2)=C1 VCYCUECVHJJFIQ-UHFFFAOYSA-N 0.000 description 3
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- FRQQKWGDKVGLFI-UHFFFAOYSA-N 2-methylundecane-2-thiol Chemical compound CCCCCCCCCC(C)(C)S FRQQKWGDKVGLFI-UHFFFAOYSA-N 0.000 description 3
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- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
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- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
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- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 3
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- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 3
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- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 3
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- 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 3
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- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 2
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
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- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/546—Flexural strength; Flexion stiffness
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/714—Inert, i.e. inert to chemical degradation, corrosion
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2419/00—Buildings or parts thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2451/00—Decorative or ornamental articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2571/00—Protective equipment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2605/00—Vehicles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2605/00—Vehicles
- B32B2605/003—Interior finishings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
- B32B37/15—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state
- B32B37/153—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer being manufactured and immediately laminated before reaching its stable state, e.g. in which a layer is extruded and laminated while in semi-molten state at least one layer is extruded and immediately laminated while in semi-molten state
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/22—Esters containing halogen
- C08F220/24—Esters containing halogen containing perhaloalkyl radicals
-
- 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
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/06—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing only carbon, hydrogen, and oxygen, the oxygen atom being present only as part of the carboxyl radical
-
- 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
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2333/14—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing halogen, nitrogen, sulfur, or oxygen atoms in addition to the carboxy oxygen
- C08J2333/16—Homopolymers or copolymers of esters containing halogen atoms
-
- 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
- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
- C08J2433/14—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters of esters containing halogen, nitrogen, sulfur, or oxygen atoms in addition to the carboxy oxygen
- C08J2433/16—Homopolymers or copolymers of esters containing halogen atoms
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions 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; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
- C09D133/16—Homopolymers or copolymers of esters containing halogen atoms
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
- Coating Of Shaped Articles Made Of Macromolecular Substances (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Description
基材フィルム上に熱履歴が発生しないウェットコーティング法にてハードコート層及び含フッ素アルキル基含有(メタ)クリレートからなる反射防止層が順次積層されている(特許文献7参照)が、ハードコート層が3次元架橋されているため真空成形加工が乏しいため、インサート、インモールド成形用途への使用は容易ではない。
得られたフィルムを、透過型電子顕微鏡(日本電子製JEM−1200EX)にて、加速電圧80kV、RuO4染色超薄切片法で撮影し、得られた写真からアクリル酸エステル系架橋弾性体粒子画像を無作為に100個選択し、それらの粒子径の平均値を求めた。
日機装株式会社製 Microtrac粒度分布測定装置MT3000を使用し、ラテックス状態で光散乱法を用いて測定した。懸濁重合にて樹脂を作成した場合はスラリー状態にて、日機装株式会社製 Microtrac粒度分布計9210SRA/9220FRAを用いて測定した。
得られたフィルムの透明性は、JIS K6714に準じて、温度23℃±2℃、湿度50%±5%の条件下にて、曇価(ヘイズ)を測定した。
<耐キシレン性>
得られたフィルム上にキシレンを一滴(0.02g)垂らし、フィルムの変化を目視で評価した。
○:変化が全く認められない。
△:微小な滴下跡が認められる。
×:表面の劣化が酷く、滴下跡がはっきり認められる。
<耐日焼け止め剤性[耐コパトーン(登録商標)性](試験法1)>
得られたフィルム上に日焼け止め剤(コパトーン ウォーター・ベイビーズ・ローションSPF50)を少量塗布し、その上にガーゼを押し当て、500gの加重をかける。そのまま室温で1時間放置した後、オーブンで54℃、64℃で1時間加熱した後、付着した日焼け止め剤をガーゼでふき取り、フィルムを水洗し、目視で塗布部の変化を観測した。
○:変化が認められない。
△:微小な塗布跡が認められる。
×:表面の劣化が酷く、塗布跡がはっきり認められる。
得られたフィルム上に日焼け止め剤(コパトーン ウォーター・ベイビーズ・ローションSPF50)を一滴(0.005g)滴下し、2×3cmの範囲に刷毛を用いて延ばし、70℃、80℃、90℃で24時間放置した後、付着した日焼け止め剤をガーゼでふき取り、フィルムを水洗、目視で塗布部の変化を観測した。
○:変化が認められない。
△:微小な塗布跡が認められる。
×:表面の劣化が酷く、塗布跡がはっきり認められる。
得られたフィルム上に10%乳酸水溶液を一滴垂らし、80℃の温度条件化で24時間放置後、フィルムを水洗し、フィルムの変化を目視で評価した。
○:変化が全く認められない。
△:微小なピンホール状の溶解跡が認められる。
×:表面の劣化が酷く、溶解跡がはっきり認められる。
得られたフィルムを1回180度折り曲げて、折り曲げ部の変化を目視で評価した。
○:割れが認められない。
△:僅かに割れが発生する。
×:フィルムが割れ、完全に破断する。
得られたフィルムを1回180度折り曲げて、折り曲げ部の変化を目視で評価した。
○:白化が認められない。
△:光を透過した時に僅かに白化が認められる。
×:白化が認められる。
得られたフィルムの表面硬度は、JIS K5600−5−4に従い、鉛筆硬度を測定して評価した。
<単層フィルム連続生産性の評価:(評価法1)>
単層フィルムの溶融押出成形を2時間連続して行い、その運転状況を観察し、以下の基準により評価を行った。フッ素含有アクリル樹脂またはアクリル樹脂の各ペレットについて、Tダイ付40mmφ単軸押出機を用いて、シリンダ設定温度180〜240℃にて吐出量10kg/hrにて溶融混練し、ダイス温度240℃にて、厚み125μmの単層樹脂フィルムの溶融押出成形を行った。
○:フィルムに発砲、スジ(ダイライン)等の外観欠陥が発生しないで生産できる。
×:フィルムに発砲、スジ(ダイライン)等の外観欠陥が発生するため生産できない。
積層フィルムの溶融共押出成形を2時間連続して行い、その運転状況を観察し、以下の基準により評価を行った。共押出に用いるTダイとしては、2種2層Tダイ(フィードブロック方式)を使用した。基材フィルムとなる樹脂側の押出機としては、40mmφ単軸押出機を用い、シリンダ設定温度200〜260℃にて吐出量5〜15kg/hrにて溶融混練し、他方、フッ素含有アクリル樹脂側の押出機としては、32mmφ単軸押出機を用い、シリンダ設定温度180〜240℃にて吐出量0.5〜3kg/hrにて溶融混練し、ダイス温度240℃に設定された上記ダイ中に溶融樹脂を投入して、積層フィルムの溶融共押成形を行った。
○:フィルムに発砲、スジ(ダイライン)等の外観欠陥が発生しないで生産できる。
×:フィルムに発砲、スジ(ダイライン)等の外観欠陥が発生するため生産できない。
積層フィルムのウェットコーティング法を2時間連続して行い、その運転状況を観察し、以下の基準により評価を行った。 ウェットコーティング法は、基材フィルム上にフッ素系(メタ)アクリル樹脂をメチルイソブチルケトンに溶解させたコーティング溶液を特定バーコーターを使用してウェットコーティングし、その後乾燥80℃×2分パスを実施した。
○:フィルムに発砲、スジ(ダイライン)等の外観欠陥が発生しないで生産できる。
×:フィルムに発砲、スジ(ダイライン)等の外観欠陥が発生するため生産できない。
得られたフッ素含有アクリル樹脂をJIS K7199に準拠した条件下(ダイス温度220℃、剪断速度122sec-1、キャピラリーダイ径1mm)で測定した。
得られたフッ素含有アクリル樹脂をJIS K7199に準拠した条件下(ダイス温度230℃、剪断速度24sec-1、キャピラリーダイ径1mm、滞留時間1時間)で測定した溶融粘度値が、対応する同じダイス温度、剪断速度、滞留時間10分の条件下で測定した溶融粘度と比した際の低下率(%)を下記式から算出した。
溶融粘度低下率(%)=
滞留時間(滞留時間10分時の溶融粘度−滞留時間1時間時の溶融粘度)/(滞留時間10分時の溶融粘度) × 100 (%)
フッ素含有アクリル樹脂のガラス転移点の測定は、JIS K7121に規定される方法に準拠して測定される。但し、溶液品は溶剤脱気乾燥後おこなったもので測定した。
協和界面科学株式会社製の接触角測定機、FACEを用いて水接触角を測定した。サンプル台の温度を80℃に設定し、シリンジ針先より0.4mlの水滴を押し出した状態でサンプル台を持上げ、水滴をサンプルに接触させた。水滴がサンプルに接触した10秒後に水の接触角を測定した。
HLC8220GPC(東ソー株式会社製)を用い、GPCカラムとしてTSKgel Super H5000、H4000、H3000(東ソー株式会社製)を3本連結したものを用い、溶媒としてTHF(安定剤入り)を用いて、ポリスチレン換算で測定した。その他の条件は、測定温度:INLET OVEN 40℃、サンプル量:10μl、液量:0.6ml/min、検出器:RI である。
<フッ素含有アクリル樹脂(A−1)>
分散容器に、脱イオン水300部、ポリビニルアルコール1部を入れた。これとは別に、2,2,2−トリフルオロエチルメタクリレート90部、メチルメタクリレート10部、2、2‘−アゾビス(2−メチルブチロニトリル)0.5部および2-エチルヘキシルチオグリコール0.06部からなる単量体溶液を調製し、上記の分散容器に加えた。得られた混合液に対してホモミキサーを用いて分散処理を行い、液滴径を100nmに調整した分散液を得た。
<フッ素含有アクリル樹脂(A−2)>
攪拌機、温度計、還流冷却器、窒素ガス導入管及び滴下ロートを備えた反応器にメチルイソブチルケトンを83部仕込み、窒素ガスを導入しつつ85℃に昇温した後、2,2,2−トリフルオロエチルメタクリレート90部、メチルメタクリレート10部および2、2‘−アゾビス(2−メチルブチロニトリル)0.5部の混合物を滴下ロートから5時間かけて等速滴下した。次に、2、2‘−アゾビス(2−メチルブチロニトリル)0.2部およびメチルイソブチルケトン35部の混合溶液を1時間かけて等速滴下した。その後、引き続き、105℃で2時間攪拌した後に50℃まで冷却し、重合体(フッ素含有アクリル樹脂)(A−2L)を合成した。得られた重合体フッ素含有アクリル樹脂の固形分(A−2)濃度は45%、GPCで測定した数平均分子量は5万であった。さらに重合体フッ素含有アクリル樹脂(A−2)をエバポレーターによる減圧脱気処理でメチルイソブチルケトンを除去した後に製造1同様の操作によりペレット(A−2P)を得た。得られた(A−2P)の溶融粘度低下率は47%であった。
<フッ素含有アクリル樹脂(A−3)>
製造例1において、メチルメタクリレート10部の代わりにブチルアクリレート10部を使用するようにした以外は、製造例1と同様の操作にてフッ素含有アクリル樹脂(A−3)の球状有機微粒子粉体(平均粒子径100μm)を得た。得られたフッ素含有アクリル樹脂(A−3)100部を使用し、製造例1と同様に、フッ素含有アクリル樹脂の樹脂ペレット(A−3P)を製造した。
<フッ素含有アクリル樹脂(A−4)>
製造例2において2,2,2−トリフルオロエチルメタクリレート90部およびメチルアメタクリレート10部の代わりに、2、2、2−トリフルオロエチルメタクリレート70部、メチルメタクリレート30部を使用するようにした以外は、製造例2と同様の操作にて重合体(A−4L)を得て、得られた重合体(A−4L)の固形分(A−4)濃度は45%、GPCで測定した数平均分子量は5万であった。さらに重合体フッ素含有アクリル樹脂(A−4)をエバポレーターによる減圧脱気処理でメチルイソブチルケトンを除去した後に製造1同様の操作によりペレット(A−4P)を得た。得られた(A−4P)の溶融粘度低下率は47%であった。
<フッ素含有アクリル樹脂(A−5)>
製造例2において2,2,2−トリフルオロエチルメタクリレート90部およびメチルアメタクリレート10部の代わりに、2、2、2−トリフルオロエチルメタクリレート40部、メチルメタクリレート60部を使用するようにした以外は、製造例2と同様の操作にて重合体(A−5L)を得て、得られた重合体(A−5L)の固形分(A−5)濃度は45%、GPCで測定した数平均分子量は5万であった。
<フッ素含有アクリル樹脂(A−6)>
製造例2において2,2,2−トリフルオロエチルメタクリレート90部およびメチルアメタクリレート10部の代わりに、2−(パーフルオロヘキシル)エチルメタクリレ-ト90部、メチルメタクリレート10部を使用するようにした以外は、製造例2と同様の操作にて含フッ素アルキル(メタ)アクリレートポリマー(A−6L)を得て、得られた重合体(A−6L)の固形分(A−6)濃度は45%、GPCで測定した数平均分子量は5万であった。
<アクリル系弾性体グラフト共重合体(C1−1)>
攪拌機付き8L重合装置に、以下の物質を仕込んだ。
脱イオン水 200部
ジオクチルスルフォコハク酸ナトリウム 0.25部
ソディウムホルムアルデヒドスルフォキシレ−ト 0.15部
エチレンジアミン四酢酸−2−ナトリウム 0.001部
硫酸第一鉄 0.00025部
単量体混合物(c1−1a):
・ビニル系単量体混合物(アクリル酸ブチル(BA)90%およびメタクリル酸メチル(MMA)10%) 100部
・アリルメタクリレート(AlMA) 1部
・クメンハイドロパーオキサイド(CHP) 0.2部
メタクリル系重合体(C1−2)として、メタクリル酸メチル/アクリル酸メチル共重合体(住友化学(株)製、スミペックスLG、ビーズ状物)を使用した。
上記の如く得られたアクリル系弾性体グラフト共重合体(C1−1)25部およびメタクリル系重合体(C1−2)75部を、ヘンシェルミキサーを用いて混合した後、シリンダ温度を200℃〜260℃に温度調整した40mmφ単軸押出機(大阪精機工作(株)製)を使用し、スクリュー回転数90rpm、吐出量15kg/時間にて溶融混練を行い、ストランド状に引き取り、水槽にて冷却後、ペレタイザーを用いて切断して、アクリル系樹脂の樹脂ペレット(C−1P)を製造した。
<アクリル系弾性体グラフト共重合体(C2−1)>
攪拌機、温度計、窒素ガス導入管、モノマー供給管、還流冷却器を備えた8リットル重合機に以下の物質を仕込んだ。
水(イオン交換水) 200部
ナトリウムホルムアルデヒドスルホキシレート 0.15部
硫酸第一鉄・2水塩 0.0015部
エチレンジアミン四酢酸−2−ナトリウム 0.006部
ジオクチルスルホコハク酸ナトリウム 0.0015部
メタクリル系重合体(C2−2)として、メタクリル酸メチル/アクリル酸メチル共重合体(住友化学(株)製、スミペックスEX、ビーズ状物)を使用した。
上記の如く得られたアクリル系弾性体グラフト共重合体(C2−1)25部およびメタクリル系重合体(C2−2)75部、紫外線吸収剤としてチヌビン234(チバジャパン製)1.0部を、ヘンシェルミキサーを用いて混合した後、シリンダ温度を240℃に温度調整した以外は、製造例7と同様にして、アクリル樹脂の樹脂ペレット(C−2P)を製造した。
(実施例1)
製造例8で得られたアクリル系樹脂の樹脂ペレット(C−2P)を、Tダイ付40mmφ単軸押出機を用いて、シリンダ設定温度180〜240℃にて吐出量10kg/hrにて溶融混練し、ダイス温度240℃にて、厚み69μmの単層樹脂フィルムを得た。そのアクリル系樹脂のフィルム上に、フッ素含有アクリル樹脂の20%溶液(A−1L)をNo.16バーコーターでコーティング後に室温で30秒セッティングし、80℃乾燥機で2分間乾燥後の表層樹脂膜厚が6μmで総膜厚が75μmであった。得られたフィルムに関する評価結果を表1に示す。
製造例2で得られたフッ素含有アクリル樹脂の45%溶液(A−2L)を使用しNo.8バーコーターでコーティングした以外は、実施例1と同様の操作にて、表層樹脂膜厚が6μmで総膜厚が75μmの積層樹脂フィルムを得た。得られたフィルムに関する評価結果を表1に示す。
製造例4で得られたフッ素含有アクリル樹脂の45%溶液(A−4L)を使用した以外は、実施例2と同様の操作にて、表層樹脂膜厚が6μmで総膜厚が75μmの積層樹脂フィルムを得た。得られたフィルムに関する評価結果を表1に示す。
製造例7で得られたアクリル系樹脂の樹脂ペレット(C−1P)を、Tダイ付40mmφ単軸押出機を用いて、シリンダ設定温度180〜240℃にて吐出量10kg/hrにて溶融混練し、ダイス温度240℃にて、厚み69μmの単層樹脂フィルムを得た。そのアクリル系樹脂のフィルム上に、フッ素系(メタ)アクリル樹脂の45%溶液(A−2L)をNo.8バーコーターでコーティング後に室温で30秒セッティングし、80℃乾燥機で2分間乾燥後の表層樹脂膜厚が6μmで総膜厚が75μmであった。得られたフィルムに関する評価結果を表1に示す。
製造例1で得られたフッ素系(メタ)アクリル樹脂の20%溶液(A−1L)をNo.8バーコーターでコーティングした以外は、実施例2と同様の操作にて、表層樹脂膜厚が3μmで総膜厚が75μmの積層樹脂フィルムを得た。得られたフィルムに関する評価結果を表1に示す。
製造例8で得られたアクリル樹脂の樹脂ペレット(C−2)を、Tダイ付40mmφ単軸押出機を用いて、シリンダ設定温度180〜240℃にて吐出量10kg/hrにて溶融混練し、ダイス温度240℃にて、厚み69μmの単層樹脂フィルムを得た。そのアクリル系樹脂のフィルム上に、フッ素系(メタ)アクリル樹脂の45%溶液(A−3L)をNo.8バーコーターで塗工後に室温で30秒セッティングし、80℃乾燥機で2分間乾燥後の表層樹脂膜厚が6μmで総膜厚が75μmであった。得られたフィルムに関する評価結果を表1に示す。
製造例5で得られたフッ素含有アクリル樹脂の45%溶液(A−5L)を使用した以外は、実施例1と同様の操作にて、表層樹脂膜厚が6μmで総膜厚が75μmの積層樹脂フィルムを得た。得られたフィルムに関する評価結果を表1に示す。
製造例6で得られたフッ素系(メタ)アクリル樹脂の45%溶液(A−6L)を使用した以外は、実施例1と同様の操作にて、表層樹脂膜厚が6μmで総膜厚が75μmの積層樹脂フィルムを得た。得られたフィルムに関する評価結果を表1に示す。
(比較例4)
製造例8で得られたアクリル樹脂の樹脂ペレット(C−2)をベース樹脂とし、製造例1で得られたフッ素含有アクリル樹脂の樹脂ペレット(A−1P)を表面層樹脂として、以下の共押出方法により、総膜厚75μm(ベース樹脂層69μmおよび表層樹脂層6μm)の積層フィルムを得た。
製造例8で得られたアクリル系樹脂の樹脂ペレット(C−2)とフッ素系(メタ)アクリル樹脂の樹脂ペレット(A−3P)を使用した以外は比較例4と同様の操作にて、総膜厚75μmの単層樹脂フィルムを得た。得られたフィルムに関する評価結果を表1に示す。
ベース樹脂層72μmおよび表層樹脂層3μmとした以外は比較例5と同様の操作にて、総膜厚75μmの積層フィルムを得た。得られたフィルムに関する評価結果を表1に示す。
Claims (8)
- 前記基材フィルムがゴム粒子含有アクリル樹脂である、請求項1に記載のフィルム。
- 前記フッ素含有アクリル樹脂のガラス転移点が70℃以上である、請求項1または2に記載のフィルム。
- 前記メタクリレート系単量体がメチルメタクリレートである、請求項1〜3のいずれか1項に記載のフィルム。
- 前記フッ素含有アクリル樹脂が、前記メタクリレート系単量体30〜1重量部に対して、前記一般式(1)で示す単量体70〜99重量部を共重合してなるフッ素含有アクリル樹脂である、請求項1〜4のいずれか1項に記載のフィルム。
- 前記基材フィルムに前記コーティング層を積層させる方法が、ウェットコーティング法である、請求項1〜5のいずれか1項に記載のフィルム。
- 請求項1〜6のいずれか1項に記載のフィルムの製造方法であって、
前記フッ素含有アクリル樹脂をウェットコーティング法により前記基材フィルムに積層させるフィルムの製造方法。 - 前記メタクリレート系単量体に対して、前記一般式(1)で示す単量体を共重合する方法が、懸濁重合である、請求項7に記載のフィルムの製造方法。
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