JP7466453B2 - ポリビニルアセタール樹脂フィルムおよびそれを含む積層体 - Google Patents
ポリビニルアセタール樹脂フィルムおよびそれを含む積層体 Download PDFInfo
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- JP7466453B2 JP7466453B2 JP2020549289A JP2020549289A JP7466453B2 JP 7466453 B2 JP7466453 B2 JP 7466453B2 JP 2020549289 A JP2020549289 A JP 2020549289A JP 2020549289 A JP2020549289 A JP 2020549289A JP 7466453 B2 JP7466453 B2 JP 7466453B2
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- polyvinyl acetal
- acetal resin
- resin film
- film
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- 229920002554 vinyl polymer Polymers 0.000 title claims description 328
- 239000011354 acetal resin Substances 0.000 title claims description 322
- 229920006324 polyoxymethylene Polymers 0.000 title claims description 322
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 title claims description 308
- 229920005989 resin Polymers 0.000 claims description 68
- 239000011347 resin Substances 0.000 claims description 68
- 239000004014 plasticizer Substances 0.000 claims description 45
- 239000000463 material Substances 0.000 claims description 40
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 27
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 27
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 27
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- 238000006116 polymerization reaction Methods 0.000 claims description 20
- 239000011521 glass Substances 0.000 claims description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 17
- 238000009826 distribution Methods 0.000 claims description 11
- 239000010410 layer Substances 0.000 description 68
- 239000005340 laminated glass Substances 0.000 description 25
- 239000002346 layers by function Substances 0.000 description 23
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical group OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 19
- 238000006359 acetalization reaction Methods 0.000 description 16
- 239000003963 antioxidant agent Substances 0.000 description 16
- 230000015572 biosynthetic process Effects 0.000 description 16
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- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 4
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
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- FRQDZJMEHSJOPU-UHFFFAOYSA-N Triethylene glycol bis(2-ethylhexanoate) Chemical compound CCCCC(CC)C(=O)OCCOCCOCCOC(=O)C(CC)CCCC FRQDZJMEHSJOPU-UHFFFAOYSA-N 0.000 description 3
- 239000003377 acid catalyst Substances 0.000 description 3
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical class OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 3
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- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical class OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 3
- 239000003381 stabilizer Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- JEYLQCXBYFQJRO-UHFFFAOYSA-N 2-[2-[2-(2-ethylbutanoyloxy)ethoxy]ethoxy]ethyl 2-ethylbutanoate Chemical compound CCC(CC)C(=O)OCCOCCOCCOC(=O)C(CC)CC JEYLQCXBYFQJRO-UHFFFAOYSA-N 0.000 description 2
- SSKNCQWPZQCABD-UHFFFAOYSA-N 2-[2-[2-(2-heptanoyloxyethoxy)ethoxy]ethoxy]ethyl heptanoate Chemical compound CCCCCCC(=O)OCCOCCOCCOCCOC(=O)CCCCCC SSKNCQWPZQCABD-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
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- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
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- 125000002723 alicyclic group Chemical group 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 239000004305 biphenyl Substances 0.000 description 2
- 235000010290 biphenyl Nutrition 0.000 description 2
- 125000006267 biphenyl group Chemical group 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
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- HHLFWLYXYJOTON-UHFFFAOYSA-N glyoxylic acid Chemical compound OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 description 2
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- 239000000113 methacrylic resin Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
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- YIMHRDBSVCPJOV-UHFFFAOYSA-N n'-(2-ethoxyphenyl)-n-(2-ethylphenyl)oxamide Chemical compound CCOC1=CC=CC=C1NC(=O)C(=O)NC1=CC=CC=C1CC YIMHRDBSVCPJOV-UHFFFAOYSA-N 0.000 description 2
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- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 2
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- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
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- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
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- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 2
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- OLAQBFHDYFMSAJ-UHFFFAOYSA-L 1,2-bis(7-methyloctyl)cyclohexane-1,2-dicarboxylate Chemical compound CC(C)CCCCCCC1(C([O-])=O)CCCCC1(CCCCCCC(C)C)C([O-])=O OLAQBFHDYFMSAJ-UHFFFAOYSA-L 0.000 description 1
- DLZBUNUDESZERL-UHFFFAOYSA-N 1-o-heptyl 6-o-nonyl hexanedioate Chemical compound CCCCCCCCCOC(=O)CCCCC(=O)OCCCCCCC DLZBUNUDESZERL-UHFFFAOYSA-N 0.000 description 1
- KGRVJHAUYBGFFP-UHFFFAOYSA-N 2,2'-Methylenebis(4-methyl-6-tert-butylphenol) Chemical compound CC(C)(C)C1=CC(C)=CC(CC=2C(=C(C=C(C)C=2)C(C)(C)C)O)=C1O KGRVJHAUYBGFFP-UHFFFAOYSA-N 0.000 description 1
- CXDRHQMFHIESDS-UHFFFAOYSA-N 2,4-ditert-butyl-6-(5-chlorobenzotriazol-2-yl)-4-methylcyclohexa-1,5-dien-1-ol Chemical compound CC(C)(C)C1(C)CC(C(C)(C)C)=C(O)C(N2N=C3C=C(Cl)C=CC3=N2)=C1 CXDRHQMFHIESDS-UHFFFAOYSA-N 0.000 description 1
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- WSOMHEOIWBKOPF-UHFFFAOYSA-N 2,6-ditert-butyl-4-[(6-oxobenzo[c][2,1]benzoxaphosphinin-6-yl)methyl]phenol Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CP2(=O)C3=CC=CC=C3C3=CC=CC=C3O2)=C1 WSOMHEOIWBKOPF-UHFFFAOYSA-N 0.000 description 1
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- GYHPTPQZVBYHLC-UHFFFAOYSA-N 2-[2-[2-[2-(2-ethylhexanoyloxy)ethoxy]ethoxy]ethoxy]ethyl 2-ethylhexanoate Chemical compound CCCCC(CC)C(=O)OCCOCCOCCOCCOC(=O)C(CC)CCCC GYHPTPQZVBYHLC-UHFFFAOYSA-N 0.000 description 1
- QSRJVOOOWGXUDY-UHFFFAOYSA-N 2-[2-[2-[3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoyloxy]ethoxy]ethoxy]ethyl 3-(3-tert-butyl-4-hydroxy-5-methylphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C)=CC(CCC(=O)OCCOCCOCCOC(=O)CCC=2C=C(C(O)=C(C)C=2)C(C)(C)C)=C1 QSRJVOOOWGXUDY-UHFFFAOYSA-N 0.000 description 1
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- HXIQYSLFEXIOAV-UHFFFAOYSA-N 2-tert-butyl-4-(5-tert-butyl-4-hydroxy-2-methylphenyl)sulfanyl-5-methylphenol Chemical compound CC1=CC(O)=C(C(C)(C)C)C=C1SC1=CC(C(C)(C)C)=C(O)C=C1C HXIQYSLFEXIOAV-UHFFFAOYSA-N 0.000 description 1
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- HRECPBLGWOTTIT-UHFFFAOYSA-N 3,9-bis(2-dodecylsulfanylethyl)-2,4,8,10-tetraoxaspiro[5.5]undecane Chemical compound C1OC(CCSCCCCCCCCCCCC)OCC21COC(CCSCCCCCCCCCCCC)OC2 HRECPBLGWOTTIT-UHFFFAOYSA-N 0.000 description 1
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- ADRNSOYXKABLGT-UHFFFAOYSA-N 8-methylnonyl diphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OCCCCCCCC(C)C)OC1=CC=CC=C1 ADRNSOYXKABLGT-UHFFFAOYSA-N 0.000 description 1
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- 230000007062 hydrolysis Effects 0.000 description 1
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- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
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- DOIRQSBPFJWKBE-UHFFFAOYSA-N phthalic acid di-n-butyl ester Natural products CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 1
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- PZTAGFCBNDBBFZ-UHFFFAOYSA-N tert-butyl 2-(hydroxymethyl)piperidine-1-carboxylate Chemical compound CC(C)(C)OC(=O)N1CCCCC1CO PZTAGFCBNDBBFZ-UHFFFAOYSA-N 0.000 description 1
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- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- XUHUMYVYHLHMCD-UHFFFAOYSA-N tris(2-cyclohexylphenyl) phosphite Chemical compound C1CCCCC1C1=CC=CC=C1OP(OC=1C(=CC=CC=1)C1CCCCC1)OC1=CC=CC=C1C1CCCCC1 XUHUMYVYHLHMCD-UHFFFAOYSA-N 0.000 description 1
- WGKLOLBTFWFKOD-UHFFFAOYSA-N tris(2-nonylphenyl) phosphite Chemical compound CCCCCCCCCC1=CC=CC=C1OP(OC=1C(=CC=CC=1)CCCCCCCCC)OC1=CC=CC=C1CCCCCCCCC WGKLOLBTFWFKOD-UHFFFAOYSA-N 0.000 description 1
- HBYRZSMDBQVSHO-UHFFFAOYSA-N tris(2-tert-butyl-4-methylphenyl) phosphite Chemical compound CC(C)(C)C1=CC(C)=CC=C1OP(OC=1C(=CC(C)=CC=1)C(C)(C)C)OC1=CC=C(C)C=C1C(C)(C)C HBYRZSMDBQVSHO-UHFFFAOYSA-N 0.000 description 1
- WRSPWQHUHVRNFV-UHFFFAOYSA-N tris[3,5-di(nonyl)phenyl] phosphite Chemical compound CCCCCCCCCC1=CC(CCCCCCCCC)=CC(OP(OC=2C=C(CCCCCCCCC)C=C(CCCCCCCCC)C=2)OC=2C=C(CCCCCCCCC)C=C(CCCCCCCCC)C=2)=C1 WRSPWQHUHVRNFV-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- 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
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- B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
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- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10761—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing vinyl acetal
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- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/10009—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets
- B32B17/10036—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising two outer glass sheets
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- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
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- B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
- B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
- B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
- B32B17/10559—Shape of the cross-section
- B32B17/10577—Surface roughness
- B32B17/10587—Surface roughness created by embossing
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/22—Layered products comprising a layer of synthetic resin characterised by the use of special additives using plasticisers
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- 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
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
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- Polymers & Plastics (AREA)
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Description
[1]ポリビニルアセタール樹脂材料から構成されるポリビニルアセタール樹脂フィルムであって、厚みが10~350μmであり、一方の面の十点平均粗さRz値が2μm未満であり、該表面の摩擦角が31°より大きく40°以下であり、かつ、他方の面の十点平均粗さRz値が2μm以上7μm以下であり、該表面の摩擦角が20°以上31°以下であり、
前記十点平均粗さRz値がJIS B0601-1994に準拠して測定した値であり、
前記摩擦角がJIS P 8147に記載の傾斜法に準処して測定した値であり、
前記ポリビニルアセタール樹脂材料中のポリビニルアセタール樹脂の、ブルックフィールド型(B型)粘度計を用いて20℃、30rpmで測定された、濃度10質量%のトルエン/エタノール=1/1(質量比)溶液の粘度が100~1000mPa・sであり、ポリビニルアセタール樹脂フィルム中の可塑剤の量がポリビニルアセタール樹脂フィルムの総質量に基づいて0~20質量%である、ポリビニルアセタール樹脂フィルム。
[2]一方の面の摩擦角と他方の面の摩擦角との差分絶対値が2°以上10°以下である、前記[1]に記載のポリビニルアセタール樹脂フィルム。
[3]一方の面の十点平均粗さRz値と他方の面の十点平均粗さRz値との差分絶対値が1μm以上5μm以下である、前記[1]または[2]に記載のポリビニルアセタール樹脂フィルム。
[4]前記ポリビニルアセタール樹脂材料中のポリビニルアセタール樹脂の、ブルックフィールド型(B型)粘度計を用いて20℃、30rpmで測定された、濃度10質量%のトルエン/エタノール=1/1(質量比)溶液の粘度が300mPa・s以下である、前記[1]~[3]のいずれかに記載のポリビニルアセタール樹脂フィルム。
[5]前記ポリビニルアセタール樹脂材料中のポリビニルアセタール樹脂の、ブルックフィールド型(B型)粘度計を用いて20℃、30rpmで測定された、濃度10質量%のトルエン/エタノール=1/1(質量比)溶液の粘度が200mPa・sより大きい、前記[1]~[3]のいずれかに記載のポリビニルアセタール樹脂フィルム。
[6]前記ポリビニルアセタール樹脂材料中のポリビニルアセタール樹脂の分子量分布が2.7以上である、前記[1]~[5]のいずれかに記載のポリビニルアセタール樹脂フィルム。
[7]前記ポリビニルアセタール樹脂材料中のポリビニルアセタール樹脂が、粘度平均重合度の異なる少なくとも2つのポリビニルアセタール樹脂の混合物、または、粘度平均重合度の異なる少なくとも2つのポリビニルアルコール系樹脂の混合物のアセタール化物である、前記[1]~[6]のいずれかに記載のポリビニルアセタール樹脂フィルム。
[8]複数の透明基材の間に、前記[1]~[7]のいずれかに記載のポリビニルアセタール樹脂フィルムが挟持されてなる、積層体。
[9]さらに可塑化ポリビニルアセタール樹脂層を含む、前記[8]に記載の積層体。
[10]前記透明基材がガラスである、前記[8]または[9]に記載の積層体。
[11]前記[8]~[10]のいずれかに記載の積層体からなる乗物用ガラス。
本発明のポリビニルアセタール樹脂フィルムの一方の面の十点平均粗さRz値は2μm未満であり、該表面の摩擦角は31°より大きく40°以下であり、他方の面の十点平均粗さRz値は2μm以上7μm以下であり、該表面の摩擦角は20°以上31°以下である。合わせガラス用中間膜に用いられるような従来のポリビニルアセタール樹脂フィルムは、一般的にその両表面が同じような表面形状を有するが、本発明のポリビニルアセタール樹脂フィルムは、一方の面と他方の面とが互いに異なる表面形状を有する。これにより、製膜後の長尺のフィルムをロール状に巻回する際に隣接する樹脂フィルムの一方の面と他方の面との間に微細な空隙が生じ、フィルム同士の密着性が適度に低下するため経時的な自着を抑制することができる。また、フィルム同士の自着や空気の巻込みによるロールじわの発生を抑制することができ、巻き出し時に均一な表面を有するフィルムロールを得ることができる。さらに、樹脂フィルムの表面粗さを制御するとともに摩擦角を制御することにより、巻回時に隣接するフィルム同士が適度な密着性をもって接するため、フィルム同士のずれや自着を抑制し、経時的な端面ずれの発生を抑制することができる。
なお、樹脂フィルム表面の十点平均粗さは、表面粗さ計またはレーザー顕微鏡を用いて、JIS B0601-1994に準拠して測定することができる。接触式の表面粗さ計による測定が好ましい。具体的には、後述の実施例に記載の方法により測定することができる。
なお、樹脂フィルム表面の摩擦角は、一般的な摩擦測定器を用いて、JIS P 8147に準拠して測定できる。具体的には、後述の実施例に記載の方法により測定することができる。
なお、ポリビニルアセタール樹脂フィルムの厚みは、例えば厚さ計またはレーザー顕微鏡等を用いて測定できる。
本発明のポリビニルアセタール樹脂フィルムは、ポリビニルアセタール樹脂を含むポリビニルアセタール樹脂材料から構成される。ポリビニルアセタール樹脂は、ポリビニルアルコールまたはエチレンビニルアルコールコポリマー等のポリビニルアルコール系樹脂のアセタール化によって製造される樹脂である。なお、本発明において「ポリビニルアセタール樹脂材料」には、ポリビニルアセタール樹脂からなるもの、および、ポリビニルアセタール樹脂を含む樹脂組成物からなるもののいずれもが含まれる。
なお、ピークトップ分子量および分子量分布は、例えばゲルパーミエーションクロマトグラフィー(GPC)を用い、分子量既知のポリスチレンを標準として求められる。
本発明において、ポリビニルアセタール樹脂フィルム中の可塑剤の量は、ポリビニルアセタール樹脂フィルムの総質量に基づいて0~20質量%である。前記可塑剤量が20質量%を超えると、良好な製膜性が得にくくなる。また、特に高温環境下で樹脂フィルムが変形しやすくなる傾向にあるため、例えば機能性層をポリビニルアセタール樹脂フィルムに付与し積層して合わせガラスを作製する場合、良好な機能性を発揮し得なくなる。可塑剤量を少なくするまたは可塑剤を配合しないことにより、ポリビニルアセタール樹脂フィルムは、成膜性および取扱性に優れる傾向にあるが、同時に低可塑または無可塑のポリビニルアセタール樹脂フィルムでは、ロールじわが発生しやすくなる傾向にある。本発明のポリビニルアセタール樹脂フィルムでは、樹脂フィルムの両表面の十点平均粗さおよび摩擦角が上記特定の関係になるよう制御することにより、樹脂フィルムの一方の面と他方の面とが異なる表面形状を有する。このため、可塑剤量が少ないことに起因して本来ロールじわが生じやすい樹脂フィルムであっても、隣接する樹脂フィルム間に適度な空隙を生じ、ロールじわの発生を効果的に抑制することができ、フィルムを巻き出した際に均一なフィルム表面が得られやすい。したがって、比較的滑らかな面(表面1)に機能性層等を積層することにより、機能性層の経時的な変形および破壊を生じ難い合わせガラスを得ることができ、本発明のポリビニルアセタール樹脂フィルムは、機能性層等を有する合わせガラス用の樹脂フィルムとして好適に使用し得る。
・多価の脂肪族または芳香族酸のエステル。例えば、ジアルキルアジペート(例えば、ジヘキシルアジペート、ジ-2-エチルブチルアジペート、ジオクチルアジペート、ジ-2-エチルヘキシルアジペート、ヘキシルシクロヘキシルアジペート、ジヘプチルアジペート、ジノニルアジペート、ジイソノニルアジペート、ヘプチルノニルアジペート);アジピン酸とアルコール若しくはエーテル化合物を含むアルコールとのエステル(例えば、ジ(ブトキシエチル)アジペート、ジ(ブトキシエトキシエチル)アジペート);ジアルキルセバケート(例えば、ジブチルセバケート);セバシン酸と脂環式若しくはエーテル化合物を含むアルコールとのエステル;フタル酸のエステル(例えば、ブチルベンジルフタレート、ビス-2-ブトキシエチルフタレート);および脂環式多価カルボン酸と脂肪族アルコールとのエステル(例えば、1,2-シクロヘキサンジカルボン酸ジイソノニルエステル)が挙げられる。
・多価の脂肪族若しくは芳香族アルコールまたは1つ以上の脂肪族若しくは芳香族置換基を有するオリゴエーテルグリコールのエステルまたはエーテル。例えば、グリセリン、ジグリコール、トリグリコール、テトラグリコール等と、直鎖状若しくは分岐状の脂肪族若しくは脂環式カルボン酸とのエステルが挙げられる。具体的には、ジエチレングリコール-ビス-(2-エチルヘキサノエート)、トリエチレングリコール-ビス-(2-エチルヘキサノエート)(以下において、「3GO」と称することもある)、トリエチレングリコール-ビス-(2-エチルブタノエート)、テトラエチレングリコール-ビス-n-ヘプタノエート、トリエチレングリコール-ビス-n-ヘプタノエート、トリエチレングリコール-ビス-n-ヘキサノエート、テトラエチレングリコールジメチルエーテル、およびジプロピレングリコールジベンゾエートが挙げられる。
・脂肪族または芳香族アルコールのリン酸エステル。例えば、トリス(2-エチルヘキシル)ホスフェート、トリエチルホスフェート、ジフェニル-2-エチルヘキシルホスフェート、およびトリクレジルホスフェートが挙げられる。
・クエン酸、コハク酸および/またはフマル酸のエステル。
紫外線吸収剤または紫外線遮蔽剤は、単独で、または2種以上を組み合わせて使用できる。
ポリビニルアセタール樹脂フィルムの製造方法は特に限定されない。前記ポリビニルアセタール樹脂、場合により所定量の可塑剤、および必要に応じて他の添加剤を配合し、これを均一に混練した後、押出法、カレンダー法、プレス法、キャスティング法、インフレーション法等の公知の製膜方法によりフィルム状に成形することで作製し得る。
本発明は、複数の透明基材の間に、本発明のポリビニルアセタール樹脂フィルムを含む積層体に関する。
この際、透明基材に接する本発明のポリビニルアセタール樹脂フィルムの表面は、十点平均粗さの大きい表面2の面であることが好ましい。表面粗さが大きい面が透明基材と接することにより、透明基材とポリビニルアセタール樹脂フィルムとを貼合する際に脱気しやすくなり、積層体(合わせガラス)における発泡を抑制することができる。
各実施例および比較例において用いたポリビニルアセタール樹脂の組成および物性を表1に示す。
上記表1および下記表2に記載のポリビニルアセタール樹脂1および2、並びに各混合物の粘度は、ポリビニルアセタール樹脂1、2およびこれらの各比率の混合物を、トルエン/エタノール=1/1の混合溶液中に濃度10質量%となるよう加え、溶解させ、得られた溶液の粘度を、ブルックフィールド型(B型)粘度計を用いて20℃、30rpmで測定した。
得られたポリビニルアセタール樹脂フィルムを構成するための樹脂を、GPCにより分析した。GPC分析には、分析装置としてViscotek製GPCmaxTDA305およびRI検出器を用い、カラムとてShodex製GPC KF-806LおよびGPC KF-806Lを2本連結して別途先端にガードカラムとしてのShodex製 KF-Gを連結したものを用い、THF溶媒および標準ポリスチレン(Agilent Technologies社製 Easical GPC/SEC Calibration Standards PS-1)を用い、解析ソフトとしてOmniSE、C4.7を用いた。40℃、注入量100μLで測定を行い、前記樹脂のピークトップ分子量および分子量分布を求めた。結果を表2に示す。
PVB-aおよびPVB-bのペレットを単軸押出機で溶融押し出しした際の製膜性を、下記基準で評価した。結果を表2に示す。
A 製膜性は非常に良好であった。
B 製膜は良好であった。
C 着色および分解ガスの発生が起こったが、製膜可能であった。
D 製膜不可能であった。
(1)ポリビニルアセタール樹脂フィルムの作製
表1に示す物性を有するポリビニルブチラール樹脂1(以下、「樹脂1」と称する)およびポリビニルブチラール樹脂2(以下、「樹脂2」と称する)を、80:20の質量比でブレンドしたPVB-aを、溶融混練してストランド状に押出し、ペレット化した。得られたペレットを単軸押出機とTダイを用いて230℃で溶融押出した。金属弾性ロールと金属剛体ロールを用いて製膜を行い、ポリビニルアセタール樹脂フィルムPVBF-Aを製造した。
得られたポリビニルアセタール樹脂フィルムの表面物性を、以下の方法に従い測定した。また、ポリビニルアセタール樹脂フィルムをロール状に巻回した際の端面ずれ、および、自着性を以下の方法に従い評価した。
フィルム両表面の十点平均粗さRz値を、株式会社ミツトヨ製サーフテストSJ-310(測定力:0.75mN、スタイラス形状:先端半径2μmR/先端角度60°)を用い、JIS B0601-1994に準拠して測定した。結果を表3に示す。
フィルムの両表面の摩擦角を、それぞれ、摩擦測定器(株式会社東洋精機製作所製、形式:AN-S形)を用いて、JIS P 8147に記載の傾斜法に準処して測定した。具体的には、傾斜板に厚み100μmのPETフィルム(東洋紡エステル(登録商標)フィルム 品名5101;片面がコロナ処理されたもの)を、コロナ処理面側が傾斜板に接しないように固定した。おもりとして、長方形の平らな底面をもつ幅60mm、長さ100mmおよび質量1000gの金属製ブロックを使用し、そのおもりに幅60mm、長さ約120mmの測定対象とするポリビニルアセタール樹脂フィルムを固定した。次に、本体の水平を確認後、傾斜板の傾斜角を0にあわせ、おもりを固定したポリビニルアセタール樹脂フィルムの測定対象とする表面が、PETフィルムのコロナ処理面と接するように設置した。1°/secの一定速度で傾斜板の傾斜角度を上げ、おもりを固定したポリビニルアセタール樹脂フィルムがすべり始めた時の傾斜角をよみとった。同様の試験を10回繰り返し、平均値を算出し、その値を摩擦角とした。測定雰囲気は、温度:20±2℃、相対湿度:65±5%である。結果を表3に示す。
厚み50μmのポリビニルアセタール樹脂フィルムを、巻取張力90N/m幅、巻取速度10m/分、巻長1000mで、内径152mm、外径164mm、幅400mmのABS樹脂製の巻軸にロール状に巻き取った。巻き取ったロール状巻物を温度35℃、相対湿度65%の環境下に1ケ月間水平に放置した後、ロール状巻物の端面のズレ状況を目視で観察した。評価基準は下記の通りである。結果を表3に示す。
A:ズレが観察されなかった。
B:フィルム端部のズレが1mm未満であった。
C:フィルム端部のズレが1mm以上であった。
ポリビニルアセタール樹脂フィルムを10cm×3cmの大きさに切断して得られた試験片の短軸の端部から5mm内側までポリイミドテープを張り付けたフィルム試験片を準備した。前記フィルム試験片に、ポリイミドテープを張り付けていない上記と同じ試験片(同一材料で同一の大きさ)を重ねて合わせて、2枚のポリビニルアセタール樹脂フィルム試験片の間に、その端部でポリイミドテープが挟持された積層体を作製した。この際に試験片の一方の面(表面1)と他方の面(表面2)が接するようにした。その上に6kgの重りを載せ、50℃で8時間静置後、23℃、50%RHの条件下で24時間放置した。その後、2枚の積層体片をポリイミドテープの部分から手ではがし、それぞれの状態を観察した。評価基準は下記の通りである。結果を表3に示す。
A:容易に剥がれ、フィルム表面に変形がみられなかった。
B:多少接着している部分があるが、剥がした際、フィルム表面に変形がみられなかった。
C:強く接着しており、剥がした際、フィルム表面に変形がみられた。
実施例1の金属弾性ロールをゴム弾性ロールに変更した以外は実施例1と同様に製膜し、ポリビニルアセタール樹脂フィルムPVBF-Bを得た。得られたPVBF-Bの表面物性および特性を、実施例1と同様の方法で測定および評価した。結果を表3に示す。
ポリビニルアセタール樹脂材料としてPVB-aの代わりにPVB-bを用いた以外は実施例1と同様に製膜し、ポリビニルアセタール樹脂フィルムPVBF-Cを得た。得られたPVBF-Cの表面物性および特性を、実施例1と同様の方法で測定および評価した。結果を表3に示す。
可塑剤として3GOを用い、該可塑剤が樹脂PVB-aに対して添加量が5質量%になるように溶融混練した。次に、得られた溶融混練物をストランド状に押出し、ペレット化した。得られたペレットを、実施例1と同様に製膜し、ポリビニルアセタール樹脂フィルムPVBF-Dを得た。得られたPVBF-Dの表面物性および特性を、実施例1と同様の方法で測定および評価した。結果を表3に示す。
実施例4の可塑剤量を5質量%から15質量%に変更した以外は実施例4と同様にペレットを得た。得られたペレットを、実施例1の金属弾性ロールをゴム弾性ロールに変更した以外は実施例1と同様に製膜し、ポリビニルアセタール樹脂フィルムPVBF-Eを得た。得られたPVBF-Eの表面物性および特性を、実施例1と同様の方法で測定および評価した。結果を表3に示す。
実施例1の金属弾性ロールを金属剛体ロールに変更した以外は実施例1と同様に製膜し、ポリビニルアセタール樹脂フィルムPVBF-Fを得た。得られたPVBF-Fの表面物性および特性を、実施例1と同様の方法で測定および評価した。結果を表3に示す。
実施例1の金属剛体ロールを金属弾性ロールに変更した以外は実施例1と同様に製膜し、ポリビニルアセタール樹脂フィルムPVBF-Gを得た。得られたPVBF-Gの表面物性および特性を、実施例1と同様の方法で測定および評価した。結果を表3に示す。
ポリビニルアセタール樹脂材料としてPVB-aの代わりにPVB-bを用いた以外は実施例6と同様に製膜し、ポリビニルアセタール樹脂フィルムPVBF-Hを得た。得られたPVBF-Hの表面物性および特性を、実施例1と同様の方法で測定および評価した。結果を表3に示す。
実施例1の金属弾性ロールをエンボスロールに変更した以外は実施例1と同様に製膜し、ポリビニルアセタール樹脂フィルムPVBF-Iを得た。得られたPVBF-Iの表面物性および特性を、実施例1と同様の方法で測定および評価した。結果を表3に示す。
Claims (11)
- ポリビニルアセタール樹脂材料から構成されるポリビニルアセタール樹脂フィルムであって、厚みが10~350μmであり、一方の面の十点平均粗さRz値が2μm未満であり、該表面の摩擦角が31°より大きく40°以下であり、かつ、他方の面の十点平均粗さRz値が2μm以上7μm以下であり、該表面の摩擦角が20°以上31°以下であり、
前記十点平均粗さRz値がJIS B0601-1994に準拠して測定した値であり、
前記摩擦角がJIS P 8147に記載の傾斜法に準処して測定した値であり、
前記ポリビニルアセタール樹脂材料中のポリビニルアセタール樹脂の、ブルックフィールド型(B型)粘度計を用いて20℃、30rpmで測定された、濃度10質量%のトルエン/エタノール=1/1(質量比)溶液の粘度が100~1000mPa・sであり、ポリビニルアセタール樹脂フィルム中の可塑剤の量がポリビニルアセタール樹脂フィルムの総質量に基づいて0~20質量%である、ポリビニルアセタール樹脂フィルム。 - 一方の面の摩擦角と他方の面の摩擦角との差分絶対値が2°以上10°以下である、請求項1に記載のポリビニルアセタール樹脂フィルム。
- 一方の面の十点平均粗さRz値と他方の面の十点平均粗さRz値との差分絶対値が1μm以上5μm以下である、請求項1または2に記載のポリビニルアセタール樹脂フィルム。
- 前記ポリビニルアセタール樹脂材料中のポリビニルアセタール樹脂の、ブルックフィールド型(B型)粘度計を用いて20℃、30rpmで測定された、濃度10質量%のトルエン/エタノール=1/1(質量比)溶液の粘度が300mPa・s以下である、請求項1~3のいずれかに記載のポリビニルアセタール樹脂フィルム。
- 前記ポリビニルアセタール樹脂材料中のポリビニルアセタール樹脂の、ブルックフィールド型(B型)粘度計を用いて20℃、30rpmで測定された、濃度10質量%のトルエン/エタノール=1/1(質量比)溶液の粘度が200mPa・sより大きい、請求項1~3のいずれかに記載のポリビニルアセタール樹脂フィルム。
- 前記ポリビニルアセタール樹脂材料中のポリビニルアセタール樹脂の分子量分布が2.7以上である、請求項1~5のいずれかに記載のポリビニルアセタール樹脂フィルム。
- 前記ポリビニルアセタール樹脂材料中のポリビニルアセタール樹脂が、粘度平均重合度の異なる少なくとも2つのポリビニルアセタール樹脂の混合物、または、粘度平均重合度の異なる少なくとも2つのポリビニルアルコール系樹脂の混合物のアセタール化物である、請求項1~6のいずれかに記載のポリビニルアセタール樹脂フィルム。
- 複数の透明基材の間に、請求項1~7のいずれかに記載のポリビニルアセタール樹脂フィルムが挟持されてなる、積層体。
- さらに可塑化ポリビニルアセタール樹脂層を含む、請求項8に記載の積層体。
- 前記透明基材がガラスである、請求項8または9に記載の積層体。
- 請求項8~10のいずれかに記載の積層体からなる乗物用ガラス。
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JP2011152693A (ja) | 2010-01-27 | 2011-08-11 | Konica Minolta Opto Inc | 樹脂フィルム基板とその製造方法 |
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