JP5174280B2 - ポリビニルアセタールフィルムおよびその用途 - Google Patents
ポリビニルアセタールフィルムおよびその用途 Download PDFInfo
- Publication number
- JP5174280B2 JP5174280B2 JP2012509545A JP2012509545A JP5174280B2 JP 5174280 B2 JP5174280 B2 JP 5174280B2 JP 2012509545 A JP2012509545 A JP 2012509545A JP 2012509545 A JP2012509545 A JP 2012509545A JP 5174280 B2 JP5174280 B2 JP 5174280B2
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- JP
- Japan
- Prior art keywords
- polyvinyl acetal
- film
- less
- resin
- acetal film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229920002554 vinyl polymer Polymers 0.000 title claims abstract description 155
- DHKHKXVYLBGOIT-UHFFFAOYSA-N acetaldehyde Diethyl Acetal Natural products CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 title claims abstract description 147
- 125000002777 acetyl group Chemical class [H]C([H])([H])C(*)=O 0.000 title 1
- 150000001241 acetals Chemical class 0.000 claims abstract description 83
- 239000002253 acid Substances 0.000 claims abstract description 81
- 239000011354 acetal resin Substances 0.000 claims abstract description 66
- 229920006324 polyoxymethylene Polymers 0.000 claims abstract description 66
- 239000004014 plasticizer Substances 0.000 claims abstract description 60
- 239000005340 laminated glass Substances 0.000 claims abstract description 57
- 125000004430 oxygen atom Chemical group O* 0.000 claims abstract description 30
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 23
- 239000000126 substance Substances 0.000 claims abstract description 15
- 229920005989 resin Polymers 0.000 claims description 74
- 239000011347 resin Substances 0.000 claims description 74
- 238000000034 method Methods 0.000 claims description 66
- 238000004519 manufacturing process Methods 0.000 claims description 53
- -1 nitrate ions Chemical class 0.000 claims description 33
- 239000011521 glass Substances 0.000 claims description 31
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 18
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 18
- 239000003513 alkali Substances 0.000 claims description 17
- 239000003054 catalyst Substances 0.000 claims description 13
- 239000011164 primary particle Substances 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229930195734 saturated hydrocarbon Natural products 0.000 claims description 10
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical group CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 9
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical group OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 5
- 229910002651 NO3 Inorganic materials 0.000 claims description 4
- 230000006837 decompression Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- 125000001183 hydrocarbyl group Chemical group 0.000 claims 4
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 125000002485 formyl group Chemical class [H]C(*)=O 0.000 claims 1
- 238000007493 shaping process Methods 0.000 claims 1
- 239000003566 sealing material Substances 0.000 abstract description 16
- 238000003475 lamination Methods 0.000 abstract description 14
- 239000010408 film Substances 0.000 description 132
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 63
- 238000006243 chemical reaction Methods 0.000 description 29
- 150000001299 aldehydes Chemical class 0.000 description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 19
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 18
- 238000004458 analytical method Methods 0.000 description 18
- 238000010030 laminating Methods 0.000 description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 15
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 13
- 230000007797 corrosion Effects 0.000 description 13
- 238000005260 corrosion Methods 0.000 description 13
- 238000010248 power generation Methods 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- 239000003963 antioxidant agent Substances 0.000 description 12
- 239000002245 particle Substances 0.000 description 12
- 230000014759 maintenance of location Effects 0.000 description 10
- 239000000178 monomer Substances 0.000 description 10
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 9
- 230000007062 hydrolysis Effects 0.000 description 9
- 229910052751 metal Inorganic materials 0.000 description 9
- 239000002184 metal Substances 0.000 description 9
- 150000003839 salts Chemical class 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- 239000005038 ethylene vinyl acetate Substances 0.000 description 8
- 238000006460 hydrolysis reaction Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 8
- 239000000758 substrate Substances 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 7
- 230000003078 antioxidant effect Effects 0.000 description 7
- 238000009835 boiling Methods 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- 239000000155 melt Substances 0.000 description 7
- 235000011121 sodium hydroxide Nutrition 0.000 description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 150000002430 hydrocarbons Chemical group 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 238000005979 thermal decomposition reaction Methods 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
- 239000006096 absorbing agent Substances 0.000 description 5
- 239000003377 acid catalyst Substances 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 229920001567 vinyl ester resin Polymers 0.000 description 5
- OBETXYAYXDNJHR-UHFFFAOYSA-N 2-Ethylhexanoic acid Chemical compound CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 4
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 4
- FBXNUYNATQIVEX-UHFFFAOYSA-N bis[2-(2-butoxyethoxy)ethyl] decanedioate Chemical compound CCCCOCCOCCOC(=O)CCCCCCCCC(=O)OCCOCCOCCCC FBXNUYNATQIVEX-UHFFFAOYSA-N 0.000 description 4
- SHZIWNPUGXLXDT-UHFFFAOYSA-N caproic acid ethyl ester Natural products CCCCCC(=O)OCC SHZIWNPUGXLXDT-UHFFFAOYSA-N 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- HHECSPXBQJHZAF-UHFFFAOYSA-N dihexyl hexanedioate Chemical compound CCCCCCOC(=O)CCCCC(=O)OCCCCCC HHECSPXBQJHZAF-UHFFFAOYSA-N 0.000 description 4
- 239000005329 float glass Substances 0.000 description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 4
- 239000011229 interlayer Substances 0.000 description 4
- 229910017604 nitric acid Inorganic materials 0.000 description 4
- 239000002530 phenolic antioxidant Substances 0.000 description 4
- 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 4
- 238000007127 saponification reaction Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 4
- 229910001887 tin oxide Inorganic materials 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 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 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- 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
- 238000006359 acetalization reaction Methods 0.000 description 3
- 229940067597 azelate Drugs 0.000 description 3
- IHTSDBYPAZEUOP-UHFFFAOYSA-N bis(2-butoxyethyl) hexanedioate Chemical compound CCCCOCCOC(=O)CCCCC(=O)OCCOCCCC IHTSDBYPAZEUOP-UHFFFAOYSA-N 0.000 description 3
- TUOSWEIWIXJUAU-UHFFFAOYSA-N bis(7-methyloctyl) cyclohexane-1,1-dicarboxylate Chemical compound CC(C)CCCCCCOC(=O)C1(C(=O)OCCCCCCC(C)C)CCCCC1 TUOSWEIWIXJUAU-UHFFFAOYSA-N 0.000 description 3
- SCABKEBYDRTODC-UHFFFAOYSA-N bis[2-(2-butoxyethoxy)ethyl] hexanedioate Chemical compound CCCCOCCOCCOC(=O)CCCCC(=O)OCCOCCOCCCC SCABKEBYDRTODC-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 238000005401 electroluminescence Methods 0.000 description 3
- 150000002484 inorganic compounds Chemical class 0.000 description 3
- 229910010272 inorganic material Inorganic materials 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- 230000000379 polymerizing effect Effects 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 238000004448 titration Methods 0.000 description 3
- 239000013638 trimer Substances 0.000 description 3
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- UZKWTJUDCOPSNM-UHFFFAOYSA-N 1-ethenoxybutane Chemical compound CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 2
- RKMGAJGJIURJSJ-UHFFFAOYSA-N 2,2,6,6-tetramethylpiperidine Chemical compound CC1(C)CCCC(C)(C)N1 RKMGAJGJIURJSJ-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000007983 Tris buffer Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 description 2
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000000539 dimer Substances 0.000 description 2
- FJKIXWOMBXYWOQ-UHFFFAOYSA-N ethenoxyethane Chemical compound CCOC=C FJKIXWOMBXYWOQ-UHFFFAOYSA-N 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000003988 headspace gas chromatography Methods 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- JARKCYVAAOWBJS-UHFFFAOYSA-N hexanal Chemical compound CCCCCC=O JARKCYVAAOWBJS-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 150000007522 mineralic acids Chemical class 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 description 2
- 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
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 2
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 2
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 description 2
- 238000004383 yellowing Methods 0.000 description 2
- YEYCMBWKTZNPDH-UHFFFAOYSA-N (2,2,6,6-tetramethylpiperidin-4-yl) benzoate Chemical compound C1C(C)(C)NC(C)(C)CC1OC(=O)C1=CC=CC=C1 YEYCMBWKTZNPDH-UHFFFAOYSA-N 0.000 description 1
- FEODVXCWZVOEIR-UHFFFAOYSA-N (2,4-ditert-butylphenyl) octyl hydrogen phosphite Chemical compound CCCCCCCCOP(O)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C FEODVXCWZVOEIR-UHFFFAOYSA-N 0.000 description 1
- PYLMCYQHBRSDND-VURMDHGXSA-N (Z)-2-ethyl-2-hexenal Chemical compound CCC\C=C(\CC)C=O PYLMCYQHBRSDND-VURMDHGXSA-N 0.000 description 1
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 1
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical group C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 description 1
- LAYAKLSFVAPMEL-UHFFFAOYSA-N 1-ethenoxydodecane Chemical compound CCCCCCCCCCCCOC=C LAYAKLSFVAPMEL-UHFFFAOYSA-N 0.000 description 1
- QJJDJWUCRAPCOL-UHFFFAOYSA-N 1-ethenoxyoctadecane Chemical compound CCCCCCCCCCCCCCCCCCOC=C QJJDJWUCRAPCOL-UHFFFAOYSA-N 0.000 description 1
- OVGRCEFMXPHEBL-UHFFFAOYSA-N 1-ethenoxypropane Chemical compound CCCOC=C OVGRCEFMXPHEBL-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
- DRIYOCKHMMVWAT-UHFFFAOYSA-N 2,3,5-tritert-butyl-4-hydroxy-6-phenylbenzoic acid Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=C(C(C)(C)C)C(C(O)=O)=C1C1=CC=CC=C1 DRIYOCKHMMVWAT-UHFFFAOYSA-N 0.000 description 1
- BSYJHYLAMMJNRC-UHFFFAOYSA-N 2,4,4-trimethylpentan-2-ol Chemical compound CC(C)(C)CC(C)(C)O BSYJHYLAMMJNRC-UHFFFAOYSA-N 0.000 description 1
- XJQMSHDKNMKUKH-UHFFFAOYSA-N 2,4-bis(octylsulfanyl)-1,3,5-triazine Chemical group CCCCCCCCSC1=NC=NC(SCCCCCCCC)=N1 XJQMSHDKNMKUKH-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
- BVUXDWXKPROUDO-UHFFFAOYSA-N 2,6-di-tert-butyl-4-ethylphenol Chemical compound CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 BVUXDWXKPROUDO-UHFFFAOYSA-N 0.000 description 1
- 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
- JRRSZPBVIHXNBS-UHFFFAOYSA-N 2-(2H-benzotriazol-4-yl)-4-(2,4,4-trimethylpentan-2-yl)phenol Chemical compound CC(C)(C)CC(C)(C)c1ccc(O)c(c1)-c1cccc2[nH]nnc12 JRRSZPBVIHXNBS-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
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- H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
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Description
本発明に使用されるポリビニルアセタール樹脂は、JIS K6728:1977年の規定に基づき測定したビニルアルコール単位量が12〜34モル%であることが好ましく、15〜32モル%がより好ましく、18〜30モル%がさらに好ましい。ビニルアルコール単位量が34モル%よりも多いと、吸湿性が高くなり、吸収した水による金属腐食や、絶縁性の低下、可塑化ポリビニルアセタールフィルムの基材からの剥離が起こる原因となるおそれがある。一方、ビニルアルコール量が12モル%よりも少ないと、力学的強度の低下、基材への接着性不良等の問題が生じるおそれがある。
本発明に使用される可塑剤において、分子を構成する炭素原子および酸素原子の総数は28以上であり、29よりも大きいことが好ましく、30よりも大きいことがさらに好ましく、31よりも大きいことが特に好ましい。可塑剤の分子を構成する炭素原子および酸素原子の総数が28未満である場合、熱分解や加水分解による酸価の上昇傾向が強くなって可塑化ポリビニルアセタールフィルム中の酸の濃度が高くなるおそれがある。また、真空ラミネーターの温度を高くしたり高真空にしたりすると可塑剤が揮発するため、ラミネート時間が長くなり、生産性が悪くなるとともに可塑化ポリビニルアセタールフィルム中の酸の濃度も高くなる。
本発明のある態様では、可塑化ポリビニルアセタールフィルムの酸価は、5.0meq/kg以下であることが必要であり、3.0meq/kg以下が好ましく、2.0meq/kg以下がより好ましく、1.5meq/kg以下がさらに好ましい。酸価が5.0meq/kgを超える場合、モジュール製造装置および得られる太陽電池や機能性合わせガラス中の金属成分の腐食原因となる。可塑化ポリビニルアセタールフィルムの酸価を5.0meq/kg以下とするためには、酸価が低いポリビニルアセタール樹脂および可塑剤を使用し、充分に乾燥させた状態で混合しできるだけ低温で溶融混練する方法があげられる。また、本発明の別の態様では、140℃で4時間加熱した後の可塑化ポリビニルアセタールフィルムの酸価が10.0meq/kg以下であることが必要であり、8.0meq/kg以下が好ましく、7.0meq/kg以下がより好ましい。ここで、酸価の測定方法は、JIS K6728:1977年の規定に記載の方法による。140℃で4時間加熱した後の可塑化ポリビニルアセタールフィルムの酸価を10.0meq/kg以下とするためには、酸価が低いポリビニルアセタール樹脂および可塑剤を使用することが好ましい。ここで、特にポリビニルアセタール樹脂は多孔質状で可塑剤吸収性に優れたもの、そして可塑剤は分子を構成する炭素原子と酸素原子の総数が28以上のものがそれぞれ好ましい。そして、このような原料を充分に乾燥させた状態で混合し、できるだけ低温で溶融混練する方法があげられる。また、適度に中和されていることも好ましく、具体的にはアルカリタイター値を前述の通りの値とすることが好ましい。
イオンの含有量は、50ppm以下であることが好ましく、25ppm以下がより好まし
い。これらの強酸イオンの含有量が50ppmを超えると、フィルムが着色したり、太陽
電池モジュール等に使用される金属成分が腐食するおそれがある。
JIS K6728:1977年の規定に基づき測定した。
JIS K6728:1977年の規定に基づき測定した。
PVB樹脂のエタノール溶液を塩酸で滴定し、100gのPVB樹脂あたりのアルカリ滴定に要する0.01モル/Lの塩酸量(アルカリタイター値:mL)で評価した。
JIS K6728:1977年の規定に基づき測定した。フィルムについては、試験管中、140℃で4時間加熱した後の酸価も同様に測定した。
島津製作所製ヘッドスペースガスクロマトグラフィーGC−14B、カラムはジーエルサイエンス株式会社製TC−1(内径0.25mm、長さ30m)を用いて測定した。
3%硝酸水溶液1mlに蒸留水10mlとエタノール80mlを加え、これにPVBフィルムサンプル約1gを精秤して加えた。攪拌してサンプルを溶解させた後、0.001モル/Lの硝酸銀水溶液を滴下し、電気伝導度の変化による滴定量からフィルム中の塩化物イオン濃度を求めた。なお、後述の実施例および比較例においては、PVB樹脂を作製する際のアセタール化触媒として塩酸のみを使用しているため、PVB樹脂またはフィルムにおける塩化物イオン量が、それぞれPVB樹脂またはフィルム中に含まれる塩化物イオン、硫酸イオンおよび硝酸イオンの含有量の合計量に相当する。
PVB樹脂の粒子形状は走査型電子顕微鏡(SEM)により観察した。また、PVB樹脂の一次粒子の平均粒子径は、走査型電子顕微鏡(SEM)を用い、樹脂を1000倍の倍率で3箇所(3枚)撮影して得られた写真から判定可能な一次粒子径を測定(写真1枚につき50点以上)し、その平均値を求めて平均粒子径とした。なお、一次粒子径の測定は、長径を対象にして行った。
攪拌機を取り付けた2m3反応器に、PVA(PVA−1:重合度1700、けん化度99モル%)の7.5質量%水溶液1700kgと、n−ブチルアルデヒド74.6kg、2,6−ジ−t−ブチル−4−メチルフェノール0.13kgを仕込み、全体を14℃に冷却した。これに、濃度20質量%の塩酸160.1Lを添加して、PVAのブチラール化を開始した。添加終了後から10分後に昇温を開始し、90分かけて65℃まで昇温し、さらに120分反応を行った。その後、室温まで冷却して析出した樹脂をろ過後、樹脂に対して10倍量のイオン交換水で10回洗浄した。その後、0.3質量%の水酸化ナトリウム水溶液を用いて充分に中和を行い、さらに樹脂に対して10倍量のイオン交換水で10回洗浄し、脱水した後、乾燥させ、PVB樹脂(PVB−1)を得た。SEMで観察された粒子形状は、図1に示すとおり、小さな一次粒子がその粒子形状をほぼ保ったままの集合体となっていた。得られたPVB樹脂の分析結果を表1に示す。
0.5質量%水酸化ナトリウム水溶液を中和に用いた以外は製造例1と同様にして、PVB樹脂(PVB−2)を得た。得られたPVB樹脂の分析結果を表1に示す。
攪拌機を取り付けた2m3反応器に、PVA−1の9.0質量%水溶液1700kgと、濃度20%の塩酸120.1Lを仕込み、全体を14℃に冷却した。これに、n−ブチルアルデヒド89.5kg、2,6−ジ−t−ブチル−4−メチルフェノール0.13kgを添加して、PVAのブチラール化を開始した。添加終了後から10分後に昇温を開始し、90分かけて65℃まで昇温し、さらに120分反応を行った。その後、室温まで冷却して析出した樹脂をろ過後、樹脂に対して10倍量のイオン交換水で10回洗浄した。その後、0.3質量%水酸化ナトリウム水溶液を用いて充分に中和を行い、さらに樹脂に対して10倍量のイオン交換水で10回洗浄し、脱水した後、乾燥させ、PVB樹脂(PVA−3)を得た。SEMで観察された粒子形状は、図2に示すとおり、一次粒子が融着し、一次粒子形状の形状が不明確となった集合体となっていた。得られたPVB樹脂の分析結果を表1に示す。
製造例1で得られたPVB樹脂(PVB−1)1kgに対し、パラメトキシフェノール1.0g、オリゴエチレングリコールジ(2−エチルヘキサノエート)(平均エチレングリコール連鎖長:9)(9GO;酸価0.4meq/kg)360gを添加し、小型二軸押出機を用いて厚さ760μm、幅50cmのPVBフィルム(F−1)を製造した。なお、押出機のベント口2つを真空ポンプに接続し、減圧により揮発成分を除去しながら行い、樹脂温度が200℃になるように調整した。分析結果を表2に示す。
可塑剤としてジ(2−ブトキシエトキシエチル)セバケート(DBEES;酸価0.7meq/kg)360gを用いた以外は実施例1と同様にしてPVBフィルム(F−2)を製造した。分析結果を表2に示す。
製造例2で得られたPVB樹脂(PVB−2)を用いた以外は実施例2と同様にしてPVBフィルム(F−3)を得た。分析結果を表2に示す。なお、該フィルムはF−1およびF−2に比べ、若干茶色く着色していた。
製造例3で得られたPVB樹脂(PVB−3)を用いた以外は実施例2と同様にしてPVBフィルム(F−4)を得た。分析結果を表2に示す。
可塑剤としてジ−n−ヘキシルアジペート(DHA;酸価0.8meq/kg)を使用した以外は、実施例1と同様にしてPVBフィルム(F−5)を製造した。分析結果を表2に示す。
上記の実施例1〜3、並びに、比較例1および2で得られたPVBフィルムを3mm厚のフロートガラス2枚にはさみ、真空バッグ法により合わせガラスを得た。この合わせガラスの黄色度(YI)を、色差計(スガ試験機株式会社製「SM−T」)を用いて測定した。
太陽電池モジュールの製造に使用される真空ラミネーター装置(株式会社エヌ・ピー・シー製)を用い、厚さ3mm、縦横50cmの2枚のガラスと、予め水分量を0.45質量%に調整したPVBフィルム(F−1、F−2およびF−3)を用いて合わせガラスのサンプルを作製した。試験は、まず、ラミネーター装置の設定温度を150℃にして、ガラス/PVBフィルム/ガラスの順で重ねたものをラミネートし、得られた合わせガラスの表面を目視により観察した。次いで、ラミネーター装置の設定温度を150℃から5℃ずつ上昇させながら、設定温度毎に、新たに合わせガラスを作製して表面を目視により観察するということを、合わせガラスのガラス表面に揮発分による汚れが発生する温度となるまで、繰り返し実施した。なお、試験は、設定温度ごとにF−1、F−2及びF−3のPVBフィルムを用いた合わせガラスを作製することで、3回ずつ行った。その他のラミネートの条件としては、減圧時の圧力100Pa、減圧時間10分、上部チャンバーを常圧に戻してさらに10分圧着させるものとした。そして、ラミネート温度160℃で得られた合わせガラスからPVBフィルムの一部を取り出し、JIS K6728:1977年の規定に基づき酸価を測定した。また、合わせガラス内に泡や汚れが発生しないラミネート温度の最高値を最高ラミネート温度とすると、実施例4では、最高ラミネート温度は170℃、実施例5および6では、最高ラミネート温度は160℃であった。結果を表3に示す。
PVBフィルム(F−4)を用いた以外は実施例4と同様にして合わせガラスのサンプルを作製し評価した。比較例3では、最高ラミネート温度は150℃であった。結果を表3に示す。
PVBフィルム(F−5)を用い、かつ試験の設定温度を140℃から5℃ずつ上昇させた以外は、実施例4と同様にして合わせガラスのサンプルを作製し、評価した。比較例4では、最高ラミネート温度は140℃であった。結果を表3に示す。
なお、上記の実施例4〜6、並びに比較例3および4で作製された、各ラミネート温度における合わせガラスの外観を肉眼で以下のように判定した。結果を表3に示す。
判定:基準
A :合わせガラス内の泡および揮発分による合わせガラス表面の汚れが見られない。
B :合わせガラス内に泡が見られる。
C :揮発分による合わせガラス表面の汚れが発生した。
攪拌機を取り付けた2m3反応器に、PVA−1の7.5質量%水溶液1700kgと、濃度20%の塩酸106.7Lを仕込み、全体を14℃に冷却した。これに、n−ブチルアルデヒド74.6kg、2,6−ジ−t−ブチル−4−メチルフェノール0.13kgを添加して、PVAのブチラール化を開始した。添加終了後から10分後に昇温を開始し、90分かけて65℃まで昇温し、さらに120分反応を行った。その後、室温まで冷却して析出した樹脂をろ過後、樹脂に対して10倍量のイオン交換水で5回洗浄した。その後、0.3質量%水酸化ナトリウム水溶液を用いて充分に中和を行い、さらに樹脂に対して10倍量のイオン交換水で10回洗浄し、脱水した後、乾燥させ、PVB樹脂(PVB−4)を得た。SEMで観察された粒子形状は、図3に示すとおり、PVB−1よりも若干大きな一次粒子がその粒子形状をほぼ保ったままの集合体となっていた。得られたPVB樹脂の分析結果を表4に示す。
2,6−ジ−t−ブチル−4−メチルフェノールを添加しなかった以外は製造例3と同様にして、PVB樹脂(PVB−5)を得た。得られたPVB樹脂の分析結果を表4に示す。
ブチルアルデヒドの仕込み量を69.9kgとした以外は製造例1と同様にして、PVB樹脂(PVB−6)を得た。得られたPVB樹脂の分析結果を表4に示す。
可塑剤としてトリエチレングリコールジ(2−エチルヘキサノエート)(3GO;酸価0.5meq/kg)360gを用いた以外は実施例1と同様にして、PVBフィルム(F−6)を製造した。分析結果を表5に示す。
製造例4で得られたPVB樹脂(PVB−4)を用い、可塑剤としてジ(2−ブトキシエトキシエチル)アジペート(DBEEA;酸価0.3meq/kg)を用いた以外は、実施例1と同様にしてPVBフィルム(F−7)を製造した。分析結果を表5に示す。
可塑剤として、原料由来の酸が不純物として多く含まれる3GO(酸価3.9meq/kg)を使用した以外は、実施例7と同様にしてPVBフィルム(F−8)を製造した。分析結果を表5に示す。
押出機温度を樹脂温度が230℃となるように調整した以外は、実施例7と同様にして
PVBフィルム(F−9)を製造した。分析結果を表5に示す。
押出機に設置されている2つのベント口の内、一つを封鎖して行った以外は、実施例7と同様にしてPVBフィルム(F−10)を製造した。分析結果を表5に示す。
製造例5で得られたPVB樹脂(PVB−5)を用いた以外は、実施例7と同様にしてPVBフィルム(F−11)を製造した。分析結果を表5に示す。
製造例6で得られたPVB樹脂(PVB−6)を用い、可塑剤としてジブチルアジペート(DBA;酸価0.4meq/kg)を使用した以外は、実施例1と同様にしてPVBフィルム(F−12)を製造した。分析結果を表5に示す。
上記の実施例7および8、並びに、比較例5〜9で得られたPVBフィルムを3mm厚のフロートガラス2枚にはさみ、真空バッグ法により合わせガラスを得た。この合わせガラスの黄色度(YI)を、色差計(スガ試験機株式会社製「SM−T」)を用いて測定した。
実施例1で得たフィルムF−1(縦横30cm)を、バスバー電極が取り付けられたa−Si太陽電池セルが設置された、厚さ3mm、縦横30cmのフロートガラスと、もう1枚の同じ厚み、大きさのガラスとの間に配して真空ラミネーターを用いて封止し、さらうにジャンクションボックスを取り付け太陽電池モジュールとした。得られた太陽電池モジュールについて85℃、85%RH、1000時間の条件でダンプヒート試験を行い、試験前後での発電効率保持率を算出した。実施例9の太陽電池モジュールにおける発電効率保持率は97%であった。
フィルムF−1の代わりに実施例2で得たフィルムF−2を用いたこと以外は実施例9と同様にしてダンプヒート試験前後の発電効率保持率を算出した。発電効率保持率は97%であった。
フィルムF−1の代わりに実施例7で得たフィルムF−6を用いた以外は実施例9と同様にしてダンプヒート試験前後の発電効率保持率を算出した。発電効率保持率は95%であった。
フィルムF−1の代わりに比較例5で得たフィルムF−8を用いた以外は実施例9と同様にしてダンプヒート試験前後の発電効率保持率を算出した。発電効率保持率は92%であった。
フィルムF−1の代わりに比較例8で得たフィルムF−11を用いた以外は実施例9と同様にしてダンプヒート試験前後の発電効率保持率を算出した。発電効率保持率は85%であった。
Claims (20)
- ビニルアルコール単位量が12〜34モル%であり、酢酸ビニル単位量が4モル%以下であるポリビニルアセタール樹脂100質量部に対し、分子を構成する炭素原子および酸素原子の総数が28以上で、且つ、下記化学式(1):
- ビニルアルコール単位量が12〜34モル%であり、酢酸ビニル単位量が4モル%以下であるポリビニルアセタール樹脂100質量部に対し、分子を構成する炭素原子および酸素原子の総数が28以上で、且つ、下記化学式(1):
- フィルムの酸価が5.0meq/kg以下である請求項2に記載の可塑化ポリビニルアセタールフィルム。
- 可塑剤の分子を構成する炭素原子および酸素原子の総数が29よりも大きい、請求項1〜3のいずれかに記載の可塑化ポリビニルアセタールフィルム。
- 塩化物イオン、硫酸イオンおよび硝酸イオンの含有量が合計50ppm以下である、請求項1〜4のいずれかに記載の可塑化ポリビニルアセタールフィルム。
- ポリビニルアセタール樹脂の酸価が3.0meq/kg以下であり、可塑剤の酸価が10.0meq/kg以下である、請求項1〜5のいずれかに記載の可塑化ポリビニルアセタールフィルム。
- 140℃で4時間加熱した後の酸価が10.0meq/kg以下である請求項1に記載の可塑化ポリビニルアセタールフィルム。
- 請求項1〜7のいずれかに記載の可塑化ポリビニルアセタールフィルムを製造する製造方法であって、ポリビニルアセタール樹脂100質量部に対し、分子を構成する炭素原子および酸素原子の総数が28以上の可塑剤15〜60質量部を混合し、成形することを特徴とする、可塑化ポリビニルアセタールフィルムの製造方法。
- 可塑剤の分子を構成する炭素原子および酸素原子の総数が29よりも大きい、請求項8に記載の可塑化ポリビニルアセタールフィルムの製造方法。
- 前記ポリビニルアセタール樹脂の平均一次粒子径が10μm以下である、請求項8または9に記載の可塑化ポリビニルアセタールフィルムの製造方法。
- 前記ポリビニルアセタール樹脂のアルカリタイター値が0.1〜30であり、酸価が3.0meq/kg以下である、請求項8〜10のいずれかに記載の可塑化ポリビニルアセタールフィルムの製造方法。
- 前記ポリビニルアセタール樹脂の塩化物イオン、硫酸イオンおよび硝酸イオンの含有量が合計100ppm以下である、請求項8〜11のいずれかに記載の可塑化ポリビニルアセタールフィルムの製造方法。
- 前記ポリビニルアセタール樹脂が、ポリビニルアルコール樹脂の水溶液に、アルデヒド類を先に添加した後に触媒を添加することで得られたものである、請求項8〜12のいずれかに記載の可塑化ポリビニルアセタールフィルムの製造方法。
- 酸価が3.0meq/kg以下であるポリビニルアセタール樹脂に対し、酸価が10.0meq/kg以下である可塑剤を混合し、成形することを特徴とする、請求項8〜13のいずれかに記載の可塑化ポリビニルアセタールフィルムの製造方法。
- 減圧により揮発成分を除去しながらポリビニルアセタール樹脂と可塑剤を混合する、請求項8〜14のいずれかに記載の可塑化ポリビニルアセタールフィルムの製造方法。
- 成形時の樹脂温度が150〜220℃の範囲である、請求項8〜15のいずれかに記載の可塑化ポリビニルアセタールフィルムの製造方法。
- 請求項1〜7のいずれかに記載の可塑化ポリビニルアセタールフィルムを用いた太陽電池モジュール。
- さらに透明導電膜層を有するガラスを備える請求項17に記載の太陽電池モジュール。
- 請求項1〜7のいずれかに記載の可塑化ポリビニルアセタールフィルムを用いた合わせガラス。
- 前記可塑化ポリビニルアセタールフィルムと接する位置に機能性ユニットを備える請求項19に記載の合わせガラス。
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KR20130051925A (ko) | 2013-05-21 |
US9676930B2 (en) | 2017-06-13 |
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US9988507B2 (en) | 2018-06-05 |
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