TWI637007B - Resin composition, curable resin composition, adhesive for lamination, and back sheet for solar cell - Google Patents
Resin composition, curable resin composition, adhesive for lamination, and back sheet for solar cell Download PDFInfo
- Publication number
- TWI637007B TWI637007B TW103130687A TW103130687A TWI637007B TW I637007 B TWI637007 B TW I637007B TW 103130687 A TW103130687 A TW 103130687A TW 103130687 A TW103130687 A TW 103130687A TW I637007 B TWI637007 B TW I637007B
- Authority
- TW
- Taiwan
- Prior art keywords
- resin composition
- polyester polyol
- acid
- adhesive
- molecular weight
- Prior art date
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- 239000011342 resin composition Substances 0.000 title claims abstract description 43
- 239000000853 adhesive Substances 0.000 title claims abstract description 35
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 33
- 238000003475 lamination Methods 0.000 title abstract description 8
- 229920005906 polyester polyol Polymers 0.000 claims abstract description 68
- -1 alkylene glycol Chemical compound 0.000 claims abstract description 33
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 29
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 239000011347 resin Substances 0.000 claims abstract description 21
- 238000009826 distribution Methods 0.000 claims abstract description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims abstract description 12
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims abstract description 11
- 125000004432 carbon atom Chemical group C* 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims description 33
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 32
- 239000004593 Epoxy Substances 0.000 claims description 18
- 239000005056 polyisocyanate Substances 0.000 claims description 15
- 229920001228 polyisocyanate Polymers 0.000 claims description 15
- 229920000515 polycarbonate Polymers 0.000 claims description 12
- 239000004417 polycarbonate Substances 0.000 claims description 12
- 239000012939 laminating adhesive Substances 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 9
- 229920000728 polyester Polymers 0.000 claims description 8
- 239000012790 adhesive layer Substances 0.000 claims description 6
- 229920005862 polyol Polymers 0.000 claims description 6
- 150000003077 polyols Chemical class 0.000 claims description 6
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 5
- 229910052731 fluorine Inorganic materials 0.000 claims description 5
- 239000011737 fluorine Substances 0.000 claims description 5
- 239000004848 polyfunctional curative Substances 0.000 claims description 5
- 125000003118 aryl group Chemical group 0.000 claims description 4
- 229920000098 polyolefin Polymers 0.000 claims description 3
- 239000011888 foil Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229920006267 polyester film Polymers 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 229920002635 polyurethane Polymers 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 17
- 239000003795 chemical substances by application Substances 0.000 abstract description 13
- 238000012545 processing Methods 0.000 abstract description 7
- 238000012360 testing method Methods 0.000 abstract description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 27
- 239000000758 substrate Substances 0.000 description 18
- 238000003756 stirring Methods 0.000 description 16
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 14
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 13
- 238000011156 evaluation Methods 0.000 description 13
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 12
- 239000003822 epoxy resin Substances 0.000 description 12
- 229920000647 polyepoxide Polymers 0.000 description 12
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 11
- 239000010410 layer Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 11
- 239000007787 solid Substances 0.000 description 11
- 238000005886 esterification reaction Methods 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 8
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 8
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 7
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 description 7
- 238000001816 cooling Methods 0.000 description 7
- 238000005227 gel permeation chromatography Methods 0.000 description 7
- 239000002985 plastic film Substances 0.000 description 7
- 229920006255 plastic film Polymers 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 238000003786 synthesis reaction Methods 0.000 description 7
- 150000003609 titanium compounds Chemical class 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- 150000002009 diols Chemical class 0.000 description 6
- 239000005038 ethylene vinyl acetate Substances 0.000 description 6
- 230000009477 glass transition Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 6
- 229930185605 Bisphenol Natural products 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 229920005668 polycarbonate resin Polymers 0.000 description 5
- 239000004431 polycarbonate resin Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 4
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- GHVNFZFCNZKVNT-UHFFFAOYSA-N decanoic acid Chemical compound CCCCCCCCCC(O)=O GHVNFZFCNZKVNT-UHFFFAOYSA-N 0.000 description 4
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 description 4
- SRPWOOOHEPICQU-UHFFFAOYSA-N trimellitic anhydride Chemical compound OC(=O)C1=CC=C2C(=O)OC(=O)C2=C1 SRPWOOOHEPICQU-UHFFFAOYSA-N 0.000 description 4
- LWBHHRRTOZQPDM-UHFFFAOYSA-N undecanedioic acid Chemical compound OC(=O)CCCCCCCCCC(O)=O LWBHHRRTOZQPDM-UHFFFAOYSA-N 0.000 description 4
- QFGCFKJIPBRJGM-UHFFFAOYSA-N 12-[(2-methylpropan-2-yl)oxy]-12-oxododecanoic acid Chemical compound CC(C)(C)OC(=O)CCCCCCCCCCC(O)=O QFGCFKJIPBRJGM-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000004793 Polystyrene Substances 0.000 description 3
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 150000001721 carbon Chemical group 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 229910052802 copper Inorganic materials 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 125000003700 epoxy group Chemical group 0.000 description 3
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 3
- 229910052738 indium Inorganic materials 0.000 description 3
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 150000007519 polyprotic acids Polymers 0.000 description 3
- 229920002223 polystyrene Polymers 0.000 description 3
- 229920002620 polyvinyl fluoride Polymers 0.000 description 3
- 238000010248 power generation Methods 0.000 description 3
- 229910052711 selenium Inorganic materials 0.000 description 3
- 239000011669 selenium Substances 0.000 description 3
- 150000005846 sugar alcohols Polymers 0.000 description 3
- ARCGXLSVLAOJQL-UHFFFAOYSA-N trimellitic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C(C(O)=O)=C1 ARCGXLSVLAOJQL-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 2
- JCTXKRPTIMZBJT-UHFFFAOYSA-N 2,2,4-trimethylpentane-1,3-diol Chemical compound CC(C)C(O)C(C)(C)CO JCTXKRPTIMZBJT-UHFFFAOYSA-N 0.000 description 2
- MARUHZGHZWCEQU-UHFFFAOYSA-N 5-phenyl-2h-tetrazole Chemical compound C1=CC=CC=C1C1=NNN=N1 MARUHZGHZWCEQU-UHFFFAOYSA-N 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- 239000005632 Capric acid (CAS 334-48-5) Substances 0.000 description 2
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 2
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 2
- 239000005057 Hexamethylene diisocyanate Substances 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 239000002033 PVDF binder Substances 0.000 description 2
- BTZVDPWKGXMQFW-UHFFFAOYSA-N Pentadecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCCC(O)=O BTZVDPWKGXMQFW-UHFFFAOYSA-N 0.000 description 2
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 150000007933 aliphatic carboxylic acids Chemical class 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 125000002947 alkylene group Chemical group 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 239000004305 biphenyl Substances 0.000 description 2
- 235000010290 biphenyl Nutrition 0.000 description 2
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
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- 238000001914 filtration Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 229910052733 gallium Inorganic materials 0.000 description 2
- KEMQGTRYUADPNZ-UHFFFAOYSA-N heptadecanoic acid Chemical compound CCCCCCCCCCCCCCCCC(O)=O KEMQGTRYUADPNZ-UHFFFAOYSA-N 0.000 description 2
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- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
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- 239000011229 interlayer Substances 0.000 description 2
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- 229910052746 lanthanum Inorganic materials 0.000 description 2
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- 239000000463 material Substances 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 description 2
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 description 2
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- 239000003566 sealing material Substances 0.000 description 2
- HQHCYKULIHKCEB-UHFFFAOYSA-N tetradecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCCC(O)=O HQHCYKULIHKCEB-UHFFFAOYSA-N 0.000 description 2
- 229920005992 thermoplastic resin Polymers 0.000 description 2
- DXNCZXXFRKPEPY-UHFFFAOYSA-N tridecanedioic acid Chemical compound OC(=O)CCCCCCCCCCCC(O)=O DXNCZXXFRKPEPY-UHFFFAOYSA-N 0.000 description 2
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- WBODDOZXDKQEFS-UHFFFAOYSA-N 1,2,3,4-tetramethyl-5-phenylbenzene Chemical group CC1=C(C)C(C)=CC(C=2C=CC=CC=2)=C1C WBODDOZXDKQEFS-UHFFFAOYSA-N 0.000 description 1
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- 229940093475 2-ethoxyethanol Drugs 0.000 description 1
- XPFCZYUVICHKDS-UHFFFAOYSA-N 3-methylbutane-1,3-diol Chemical compound CC(C)(O)CCO XPFCZYUVICHKDS-UHFFFAOYSA-N 0.000 description 1
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- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 1
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Abstract
提供一種聚酯多元醇、使用其之樹脂組成物、含有該樹脂組成物而成之2液型積層用接著劑、及太陽能電池之背板;該聚酯多元醇在作為積層接著劑用之主劑而使用之情形,硬化後的接著強度高,於所謂耐濕熱性試驗中接著強度不劣化之經時穩定性優良,且於積層加工後的外觀亦優良。
使用一種聚酯多元醇作為2液型積層用接著劑的主成分,其特徵為:具有使分枝伸烷二醇、碳原子數8~20的長鏈脂肪族二羧酸、芳香族三羧酸反應所得之樹脂結構,且重量平均分子量(Mw)在10,000~100,000之範圍,分子量分布(Mw/Mn)在3.0~4.7之範圍。
Description
本發明係關於在濕熱條件下之基材接著性與耐紫外線性優良的太陽能電池用背板、作為該背板用接著劑有用之積層用接著劑、構成該積層用接著劑之硬化性樹脂組成物、構成其主劑之聚酯多元醇及積層接著劑用多元醇劑、以及樹脂組成物。
近年來,以石油、煤炭為首之石化燃料有枯竭的危機,而為了確保由這些石化燃料所能得到之替代能源的開發則成為當務之急。這些石化燃料之替代能源中,能將太陽光能直接轉換為電能之太陽光發電,正逐漸被實用化來作為半永久性且無公害的新能源來源,已展開在實際利用上的性價比之提升,作為清淨能源來源受到非常高的期望。
太陽光發電所使用之太陽能電池,係構成將太陽光的能量直接轉換為電能之太陽光發電系統的心臓部者,由矽等所代表之半導體所構成,其構造係將太陽能電池元件串聯、並聯配線,且為了保護該元件施以各種封裝而單元化。此種被組合在封裝內的單元被稱為太陽能電池模組,一般係成為以玻璃覆蓋太陽光照射之
面,以包含熱塑性樹脂之填充材料填補間隙,以密封片保護背面的結構。作為包含熱塑性樹脂之填充材料,由於所謂透明性高、耐濕性亦優良的理由,多數使用乙烯-乙酸乙烯酯共聚樹脂。另一方面,背面保護板(背板)係要求機械強度、耐候性、耐熱性、耐濕熱性、耐光性等特性。由於此種太陽能電池模組通常係跨30年左右之長期而於室外使用,對於構成背板之接著劑要求具長期信賴性之接著強度,具體來說,係以高水準而被要求對於聚酯膜或聚氟乙烯膜等具有不同特徵之各種薄膜的高接著性、或用以在即使是露天環境下也長期地維持接著性的耐濕熱性。
作為此種背板用接著劑,已知有例如將使用了芳香族二元酸、C9以上的脂肪族羧酸、及C5以上的脂肪族醇類作為原料單體之高分子量聚酯多元醇,與低分子量聚酯聚胺甲酸酯多元醇併用作為主劑,且使用聚異氰酸酯化合物作為硬化劑,藉以提高源自芳香族二元酸之樹脂的凝集力,且藉由長鏈脂肪族醇類而伸長酯鍵間距離以抑制水分浸入、改善耐濕熱性,並同時藉由併用低分子量胺甲酸酯而改善塗布性、潤濕性之技術(例如參照專利文獻1)。
然而,前述專利文獻1記載之接著劑,由於係使用將C9以上的脂肪族羧酸用作為原料之聚酯多元醇,所以雖然耐濕熱性被某程度地改善但還不到充分的水準,也還有所謂硬化後的塗膜強度弱、且積層加工後的薄膜外觀之平滑性差的問題。
專利文獻1 日本專利第4416047號公報
因此,本發明所欲解決之課題在於提供一種聚酯多元醇,在使用其作為積層接著劑用的主劑之情形,硬化後的接著強度高、所謂於耐濕熱性試驗的接著強度不會劣化之經時穩定性優良,且積層加工後的外觀亦優良;並提供使用其之樹脂組成物、含有該樹脂組成物而成之2液型積層用接著劑、及太陽能電池之背板。
本發明人們為了解決上述課題而不斷戮力研究的結果,發現了具有使分枝伸烷二醇、碳原子數8~20的長鏈脂肪族二羧酸、芳香族三羧酸進行反應所得到之樹脂結構,且具既定之重量平均分子量範圍、分子量分布的聚酯多元醇,係於其本身的耐濕性優良之同時,在將其使用在太陽能電池用背板的外部薄膜用接著劑之主劑的情形,於硬化後的接著強度提升之同時,在濕熱條件下的經時變化也變少,且在積層加工後,片材外觀亦優良,乃至完成本發明。
即,本發明係提供一種聚酯多元醇,其特徵為:具有使分枝伸烷二醇、碳原子數8~20的長鏈脂肪族二羧酸、芳香族三羧酸反應所得之樹脂結構,且重量
平均分子量(Mw)在10,000~100,000之範圍,及分子量分布(Mw/Mn)在3.0~4.7之範圍。
本發明進一步提供一種2液型積層接著劑用多元醇劑,其係包含前述聚酯多元醇。
本發明進一步提供一種樹脂組成物,其係以前述聚酯多元醇及多官能環氧化合物作為必須成分。
本發明進一步提供一種硬化性樹脂組成物,其係使用聚酯二醇或前述樹脂組成物作為主劑,且摻合脂肪族聚異氰酸酯作為硬化劑。
本發明進一步提供一種2液型積層用接著劑,其係包含硬化性樹脂組成物。
本發明進一步提供一種太陽能電池用背板,其係由選自包含聚酯膜、氟系樹脂膜、聚烯烴膜及金屬箔之群組中的1種以上之薄膜,與包含用以貼合此等薄膜彼此的2液型積層用接著劑之接著層所形成。
如依據本發明,則能提供一種在使用作為積層接著劑用的主劑之情形,硬化後的接著強度高,所謂於耐濕熱性試驗中接著強度不會劣化之經時穩定性優良,且積層加工後的外觀亦優良的聚酯多元醇,一種使用其之樹脂組成物、一種含有該樹脂組成物而成之2液型積層用接著劑、及一種太陽能電池之背板。
第1圖係於實施例2所得到之聚酯多元醇(A2)的GPC圖。
第2圖係於實施例2所得到之聚酯多元醇(A2)的紅外線吸收光譜圖。
本發明之聚酯多元醇係作為太陽能電池用背板接著劑的主劑之2液型積層接著劑用多元醇劑為有用之物,係將分枝伸烷二醇、與碳原子數8~20的長鏈脂肪族二羧酸、與芳香族三羧酸作為必須的原料成分,而反應所得。
此處,由於使用分枝伸烷二醇作為原料,而所得到之聚酯多元醇的耐水解性飛躍性地提升,且能得到在用於積層接著劑之情形的初期接著性與耐濕熱後的接著性之變化少的耐濕熱性優良之接著劑。此種分枝伸烷二醇具體而言係其分子結構內具有3級碳原子或4級碳原子之伸烷二醇,可列舉出例如:1,2,2-三甲基-1,3-丙二醇、2,2-二甲基-3-異丙基-1,3-丙二醇、3-甲基-1,3-丁二醇、3-甲基-1,5-戊二醇、新戊二醇、1,4-雙(羥甲基)環己烷、2,2,4-三甲基-1,3-戊二醇等。這些之中特別從耐濕熱性優良的點來看,較佳為新戊二醇。
又,由於使用碳原子數8~20的長鏈脂肪族二羧酸,而所得到之聚酯多元醇的黏度減低,除了能使對基材的密著性提升以外,聚酯多元醇之黏度被減低,在使用作為積層接著劑之情形,積層加工後的片材外觀係提升。
此種碳原子數8~20之長鏈脂肪族二羧酸可列舉出:辛二酸、庚二酸、癸二酸、十一烷二酸、十二烷二酸、十三烷二酸、十四烷二酸、十五烷二酸、十六烷二酸、十七烷二酸、十八烷二酸、十九烷二酸、二十烷二酸等。
此等當中,特別從對前述基材的密著性改善效果顯著的點來看,特佳為如辛二酸、庚二酸、癸二酸、十一烷二酸、十二烷二酸、十三烷二酸、1,2,5-己三酸、1,2,4-環己三酸之碳原子數在8~13之範圍的脂肪族多元酸。
接下來,藉由使用芳香族三羧酸,而除了硬化物的耐熱性變好以外,所得到之聚酯多元醇的分子量分布變寬,對基材的密著性提升,在使用作為積層接著劑之情形的耐濕熱性變好。此種芳香族三羧酸,具體來說可列舉出:如苯偏三酸、苯偏三酸酐、1,2,5-苯三甲酸、2,5,7-萘三甲酸、焦蜜石酸二酐之芳香族三元酸及其酸酐等。
本發明之聚酯多元醇,係將以上詳述之分枝伸烷二醇、碳原子數8~20之長鏈脂肪族二羧酸、及芳香族三羧酸作為必須的原料成分而進行反應所得之物,以提升作為接著劑之柔軟性、潤濕性之目的,而在不損及本發明之效果的範圍內,可於上述各原料成分進一步併用乙二醇、1,3-丙二醇、1,4-丁二醇、1,6-己二醇、1,8-壬二醇、二乙二醇等直鏈狀烷二醇,又,也可併用三羥甲基丙烷等含有分枝烷結構之3官能醇。並且,在使用
含有分枝烷結構之3官能醇的情形,從不會引起過度的高黏度化,且能得到適度的分枝結構之點來看,較佳使分枝伸烷二醇與含有分枝烷結構之3官能醇的比例成為質量比[分枝烷二醇/含有分枝烷結構之3官能醇]為90/10~99/1。
此外,本發明中作為羧酸成分,除了前述碳原子數8~20的長鏈脂肪族二羧酸以外,以調整最終所得到之新聚酯多元醇的分子量與黏度作為目的,也可併用如甲酸、乙酸、丙酸、丁酸、戊酸、己酸、庚酸、辛酸、壬酸、癸酸、十二烷酸、十四烷酸、十六烷酸、十七烷酸、十八烷酸、苯甲酸之一元羧酸。
由上述各成分來製造本發明之聚酯多元醇的方法,可舉出例如:使以分枝伸烷二醇、碳原子數8~20的長鏈脂肪族二羧酸、及芳香族三羧酸為必須的原料成分,在酯化觸媒的存在下,於150~270℃之溫度範圍進行反應之方法等。此處所使用之酯化觸媒可列舉出例如:有機錫化合物、無機錫化合物、有機鈦化合物、有機鋅化合物等。
如此地進行所得到之聚酯多元醇,特徵為其重量平均分子量(Mw)在10,000~100,000之範圍,且分子量分布(Mw/Mn)在3.0~4.7之範圍。在重量平均分子量(Mw)小於10,000之情形,初期接著強度會有降低的傾向,由於黏度低而成為不易均勻地塗布之樹脂組成物。在重量平均分子量(Mw)大於100,000之情形,由於因樹脂組成物的黏度高,在塗布時必須以大量溶劑稀釋,而
接著層會變薄,所以初期接著強度會有降低的傾向,而因在溶劑的乾燥工程需要高溫長時間,對於生產成本與環境也成為不良影響。
又,前述聚酯多元醇的分子量分布(Mw/Mn)在小於3之情形,於作為2液型積層用接著劑使用之情形,對基材的接著性會變低,且硬化後的接著強度與耐濕熱性會變差。另一方面,在分子量分布(Mw/Mn)大於4.7之情形,則也是在作為2液型積層用接著劑使用之情形,硬化後的接著強度會有降低的傾向。從此種對基材之接著強度的觀點來看,前述聚酯多元醇的分子量分布(Mw/Mn)特別更佳為3.0~4.5之範圍。
又,本案發明中,聚酯多元醇的重量平均分子量(Mw)及數量平均分子量(Mn)係藉由下述條件之凝膠滲透層析儀(GPC)所測定之值。
測定裝置:Tosoh株式會社製 HLC-8220GPC
管柱:Tosoh株式會社製 TSK-GUARDCOLUMN SuperHZ-L
+Tosoh株式會社製 TSK-GEL SuperHZM-M×4
檢測器:RI(微差折射器)
資料處理:Tosoh株式會社製 Multi-station GPC-8020 model II
測定條件:管柱溫度40℃
溶媒 四氫呋喃
流速 0.35ml/分
標準:單分散聚苯乙烯
試料:將以樹脂固體含量換算為0.2質量%的四氫呋喃溶液用微過濾器過濾而得之物(100μl)
又,前述聚酯多元醇的羥基價,以在濕熱條件下的基材接著性優良的點來說,較佳在5~30mgKOH/g之範圍,更佳在7~15mgKOH/g之範圍。
以上詳述之本發明之聚酯多元醇,係作為2液型積層接著劑的主劑之多元醇劑係有用的,能與硬化劑一起使用,但本發明中,較佳為使用含有此種聚酯多元醇(以下將其記述為「聚酯多元醇(A)」)、與多官能環氧化合物(B)之樹脂組成物作為2液型積層接著劑之主劑。即,藉由除了前述聚酯多元醇(A),併用多官能環氧化合物(B),而能夠在接著層吸濕時,前述多官能環氧化合物(B)中的環氧基會捕捉由於該聚酯多元醇(A)的水解所產生的羧基,使該接著層之耐濕熱性進一步提升。此種多官能環氧化合物(B)較佳為其數量平均分子量(Mn)在300~5,000之範圍的含羥基之環氧樹脂。即,在數量平均分子量(Mn)為300以上之情形,除了耐濕熱性,對基材的接著強度會更加良好以外,在數量平均分子量(Mn)為5,000以下之情形,與前述聚酯多元醇(A)之相溶性會變良好。從此等之均衡優良的點來看,其中更佳為數量平均分子量(Mn)為400~2,000之範圍者。
又,前述多官能環氧化合物(B),從可得到硬化性更優良之樹脂組成物而言,羥基價較佳為30~160mgKOH之範圍,更佳為50~150mgKOH/g之範圍。
前述多官能環氧化合物(B)可列舉出例如:雙酚A型環氧樹脂、雙酚F型環氧樹脂等雙酚型環氧樹脂;聯苯型環氧樹脂、四甲基聯苯型環氧樹脂等聯苯型環氧樹脂;雙環戊二烯-苯酚加成反應型環氧樹脂等。其可分別單獨使用也可二種以上併用。此等之中,以得到在濕熱條件下的基材接著性及初期接著強度優良之樹脂組成物的點來說,較佳為雙酚型環氧樹脂。
此外,前述樹脂組成物係藉由與前述聚酯多元醇(A)及多官能環氧化合物(B)一起,更進一步併用含羥基之脂肪族聚碳酸酯(C),而可飛越性地使硬化物的交聯密度提升,能進一步提高基材接著性。
此處所使用的含羥基之脂肪族聚碳酸酯(C),數量平均分子量(Mn)在500~3,000之範圍者,羥基濃度會適度地變高,而就硬化時的交聯密度顯著提升的點來說為較佳,特別是數量平均分子量(Mn)在800~2,000之範圍者更佳。且此處,數量平均分子量(Mn)之測定方法,係以與前述聚酯多元醇的GPC測定條件相同條件所測定之值。
前述含羥基之脂肪族聚碳酸酯(C),就成為硬化性更優良的樹脂組成物的點來說,羥基價係為20~300mgKOH/g之範圍,特別更佳為40~250mgKOH/g之範圍。又,以在濕熱條件下的基材接著性優良的點來說,較佳為聚碳酸酯二醇。
此處,前述含羥基之脂肪族聚碳酸酯(C)能藉由例如使多元醇與羰化劑進行聚縮合反應之方法來製造。
用於前述含羥基之脂肪族聚碳酸酯(C)之製造的多元醇,可使用例如任何的前述聚酯二醇的原料之分枝烷多元醇或非分枝烷二醇。
又,用於前述含羥基之脂肪族聚碳酸酯(C)之製造的羰化劑,可列舉出例如:碳酸伸乙酯、碳酸丙烯酯、碳酸二甲酯、碳酸二乙酯、碳酸二丁酯、碳酸二苯酯等。此等可分別單獨使用也可併用二種以上。
由成為對各種基材之接著性優良,且即使在
濕熱條件下也能維持高基材接著性之樹脂組成物的點來說,本發明之樹脂組成物,較佳為藉由相對於100質量份的前述聚酯多元醇(A),以前述多官能環氧化合物(B)成為5~20質量份之範圍的比例,且前述聚碳酸酯樹脂(C)成為5~20質量份之範圍的比例,來含有前述聚酯多元醇(A)、前述多官能環氧化合物(B)、及前述含羥基之脂肪族聚碳酸酯樹脂(C)。
本發明之樹脂組成物也可含有前述聚酯多元醇(A)、前述多官能環氧化合物(B)、及前述含羥基之脂肪族聚碳酸酯樹脂(C)以外的含羥基之化合物。此種含羥基之化合物可列舉出例如:使多元酸與多元醇反應所得之聚酯多元醇、使多元酸、多元醇及聚異氰酸酯反應所得之數量平均分子量(Mw)小於25,000之聚酯聚胺甲酸酯多元醇、使二元酸、二醇及二異氰酸酯反應所得之直鏈型聚酯聚胺甲酸酯多元醇、聚氧乙烯二醇、聚氧丙烯二醇等醚二醇、雙酚A、雙酚F等雙酚、於前述雙酚加成環氧乙烷、環氧丙烷等所得之雙酚的環氧烷加成物等。此等可分別單獨使用也可併用二種以上。
在本發明之樹脂組成物係含有前述聚酯多元醇(A)、前述多官能環氧化合物(B)、及前述含羥基之脂肪族聚碳酸酯樹脂(C)以外的含羥基之化合物之情形,從可獲得對各種基材之接著性優良,且即使在濕熱條件下也能維持高基材接著性之樹脂組成物來看,其含量相對於100質量份的前述聚酯多元醇(A),較佳係成為5~20質量份之範圍的比例。
本發明之硬化性樹脂組成物,係使用包含前述聚酯多元醇(A)之積層接著劑用多元醇劑、或包含前述(A)~(C)各成分之樹脂組成物作為主劑,且使用脂肪族聚異氰酸酯(D)作為其硬化劑。
該脂肪族聚異氰酸酯(D)可列舉出例如各種的聚異氰酸酯。此等聚異氰酸酯(D)可以單獨使用一種,也可併用二種以上。
此等脂肪族聚異氰酸酯(D)之中,以在濕熱條件下的基材密著性優良的點來說,較佳為尿酸酯型聚異氰酸酯化合物。
本發明中,前述脂肪族聚異氰酸酯(D)的摻合比例,從成為硬化性更優良之硬化性樹脂組成物來看,前述聚酯多元醇(A)、前述環氧化合物(B)及前述含羥基之聚碳酸酯樹脂(C)中所含之羥基的合計莫耳數[OH],與前述脂肪族聚異氰酸酯(D)中所含之異氰酸酯基的莫耳數[NCO]之比[OH]/[NCO],較佳為1/1~1/2之範圍,更佳為1/1.05~1/1.5之範圍。
又,在作為主劑使用之前述樹脂組成物含有前述聚酯多元醇(A)、前述多官能環氧化合物(B)、及前述含羥基之聚碳酸酯(C)以外的含羥基之化合物之情形,前述脂肪族聚異氰酸酯(D)的摻合比例較佳為前述硬化性樹脂組成物中羥基的合計莫耳數[OH],與前述聚異氰酸酯化合物(D)所含有的異氰酸酯基的莫耳數[NCO]之比[OH]/[NCO]在1/1~1/2之範圍,更佳在1/1.05~1/1.5之範圍。
本發明之硬化性樹脂組成物也可進一步含有各種的溶劑。前述溶媒可列舉出例如:丙酮、甲乙酮(MEK)、甲基異丁基酮等酮系化合物、四氫呋喃(THF)、二(dioxolane)等環狀醚系化合物、乙酸甲酯、乙酸乙酯、乙酸丁酯等酯系化合物、甲苯、二甲苯等芳香族系化合物、卡必醇、2-乙氧乙醇(cellosolve)、甲醇、異丙醇、丁醇、丙二醇單甲醚等醇系化合物。此等可以單獨使用也可併用二種以上。
本發明之硬化性樹脂組成物也可進一步含有紫外線吸收劑、抗氧化劑、矽系添加劑、氟系添加劑、流變控制劑、消泡劑、抗靜電劑、防霧劑等各種添加劑。
本發明之硬化性樹脂組成物作為用以接著各種的塑膠膜之2液型積層用接著劑係有用的。
此處於貼合所使用之塑膠膜,可列舉出例如:包含聚碳酸酯、聚對苯二甲酸乙二酯、聚甲基丙烯酸甲酯、聚苯乙烯、聚酯、聚烯烴、環氧樹脂、三聚氰胺樹脂、三乙酸纖維素樹脂、聚乙烯醇、ABS樹脂、降
莰烯系樹脂、環烯烴系樹脂、聚醯亞胺樹脂、聚氟乙烯樹脂、聚偏氟乙烯樹脂等之薄膜。本案發明之2液型積層用接著劑,即便是對於上述各種薄膜之中特別難接著之包含聚氟乙烯樹脂或聚偏氟乙烯樹脂的薄膜也顯示高接著性。
接著前述各種薄膜彼此時,本案發明之2液型積層用接著劑的使用量係較佳為2~50g/m2之範圍。
使用本發明之2液型積層用接著劑而接著複數薄膜所得到之積層薄膜,具有所謂即使在濕熱條件下也具高接著性,且薄膜彼此難以剝離之特徵。因此,本發明之2液型積層用接著劑能適用於在室外等嚴厲環境下使用之積層薄膜用途,如上所述,特別能較佳地使用作為製造太陽能電池的背板時之接著劑。
使用本發明之2液型積層用接著劑來製造太陽能電池背板之方法,可舉出例如:將本發明之2液型積層用接著劑塗布於塑膠膜上,接著,於此硬化性樹脂組成物層重疊其它的塑膠基材後,以25~80℃之溫度條件使其硬化而得到片狀成形體的方法。
此處,作為將本發明之2液型積層用接著劑塗布於塑膠膜上的裝置,可列舉出:缺角輪塗布機、輥式刮刀塗布機、狹縫塗布機、輥塗機、棒式塗布機、凹版輥式塗布機、逆輥塗布機、刮刀塗布機、凹版印刷塗布機、微凹版印刷塗布機等。又,前述2液型積層用接著劑對塑膠基材之塗布量,較佳為以乾燥膜厚為1~50μm左右。
上述之塑膠膜及接著劑層也可存在複數個。又,也可為在塑膠膜的表面設置金屬蒸鍍膜等阻氣層,於其上塗布前述2液型積層用接著劑,而積層另一個塑膠膜之結構。進一步,為了提升與密封太陽能電池元件之密封材料的接著性,在該太陽能電池用背板的密封材料側表面也可設置有易接著層。此易接著層可在易接著層的表面形成凹凸,而為了提升密著性,較佳為由TiO2、SiO2、CaCO3、SnO2、ZrO2及MgCO3等金屬微粒與黏結劑所構成者。
又,本發明之太陽能電池用背板中之接著層的厚度為1~50μm之範圍,特別較佳為5~15μm之範圍。
又,使用此種太陽能電池用背板而成的太陽能電池模組,能藉由將乙烯-乙酸乙烯酯樹脂(EVA)片、複數個太陽能電池單元、乙烯-乙酸乙烯酯樹脂(EVA)片、本發明之背板配置於防護玻璃板上,一邊抽真空一邊加熱,EVA片溶解將太陽能電池元件密封,來製造。此時,複數個太陽能電池元件係藉由聯絡線路(interconnector)而被串聯地接合。此處,作為太陽能電池元件可列舉出例如:單結晶矽系太陽能電池元件、多結晶矽系太陽能電池元件、以單接合(single-junction)型、或串接(tandem)型等所構成之非晶矽系太陽能電池元件、砷化鎵(GaAs)或磷化銦(InP)等III-V族化合物半導體太陽能電池元件、碲化鎘(CdTe)等II-VI族化合物半導體太陽能電池元件、銅/銦/硒系(CIS系)、銅/銦/鎵/硒系(CIGS系)、銅/銦/鎵/硒/硫系(CIGSS系)等I-III-VI族
化合物半導體太陽能電池元件、染料敏化型太陽能電池元件、有機太陽能電池元件等。
以下舉出具體合成例、實施例更詳細地說明本發明,但本發明不受這些實施例所限定。又,只要沒有特別說明,「份」為質量基準。
又,本實施例中,數量平均分子量(Mn)及重量平均分子量(Mw)係藉由下述條件之凝膠滲透層析儀(GPC)而測定。
測定裝置:Tosoh株式會社製 HLC-8220GPC
管柱:Tosoh株式會社製 TSK-GUARDCOLUMN SuperHZ-L
+Tosoh株式會社製 TSK-GEL SuperHZM-M×4
檢測器:RI(微差折射器)
資料處理:Tosoh株式會社製 Multi-station GPC-8020 model II
測定條件:管柱溫度40℃
溶媒 四氫呋喃
流速 0.35ml/分
標準:單分散聚苯乙烯
試料:將以樹脂固體含量換算為0.2質量%的四氫呋喃溶液用微過濾器過濾而得之物(100μl)
又,紅外線吸收光譜,係將聚酯多元醇(A)的溶液塗布於KBr板上,並製成使溶劑揮發之試料而測定。
於具有攪拌棒、溫度感應計、精餾管之燒瓶中,加入788份的新戊二醇、21份的三羥甲基丙烷、578份的間苯二甲酸、272份的鄰苯二甲酸酐、419份的癸二酸、17份的苯偏三酸酐及0.2份的有機鈦化合物,使乾燥氮流入燒瓶內,並一邊攪拌一邊加熱至230~250℃而進行酯化反應。在酸價達1.0mgKOH/g以下時停止反應,冷卻至100℃後,以乙酸乙酯稀釋為固體含量62%,而得到重量平均分子量(Mw)為48,000、分子量分布(Mw/Mn)為4.5、羥基價為19、玻璃轉移點(Tg)為10℃之聚酯多元醇(A1)。
於具有攪拌棒、溫度感應計、精餾管之燒瓶中,加入836份的新戊二醇、588份的間苯二甲酸、274份的鄰苯二甲酸酐、406份的癸二酸、15.2份的苯偏三酸酐及0.2份的有機鈦化合物,使乾燥氮流入燒瓶內,並一邊攪拌一邊加熱至230~250℃而進行酯化反應。在酸價達1.0mgKOH/g以下時停止反應,冷卻至100℃後,以乙酸乙酯稀釋為固體含量62%,而得到重量平均分子量(Mw)為25,000、分子量分布(Mw/Mn)為3.2、羥基價為10、玻璃轉移點(Tg)為6℃之聚酯多元醇(A2)。所得到之聚酯多元醇(A2)的GPC圖示於圖1,紅外線吸收光譜圖示於圖2。
於具有攪拌棒、溫度感應計、精餾管之燒瓶中,加入794份的新戊二醇、511份的間苯二甲酸、272份的鄰苯二甲酸酐、230份的癸二酸、261份的十二烷二酸、21份的苯偏三酸酐及0.2份的有機鈦化合物,使乾燥氮流入燒瓶內,並一邊攪拌一邊加熱至230~250℃而進行酯化反應。在酸價達1.0mgKOH/g以下時停止反應,冷卻至100℃後,以乙酸乙酯稀釋為固體含量62%,得到重量平均分子量(Mw)為24,000、分子量分布(Mw/Mn)為3.5、羥基價為18、玻璃轉移點(Tg)為-5℃之聚酯多元醇(A3)。
於具有攪拌棒、溫度感應計、精餾管之燒瓶中,加入1088份的新戊二醇、727份的間苯二甲酸、353份的鄰苯二甲酸酐、524份的癸二酸及0.2份的有機鈦化合物,使乾燥氮流通於燒瓶內,並一邊攪拌一邊加熱至240~260℃而進行酯化反應。在酸價達0.5mgKOH/g以下時停止反應,冷卻至100℃後,以乙酸乙酯稀釋為固體含量62%,得到重量平均分子量(Mw)為78,000、分子量分布(Mw/Mn)為2.5、羥基價為5、玻璃轉移點(Tg)為-10℃之聚酯多元醇(a1)。
於具有攪拌棒、溫度感應計、精餾管之燒瓶中,加入843份的新戊二醇、519份的間苯二甲酸、694份的鄰苯二甲酸酐及0.02份的有機鈦化合物,使乾燥氮
流入燒瓶內,並一邊攪拌一邊加熱至230~250℃而進行酯化反應。在酸價達1.0mgKOH/g以下時停止反應,冷卻至100℃後,以乙酸乙酯稀釋為固體含量62%,得到重量平均分子量(Mw)為13,000、分子量分布(Mw/Mn)為2.2、羥基價為20、玻璃轉移點(Tg)為35℃之聚酯多元醇(a2)。
於具有攪拌棒、溫度感應計、精餾管之燒瓶中,加入862份的新戊二醇、389份的間苯二甲酸、520份的鄰苯二甲酸酐、313份的己二酸及0.02份的有機鈦化合物,使乾燥氮流入燒瓶內,並一邊攪拌一邊加熱至230~250℃而進行酯化反應。在酸價達1.0mgKOH/g以下時停止反應,冷卻至100℃後,以乙酸乙酯稀釋為固體含量62%,得到重量平均分子量(Mw)為15,000、分子量分布(Mw/Mn)為2.1、羥基價為18、玻璃轉移點(Tg)為20℃之聚酯多元醇(a3)。
於具有攪拌棒、溫度感應計、精餾管之燒瓶中,加入1130份的新戊二醇、759份的間苯二甲酸、342份的鄰苯二甲酸酐、534份的癸二酸及1.2份的有機鈦化合物,使乾燥氮在燒瓶內流通,並一邊攪拌一邊加熱至230~250℃而進行酯化反應。在酸價達1.0mgKOH/g以下時停止反應,冷卻至100℃後,以乙酸乙酯稀釋為固體含量80%。接著,加入108份的伸己二異氰酸酯,使
乾燥氮流通於燒瓶內,並一邊攪拌一邊加熱至70~80℃而進行胺甲酸酯化反應。在異氰酸酯含有率達0.3%以下時停止反應,得到數量平均分子量為10000、重量平均分子量為22000,且羥基價為9之聚酯多元醇。把將此以乙酸乙酯稀釋所得到的固體含量62%之樹脂溶液作為聚酯多元醇(a4)。
使用數量平均分子量(Mn)470、環氧基當量245g/eq之雙酚A型環氧樹脂(DIC株式會社製「EPICLON 860」)作為多官能環氧化合物(B1),使用數量平均分子量(Mn)900、環氧基當量475g/eq之雙酚A型環氧樹脂(三菱化學公司製「JER1001」)作為多官能環氧化合物(B2),使用數量平均分子量約1000、羥基價約110之Placcel CD210(大賽璐化學公司製)作為聚碳酸酯(C),並依據表1及表2,調製接著劑主劑。
使用尿酸酯型的伸己二異氰酸酯(D)Sumidur N3300(Sumitomo Bayer Urethane公司製)作為接著劑硬化劑的聚異氰酸酯。
以表1、表2所示之配方,將含有聚酯多元醇、環氧化合物及聚碳酸酯之主劑、硬化劑一起混合,而調製成各接著劑。又,表中的摻合量為固體含量質量份,硬化劑的摻合量係相對於100質量份的主劑之摻合量。
使用125μm厚的PET薄膜(Toray(股)製「X10S」)作為原卷(original fabric),將上述各接著劑組
成物以5~6g/m2(乾燥質量)塗布,使用25μm厚的氟薄膜(旭硝子(股)AFLEX25PW)作為貼合用薄膜,而得到評價樣本。評價樣本在50℃老化72小時後,用於評價。
評價1:外觀 對以前述方法製成之評價樣本,由氟薄膜側目視評價積層外觀。
○:薄膜表面平滑 △:於薄膜表面存在一些坑洞×:於薄膜表面存在大量坑洞(凹陷)
評價2:在濕熱條件下的接著力之測定 對以前述方法製成之評價樣本,使用拉伸試驗機(SHIMADZU公司製「AGS500NG」),在剝離速度300mm/min、強度N/15mm之條件下進行T型剝離試驗,評價其強度作為接著力。
測定評價樣本的初期接著力與在121℃、濕度100%的環境下暴露25小時、50小時、75小時後之樣本的接著力。
評價3:耐濕熱性之評價 將於前述評價2測定之評價樣本的初期接著力,與在121℃、濕度100%的環境下暴露75小時暴露後的樣本的接著力進行比較,將暴露後的接著力為初期接著力的80%以上者評價為◎、65%以上小於80%者評價為○、40%以上小於65%者評價為△、小於40%者評價為×。
Claims (7)
- 一種樹脂組成物,其特徵為含有聚酯多元醇(A)及多官能環氧化合物(B)為必須成分,且不含有聚酯聚胺甲酸酯多元醇,其中該聚酯多元醇(A)係:具有使分枝伸烷二醇、碳原子數8~20的長鏈脂肪族二羧酸、與芳香族三羧酸反應所得之樹脂結構,且重量平均分子量(Mw)在10,000~100,000之範圍,分子量分布(Mw/Mn)在3.0~4.7之範圍。
- 如請求項1之樹脂組成物,其中聚酯多元醇(A)係除了分枝伸烷二醇、碳原子數8~20的長鏈脂肪族二羧酸、及芳香族三羧酸以外,更進一步使用芳香族二羧酸作為原料成分進行反應所得。
- 如請求項1之樹脂組成物,其中聚酯多元醇(A)的羥基價係在2~30mgKOH/g之範圍。
- 如請求項1至3中任一項之樹脂組成物,其係以聚酯多元醇(A)、多官能環氧化合物(B)、及含羥基之脂肪族聚碳酸酯(C)為必須成分。
- 一種硬化性樹脂組成物,其係使用如請求項4之樹脂組成物作為主劑,且摻合作為硬化劑之脂肪族聚異氰酸酯(D)而成。
- 一種2液型積層用接著劑,其係包含如請求項5之硬化性樹脂組成物。
- 一種太陽能電池用背板,其係由選自包含聚酯膜、氟系樹脂膜、聚烯烴膜及金屬箔之群組中的1種以上之薄膜,與包含用以貼合此等薄膜彼此之如請求項6之2液型積層用接著劑的接著層所形成。
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JP6439237B2 (ja) * | 2013-06-19 | 2018-12-19 | Dic株式会社 | 新規ポリエステルポリウレタンポリオール、2液型ラミネート接着剤用ポリオール剤、樹脂組成物、硬化性樹脂組成物、2液型ラミネート用接着剤、及び太陽電池用バックシート |
CN110406236B (zh) * | 2013-10-15 | 2021-10-26 | 陶氏环球技术有限责任公司 | 制备具有降低的透氧性的层压制品的方法 |
CN108884373B (zh) * | 2016-03-28 | 2022-01-25 | 陶氏环球技术有限责任公司 | 双组分无溶剂粘合剂组合物及其制备方法 |
CN105906790B (zh) * | 2016-05-06 | 2017-12-22 | 浙江枧洋高分子科技有限公司 | 一种合成湿气固化聚氨酯热熔胶的聚酯多元醇 |
CN109642013B (zh) * | 2016-07-11 | 2022-06-21 | 陶氏环球技术有限责任公司 | 高固体含量的基于溶剂的粘着剂组合物和其制造方法 |
BR112019003697B1 (pt) * | 2016-08-25 | 2022-12-20 | Stepan Company | Composição de polímero de poliéster-epóxido, revestimento, elastômero, elastômero microcelular, adeviso, selante e processos para preparar uma composição de polímero de poliéster-epóxido |
WO2018117082A1 (ja) * | 2016-12-20 | 2018-06-28 | Dic株式会社 | ポリエステルポリオール、反応型接着剤、および積層体 |
JP7130947B2 (ja) * | 2017-05-23 | 2022-09-06 | 三菱ケミカル株式会社 | ポリエステル系粘着剤組成物、ポリエステル系粘着剤、粘着シート及び粘着剤層付き光学部材 |
KR102460457B1 (ko) * | 2016-12-28 | 2022-10-28 | 미쯔비시 케미컬 주식회사 | 폴리에스테르계 점착제 조성물, 폴리에스테르계 점착제, 점착 시트 및 점착제층 부착 광학 부재 |
WO2018124200A1 (ja) * | 2016-12-28 | 2018-07-05 | 日本合成化学工業株式会社 | ポリエステル系粘着剤組成物、ポリエステル系粘着剤、粘着シート及び粘着剤層付き光学部材 |
JP7067038B2 (ja) * | 2016-12-28 | 2022-05-16 | 三菱ケミカル株式会社 | ポリエステル系粘着剤組成物、ポリエステル系粘着剤、粘着シート及び粘着剤層付き光学部材 |
WO2018179707A1 (ja) * | 2017-03-28 | 2018-10-04 | 東洋紡株式会社 | カルボン酸基含有ポリエステル系接着剤組成物 |
JP6834702B2 (ja) * | 2017-03-31 | 2021-02-24 | 東洋インキScホールディングス株式会社 | 接着剤組成物 |
KR102146540B1 (ko) | 2017-09-15 | 2020-08-20 | 주식회사 엘지화학 | 배터리 모듈 |
JP7047353B2 (ja) * | 2017-12-01 | 2022-04-05 | 東洋インキScホールディングス株式会社 | 積層シート形成用接着剤組成物 |
KR102070573B1 (ko) * | 2018-04-20 | 2020-01-29 | 주식회사 엘지화학 | 수지 조성물 및 이를 포함하는 배터리 모듈 |
TWI819147B (zh) * | 2018-11-28 | 2023-10-21 | 日商Dic股份有限公司 | 反應性接著劑及其製造方法、積層體及包裝體 |
JP6892036B1 (ja) * | 2019-08-26 | 2021-06-18 | Dic株式会社 | 2液型接着剤、積層体、成型体、包装材 |
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