WO2023075501A1 - 에틸렌/알파-올레핀 공중합체 및 이를 포함하는 봉지재 필름용 조성물 - Google Patents
에틸렌/알파-올레핀 공중합체 및 이를 포함하는 봉지재 필름용 조성물 Download PDFInfo
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- WO2023075501A1 WO2023075501A1 PCT/KR2022/016694 KR2022016694W WO2023075501A1 WO 2023075501 A1 WO2023075501 A1 WO 2023075501A1 KR 2022016694 W KR2022016694 W KR 2022016694W WO 2023075501 A1 WO2023075501 A1 WO 2023075501A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- alpha
- carbon atoms
- ethylene
- olefin copolymer
- olefin
- Prior art date
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- 239000004711 α-olefin Substances 0.000 title claims abstract description 111
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 239000005977 Ethylene Substances 0.000 title claims abstract description 92
- 229920000089 Cyclic olefin copolymer Polymers 0.000 title claims abstract description 78
- 239000000203 mixture Substances 0.000 title claims abstract description 36
- 239000000565 sealant Substances 0.000 title abstract 2
- 239000008393 encapsulating agent Substances 0.000 claims description 31
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 claims description 22
- 238000000034 method Methods 0.000 claims description 19
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 claims description 18
- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 claims description 16
- 238000004736 wide-angle X-ray diffraction Methods 0.000 claims description 16
- 239000000155 melt Substances 0.000 claims description 14
- 238000000235 small-angle X-ray scattering Methods 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 13
- 230000008018 melting Effects 0.000 claims description 13
- ZGEGCLOFRBLKSE-UHFFFAOYSA-N 1-Heptene Chemical compound CCCCCC=C ZGEGCLOFRBLKSE-UHFFFAOYSA-N 0.000 claims description 10
- AFFLGGQVNFXPEV-UHFFFAOYSA-N 1-decene Chemical compound CCCCCCCCC=C AFFLGGQVNFXPEV-UHFFFAOYSA-N 0.000 claims description 10
- CRSBERNSMYQZNG-UHFFFAOYSA-N 1-dodecene Chemical compound CCCCCCCCCCC=C CRSBERNSMYQZNG-UHFFFAOYSA-N 0.000 claims description 10
- GQEZCXVZFLOKMC-UHFFFAOYSA-N 1-hexadecene Chemical compound CCCCCCCCCCCCCCC=C GQEZCXVZFLOKMC-UHFFFAOYSA-N 0.000 claims description 10
- HFDVRLIODXPAHB-UHFFFAOYSA-N 1-tetradecene Chemical compound CCCCCCCCCCCCC=C HFDVRLIODXPAHB-UHFFFAOYSA-N 0.000 claims description 10
- DCTOHCCUXLBQMS-UHFFFAOYSA-N 1-undecene Chemical compound CCCCCCCCCC=C DCTOHCCUXLBQMS-UHFFFAOYSA-N 0.000 claims description 10
- WSSSPWUEQFSQQG-UHFFFAOYSA-N 4-methyl-1-pentene Chemical compound CC(C)CC=C WSSSPWUEQFSQQG-UHFFFAOYSA-N 0.000 claims description 10
- VAMFXQBUQXONLZ-UHFFFAOYSA-N n-alpha-eicosene Natural products CCCCCCCCCCCCCCCCCCC=C VAMFXQBUQXONLZ-UHFFFAOYSA-N 0.000 claims description 10
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 claims description 10
- 238000000113 differential scanning calorimetry Methods 0.000 claims description 9
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 8
- 229940106006 1-eicosene Drugs 0.000 claims description 5
- FIKTURVKRGQNQD-UHFFFAOYSA-N 1-eicosene Natural products CCCCCCCCCCCCCCCCCC=CC(O)=O FIKTURVKRGQNQD-UHFFFAOYSA-N 0.000 claims description 5
- 229940069096 dodecene Drugs 0.000 claims description 5
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 5
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 5
- 229940095068 tetradecene Drugs 0.000 claims 1
- 238000004132 cross linking Methods 0.000 abstract description 32
- 239000003431 cross linking reagent Substances 0.000 abstract description 30
- 230000000704 physical effect Effects 0.000 abstract description 14
- 238000005470 impregnation Methods 0.000 abstract description 13
- 125000004432 carbon atom Chemical group C* 0.000 description 166
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 41
- 229910052739 hydrogen Inorganic materials 0.000 description 37
- 239000001257 hydrogen Substances 0.000 description 37
- 125000000217 alkyl group Chemical group 0.000 description 32
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 30
- 125000003118 aryl group Chemical group 0.000 description 28
- 125000003342 alkenyl group Chemical group 0.000 description 26
- 239000000178 monomer Substances 0.000 description 24
- -1 tbutyl Chemical group 0.000 description 24
- 239000013598 vector Substances 0.000 description 24
- 125000000753 cycloalkyl group Chemical group 0.000 description 22
- 150000001875 compounds Chemical class 0.000 description 21
- 229920001577 copolymer Polymers 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 18
- 150000003623 transition metal compounds Chemical class 0.000 description 18
- 239000011342 resin composition Substances 0.000 description 16
- 125000002877 alkyl aryl group Chemical group 0.000 description 14
- 125000003710 aryl alkyl group Chemical group 0.000 description 14
- 229910052736 halogen Inorganic materials 0.000 description 14
- 150000002367 halogens Chemical class 0.000 description 14
- 238000006116 polymerization reaction Methods 0.000 description 14
- 238000004519 manufacturing process Methods 0.000 description 12
- 239000013078 crystal Substances 0.000 description 11
- 238000002360 preparation method Methods 0.000 description 10
- 239000000126 substance Substances 0.000 description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 9
- 125000003545 alkoxy group Chemical group 0.000 description 9
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000006096 absorbing agent Substances 0.000 description 5
- 125000002102 aryl alkyloxo group Chemical group 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 5
- 125000001475 halogen functional group Chemical group 0.000 description 5
- 229910052698 phosphorus Inorganic materials 0.000 description 5
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 4
- 239000006087 Silane Coupling Agent Substances 0.000 description 4
- 238000000333 X-ray scattering Methods 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 125000003282 alkyl amino group Chemical group 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 4
- 125000001769 aryl amino group Chemical group 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000012760 heat stabilizer Substances 0.000 description 4
- 230000000977 initiatory effect Effects 0.000 description 4
- 238000003475 lamination Methods 0.000 description 4
- 239000003446 ligand Substances 0.000 description 4
- 239000004611 light stabiliser Substances 0.000 description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 150000001451 organic peroxides Chemical class 0.000 description 4
- 230000000379 polymerizing effect Effects 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 150000003254 radicals Chemical group 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 description 3
- 238000005160 1H NMR spectroscopy Methods 0.000 description 3
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical group CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 229910052735 hafnium Inorganic materials 0.000 description 3
- DLEDOFVPSDKWEF-UHFFFAOYSA-N lithium butane Chemical compound [Li+].CCC[CH2-] DLEDOFVPSDKWEF-UHFFFAOYSA-N 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- PHQOGHDTIVQXHL-UHFFFAOYSA-N n'-(3-trimethoxysilylpropyl)ethane-1,2-diamine Chemical compound CO[Si](OC)(OC)CCCNCCN PHQOGHDTIVQXHL-UHFFFAOYSA-N 0.000 description 3
- MZRVEZGGRBJDDB-UHFFFAOYSA-N n-Butyllithium Substances [Li]CCCC MZRVEZGGRBJDDB-UHFFFAOYSA-N 0.000 description 3
- 230000005693 optoelectronics Effects 0.000 description 3
- 150000002978 peroxides Chemical class 0.000 description 3
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical class [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 3
- 229910000077 silane Inorganic materials 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- DLSMLZRPNPCXGY-UHFFFAOYSA-N tert-butylperoxy 2-ethylhexyl carbonate Chemical compound CCCCC(CC)COC(=O)OOOC(C)(C)C DLSMLZRPNPCXGY-UHFFFAOYSA-N 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- KOMNUTZXSVSERR-UHFFFAOYSA-N 1,3,5-tris(prop-2-enyl)-1,3,5-triazinane-2,4,6-trione Chemical compound C=CCN1C(=O)N(CC=C)C(=O)N(CC=C)C1=O KOMNUTZXSVSERR-UHFFFAOYSA-N 0.000 description 2
- FCEHBMOGCRZNNI-UHFFFAOYSA-N 1-benzothiophene Chemical compound C1=CC=C2SC=CC2=C1 FCEHBMOGCRZNNI-UHFFFAOYSA-N 0.000 description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- KUDUQBURMYMBIJ-UHFFFAOYSA-N 2-prop-2-enoyloxyethyl prop-2-enoate Chemical compound C=CC(=O)OCCOC(=O)C=C KUDUQBURMYMBIJ-UHFFFAOYSA-N 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 2
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 description 2
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 125000003277 amino group Chemical group 0.000 description 2
- 125000000751 azo group Chemical group [*]N=N[*] 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000010924 continuous production Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000007334 copolymerization reaction Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000007872 degassing Methods 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 238000010292 electrical insulation Methods 0.000 description 2
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 150000002432 hydroperoxides Chemical class 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- NXPHGHWWQRMDIA-UHFFFAOYSA-M magnesium;carbanide;bromide Chemical compound [CH3-].[Mg+2].[Br-] NXPHGHWWQRMDIA-UHFFFAOYSA-M 0.000 description 2
- 238000001782 photodegradation Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- JMTMWSZLPHDWBQ-UHFFFAOYSA-N tetrakis[ethenyl(dimethyl)silyl] silicate Chemical compound C=C[Si](C)(C)O[Si](O[Si](C)(C)C=C)(O[Si](C)(C)C=C)O[Si](C)(C)C=C JMTMWSZLPHDWBQ-UHFFFAOYSA-N 0.000 description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052726 zirconium Inorganic materials 0.000 description 2
- WRXCBRHBHGNNQA-UHFFFAOYSA-N (2,4-dichlorobenzoyl) 2,4-dichlorobenzenecarboperoxoate Chemical compound ClC1=CC(Cl)=CC=C1C(=O)OOC(=O)C1=CC=C(Cl)C=C1Cl WRXCBRHBHGNNQA-UHFFFAOYSA-N 0.000 description 1
- ZICNIEOYWVIEQJ-UHFFFAOYSA-N (2-methylbenzoyl) 2-methylbenzenecarboperoxoate Chemical compound CC1=CC=CC=C1C(=O)OOC(=O)C1=CC=CC=C1C ZICNIEOYWVIEQJ-UHFFFAOYSA-N 0.000 description 1
- FVQMJJQUGGVLEP-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOOC(C)(C)C FVQMJJQUGGVLEP-UHFFFAOYSA-N 0.000 description 1
- QEQBMZQFDDDTPN-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy benzenecarboperoxoate Chemical compound CC(C)(C)OOOC(=O)C1=CC=CC=C1 QEQBMZQFDDDTPN-UHFFFAOYSA-N 0.000 description 1
- KDGNCLDCOVTOCS-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy propan-2-yl carbonate Chemical compound CC(C)OC(=O)OOC(C)(C)C KDGNCLDCOVTOCS-UHFFFAOYSA-N 0.000 description 1
- RSGZQYVTVPJMTG-UHFFFAOYSA-N (5-benzoylperoxy-2,5-dimethylhex-3-yn-2-yl) benzenecarboperoxoate Chemical compound C=1C=CC=CC=1C(=O)OOC(C)(C)C#CC(C)(C)OOC(=O)C1=CC=CC=C1 RSGZQYVTVPJMTG-UHFFFAOYSA-N 0.000 description 1
- UICXTANXZJJIBC-UHFFFAOYSA-N 1-(1-hydroperoxycyclohexyl)peroxycyclohexan-1-ol Chemical compound C1CCCCC1(O)OOC1(OO)CCCCC1 UICXTANXZJJIBC-UHFFFAOYSA-N 0.000 description 1
- ZDKPIHMFWCOHRD-UHFFFAOYSA-N 1-[[4-[4-bis(2,4-ditert-butylphenoxy)phosphorylphenyl]phenyl]-(2,4-ditert-butylphenoxy)phosphoryl]oxy-2,4-ditert-butylbenzene Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(=O)(C=1C=CC(=CC=1)C=1C=CC(=CC=1)P(=O)(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C ZDKPIHMFWCOHRD-UHFFFAOYSA-N 0.000 description 1
- LGJCFVYMIJLQJO-UHFFFAOYSA-N 1-dodecylperoxydodecane Chemical compound CCCCCCCCCCCCOOCCCCCCCCCCCC LGJCFVYMIJLQJO-UHFFFAOYSA-N 0.000 description 1
- BJELTSYBAHKXRW-UHFFFAOYSA-N 2,4,6-triallyloxy-1,3,5-triazine Chemical compound C=CCOC1=NC(OCC=C)=NC(OCC=C)=N1 BJELTSYBAHKXRW-UHFFFAOYSA-N 0.000 description 1
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 description 1
- JGBAASVQPMTVHO-UHFFFAOYSA-N 2,5-dihydroperoxy-2,5-dimethylhexane Chemical compound OOC(C)(C)CCC(C)(C)OO JGBAASVQPMTVHO-UHFFFAOYSA-N 0.000 description 1
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 1
- WYGWHHGCAGTUCH-UHFFFAOYSA-N 2-[(2-cyano-4-methylpentan-2-yl)diazenyl]-2,4-dimethylpentanenitrile Chemical compound CC(C)CC(C)(C#N)N=NC(C)(C#N)CC(C)C WYGWHHGCAGTUCH-UHFFFAOYSA-N 0.000 description 1
- WFUGQJXVXHBTEM-UHFFFAOYSA-N 2-hydroperoxy-2-(2-hydroperoxybutan-2-ylperoxy)butane Chemical compound CCC(C)(OO)OOC(C)(CC)OO WFUGQJXVXHBTEM-UHFFFAOYSA-N 0.000 description 1
- AIBRSVLEQRWAEG-UHFFFAOYSA-N 3,9-bis(2,4-ditert-butylphenoxy)-2,4,8,10-tetraoxa-3,9-diphosphaspiro[5.5]undecane Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP1OCC2(COP(OC=3C(=CC(=CC=3)C(C)(C)C)C(C)(C)C)OC2)CO1 AIBRSVLEQRWAEG-UHFFFAOYSA-N 0.000 description 1
- 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 1
- HXLAEGYMDGUSBD-UHFFFAOYSA-N 3-[diethoxy(methyl)silyl]propan-1-amine Chemical compound CCO[Si](C)(OCC)CCCN HXLAEGYMDGUSBD-UHFFFAOYSA-N 0.000 description 1
- ZYAASQNKCWTPKI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-amine Chemical compound CO[Si](C)(OC)CCCN ZYAASQNKCWTPKI-UHFFFAOYSA-N 0.000 description 1
- CAMBAGZYTIDFBK-UHFFFAOYSA-N 3-tert-butylperoxy-2-methylpropan-1-ol Chemical compound CC(CO)COOC(C)(C)C CAMBAGZYTIDFBK-UHFFFAOYSA-N 0.000 description 1
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 1
- QQPVHTMPKWDLRM-UHFFFAOYSA-N C(C)(C)(C)N[Si](C)(C)C1C(=C(C=2C3=C(SC=21)C=CC=C3)C)C Chemical compound C(C)(C)(C)N[Si](C)(C)C1C(=C(C=2C3=C(SC=21)C=CC=C3)C)C QQPVHTMPKWDLRM-UHFFFAOYSA-N 0.000 description 1
- JZJDQBZDSBCARL-UHFFFAOYSA-N CC1=C(CC2=C1C1=C(S2)C=CC=C1)C Chemical compound CC1=C(CC2=C1C1=C(S2)C=CC=C1)C JZJDQBZDSBCARL-UHFFFAOYSA-N 0.000 description 1
- 239000004641 Diallyl-phthalate Substances 0.000 description 1
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 description 1
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 description 1
- 238000005481 NMR spectroscopy Methods 0.000 description 1
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
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- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 1
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- ZPOLOEWJWXZUSP-WAYWQWQTSA-N bis(prop-2-enyl) (z)-but-2-enedioate Chemical compound C=CCOC(=O)\C=C/C(=O)OCC=C ZPOLOEWJWXZUSP-WAYWQWQTSA-N 0.000 description 1
- QUDWYFHPNIMBFC-UHFFFAOYSA-N bis(prop-2-enyl) benzene-1,2-dicarboxylate Chemical compound C=CCOC(=O)C1=CC=CC=C1C(=O)OCC=C QUDWYFHPNIMBFC-UHFFFAOYSA-N 0.000 description 1
- 125000004799 bromophenyl group Chemical group 0.000 description 1
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- MABAWBWRUSBLKQ-UHFFFAOYSA-N ethenyl-tri(propan-2-yloxy)silane Chemical compound CC(C)O[Si](OC(C)C)(OC(C)C)C=C MABAWBWRUSBLKQ-UHFFFAOYSA-N 0.000 description 1
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 description 1
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- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
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- CIAYYZGZMJDALI-UHFFFAOYSA-N n'-(triethoxysilylmethyl)ethane-1,2-diamine Chemical compound CCO[Si](OCC)(OCC)CNCCN CIAYYZGZMJDALI-UHFFFAOYSA-N 0.000 description 1
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- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 description 1
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- LIBWSLLLJZULCP-UHFFFAOYSA-N n-(3-triethoxysilylpropyl)aniline Chemical compound CCO[Si](OCC)(OCC)CCCNC1=CC=CC=C1 LIBWSLLLJZULCP-UHFFFAOYSA-N 0.000 description 1
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- DRRZZMBHJXLZRS-UHFFFAOYSA-N n-[3-[dimethoxy(methyl)silyl]propyl]cyclohexanamine Chemical compound CO[Si](C)(OC)CCCNC1CCCCC1 DRRZZMBHJXLZRS-UHFFFAOYSA-N 0.000 description 1
- FVMHCRMQWNASEI-UHFFFAOYSA-N n-[[diethoxy(methyl)silyl]methyl]aniline Chemical compound CCO[Si](C)(OCC)CNC1=CC=CC=C1 FVMHCRMQWNASEI-UHFFFAOYSA-N 0.000 description 1
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- SRSFOMHQIATOFV-UHFFFAOYSA-N octanoyl octaneperoxoate Chemical compound CCCCCCCC(=O)OOC(=O)CCCCCCC SRSFOMHQIATOFV-UHFFFAOYSA-N 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 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 1
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- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- ROEHNQZQCCPZCH-UHFFFAOYSA-N tert-butyl 2-tert-butylperoxycarbonylbenzoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1C(=O)OC(C)(C)C ROEHNQZQCCPZCH-UHFFFAOYSA-N 0.000 description 1
- SWAXTRYEYUTSAP-UHFFFAOYSA-N tert-butyl ethaneperoxoate Chemical compound CC(=O)OOC(C)(C)C SWAXTRYEYUTSAP-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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- SGCFZHOZKKQIBU-UHFFFAOYSA-N tributoxy(ethenyl)silane Chemical compound CCCCO[Si](OCCCC)(OCCCC)C=C SGCFZHOZKKQIBU-UHFFFAOYSA-N 0.000 description 1
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- MCULRUJILOGHCJ-UHFFFAOYSA-N triisobutylaluminium Chemical compound CC(C)C[Al](CC(C)C)CC(C)C MCULRUJILOGHCJ-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/16—Copolymers of ethene with alpha-alkenes, e.g. EP rubbers
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08F4/00—Polymerisation catalysts
- C08F4/42—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors
- C08F4/44—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides
- C08F4/60—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides together with refractory metals, iron group metals, platinum group metals, manganese, rhenium technetium or compounds thereof
- C08F4/62—Refractory metals or compounds thereof
- C08F4/64—Titanium, zirconium, hafnium or compounds thereof
- C08F4/659—Component covered by group C08F4/64 containing a transition metal-carbon bond
- C08F4/6592—Component covered by group C08F4/64 containing a transition metal-carbon bond containing at least one cyclopentadienyl ring, condensed or not, e.g. an indenyl or a fluorenyl ring
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- 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
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- C08F2420/02—Cp or analog bridged to a non-Cp X anionic donor
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- 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
- C08F2420/00—Metallocene catalysts
- C08F2420/06—Cp analog where at least one of the carbon atoms of the non-coordinating part of the condensed ring is replaced by a heteroatom
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- 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
- C08F2500/00—Characteristics or properties of obtained polyolefins; Use thereof
- C08F2500/12—Melt flow index or melt flow ratio
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- 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
- C08F2500/00—Characteristics or properties of obtained polyolefins; Use thereof
- C08F2500/18—Bulk density
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- 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
- C08F2500/00—Characteristics or properties of obtained polyolefins; Use thereof
- C08F2500/26—Use as polymer for film forming
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- 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
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- C08F4/42—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors
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- C08F4/60—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides together with refractory metals, iron group metals, platinum group metals, manganese, rhenium technetium or compounds thereof
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- C08F4/65908—Component covered by group C08F4/64 containing a transition metal-carbon bond in combination with an ionising compound other than alumoxane, e.g. (C6F5)4B-X+
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08F4/42—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors
- C08F4/44—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides
- C08F4/60—Metals; Metal hydrides; Metallo-organic compounds; Use thereof as catalyst precursors selected from light metals, zinc, cadmium, mercury, copper, silver, gold, boron, gallium, indium, thallium, rare earths or actinides together with refractory metals, iron group metals, platinum group metals, manganese, rhenium technetium or compounds thereof
- C08F4/62—Refractory metals or compounds thereof
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Definitions
- the present invention relates to an ethylene/alpha-olefin copolymer having excellent properties in which a crosslinking agent impregnation time is shortened and a degree of crosslinking is high, and a composition for an encapsulant film including the same.
- solar cells are attracting attention as a means of generating energy without fear of environmental pollution and depletion.
- a solar cell When a solar cell is used outdoors, such as on the roof of a building, it is generally used in the form of a solar cell module.
- front glass/solar cell encapsulant/crystalline solar cell element/solar cell encapsulant/rear glass (or back protection sheet) are laminated in this order.
- the solar cell encapsulant an ethylene/vinyl acetate copolymer or an ethylene/alpha-olefin copolymer having excellent transparency, flexibility, adhesiveness, etc. is generally used.
- the degree of crosslinking can be used as an indicator for evaluating mechanical strength and heat resistance, and the higher the degree of crosslinking, the better the encapsulation When used as materials, mechanical strength and heat resistance are excellent, and the long-term stability of the module is high.
- Patent Document 1 Japanese Patent Laid-Open No. 2010-258439
- An object of the present invention is to provide an ethylene/alpha-olefin copolymer having excellent physical properties, such as a shortened impregnation time of a crosslinking agent and a high degree of crosslinking, and a method for preparing the same.
- the present invention provides an ethylene/alpha-olefin copolymer and a composition for an encapsulant film comprising the same.
- the present invention provides an ethylene/alpha-olefin copolymer that satisfies the following conditions (a) to (d).
- the present invention provides the ethylene/alpha-olefin copolymer according to (1) above, wherein the crystallinity is 13% or less.
- the present invention provides an ethylene/alpha-olefin copolymer having a hardness (shore A) of 63 or less.
- the present invention provides the ethylene/alpha-olefin copolymer according to any one of (1) to (3) above, wherein the melting temperature is 50 to 65°C.
- the present invention provides the ethylene/alpha-olefin copolymer according to any one of (1) to (4) above, having a density of 0.85 to 0.89 g/cc.
- the present invention is any one of (1) to (5) above, wherein the melt index (Melt Index, MI, 190 ° C, 2.16 kg load conditions) is 1 to 100 dg / min ethylene / alpha-olefin air provide synthesis.
- MI Melt Index
- melt index MI 10 , 190 °C, 10 kg load condition
- melt index MI 2.16 , 190 °C, 2.16 kg load condition
- MFRR melt flow rate ratio
- alpha-olefin is propylene, 1-butene, 1-pentene, 4-methyl-1-pentene, 1-hexene, 1-heptene , 1-octene, 1-decene, 1-undecene, 1-dodecene, 1-tetradecene, 1-hexadecene and 1-eicosene containing at least one selected from the group consisting of ethylene / alpha- An olefin copolymer is provided.
- the present invention is the ethylene/alpha-olefin copolymer according to any one of (1) to (8) above, wherein the alpha-olefin is contained in an amount greater than 0 and less than or equal to 99 mole% based on the ethylene/alpha-olefin copolymer. to provide.
- the present invention provides a composition for an encapsulant film comprising the ethylene/alpha-olefin copolymer of any one of (1) to (9) above.
- the ethylene/alpha-olefin copolymer of the present invention shows a low crystallinity due to a high ratio of amorphous regions. Due to this, the ethylene/alpha-olefin copolymer exhibits high water absorption, can be impregnated with a crosslinking agent in a short time, and can exhibit an excellent degree of crosslinking.
- Figure 1 shows the deconvolution result of the peak in Example 1.
- the ethylene/alpha-olefin copolymer of the present invention is characterized by satisfying the following conditions (a) to (d).
- the ethylene/alpha-olefin copolymer of the present invention has a low crystallinity and a high proportion of amorphous regions, so it exhibits excellent absorption of polar substances such as crosslinking agents and crosslinking aids.
- the ethylene/alpha-olefin copolymer of the present invention is prepared by adding a transition metal compound, a cocatalyst, ethylene, and an alpha-olefin monomer into a polymerization reactor and polymerizing the mixture. It is characterized by a high ratio of amorphous regions in the ethylene/alpha-olefin copolymer and wide spacing between crystalline regions.
- the ethylene/alpha-olefin copolymer of the present invention has a d-spacing of 12 nm or more as measured by SAXS (Small-Angle X-Ray Scattering).
- the d-spacing represents a distance (d-spacing) between domains in a crystal structure, and the lower the d-spacing value, the shorter the distance between crystal structures, and thus indicates high crystallinity.
- the d-spacing can be measured by SAXS (Small-Angle X-Ray Scattering). Specifically, X-rays were transmitted through the sample using Xenocs' model name Xeuss 2.0 X-ray scattering equipment, and the scattering intensity (I(q)) according to the scattering vector (q) was measured. More specifically, the small-angle X-ray scattering measurement (SAXS) was measured by placing the sample at a location 2.5 m away from the detector and incident X-rays, and a Pilatus3 300K (2D detector) was used as the detector.
- SAXS Small-angle X-ray scattering measurement
- the scattered 2D diffraction pattern is obtained as an image, calibrated using the sample-to-detector distance obtained through the standard sample, and then circularly averaged using the 2D diffraction pattern obtained through the sample analysis to calculate the scattering vector (q The scattering intensity (I(q)) according to ) was converted.
- q is a scattering vector
- ⁇ is a value of 1/2 the scattering angle
- ⁇ is the wavelength of the irradiated X-ray.
- the distance of the crystal domain was analyzed by measuring the scattering intensity (I(q)) according to the scattering vector (q) obtained through SAXS.
- the measured scattering intensity (I(q)) is multiplied by the square of the scattering vector (q), and a peak is observed in a graph of I(q) ⁇ q 2 according to the scattering vector (q).
- a distance (d-spacing) between crystal domains was obtained using the scattering vector value (q*) of the observed peak.
- the q* represents the scattering vector value at the peak of the graph of I(q) ⁇ q 2 according to the scattering vector (q).
- d-spacing is greater than 12 nm.
- the range of d-spacing is 12 nm or more, there is an advantage in that a large amount of crosslinking agent can be impregnated in a short time because the absorption of the ethylene/alpha-olefin copolymer for the crosslinking agent component increases.
- the ethylene/alpha-olefin copolymer of the present invention may have a crystallinity of 14% or less, specifically, 13% or less, or 12% or less, as measured by WAXS (Wide-Angle X-ray Scattering).
- the alpha-olefin copolymer of the present invention exhibits crystallinity in a low range as in the above range.
- the crystallinity can be measured by WAXS (Wide-Angle X-ray Scattering). X-rays were transmitted through the sample using Xenocs' model name Xeuss 2.0 X-ray scattering equipment, and the scattering intensity (I(q)) according to the scattering vector (q) was measured. More specifically, the wide-angle X-ray scattering measurement (WAXS) was measured by placing the sample at a distance of about 0.7 m from the detector and incident X-rays, and a Pilatus3 300K (2D detector) was used as the detector. WAXS is a parallel beam method, which measures the interference of X-rays generated by colliding with a sample during transmission. By assigning peaks resulting from the crystal structure, it is possible to determine how much the area of the crystalline peak occupies compared to the total area. Calculate the degree of crystallinity.
- WAXS Wide-Angle X-ray Scattering
- the scattering or diffraction intensity (I(q)) according to the scattering vector (q) obtained through WAXS was measured and analyzed.
- the diffraction peaks by Amorphous halo (Ia(q)), Mesophase (Im(q)), and Crystal (Ic(q)) were deconvolved from the obtained scattering or diffraction intensity, and through this, the crystallinity was determined according to the following [General Equation 3] Calculated.
- Ia is an amorphous halo peak.
- the crystallinity of the ethylene/alpha-olefin copolymer of the present invention is within the above range, the relative amorphous content in the copolymer increases to increase the absorbability of the crosslinking agent component, and therefore, impregnation of the crosslinking agent component within a short period of time is possible.
- the ethylene/alpha-olefin copolymer of the present invention may have a hardness (shore A) of 65 or less, specifically, 63 or less, 62 or less, or 61 or less, as measured at 40°C.
- the hardness represents Shore A hardness according to ASTM D 2240 standard. Since the ethylene/alpha-olefin copolymer of the present invention contains a large amount of amorphous region and has a high impregnation rate of polar substances such as crosslinking agents, it is measured at an impregnation temperature of 40 ° C. One hardness appears as a low value as described above.
- the hardness (shore A) of the ethylene/alpha-olefin copolymer of the present invention measured at 40° C. is within the above range, it is easy for the crosslinking agent component to penetrate into the ethylene/alpha-olefin copolymer, so that the impregnation time of the crosslinking agent component is reduced. There are advantages to shortening.
- the ethylene/alpha-olefin copolymer of the present invention has a melting temperature (Tm) of 70° C. or less, specifically, 65° C. or less, 60° C. or less, 58° C. or less, 45° C. or less, as measured by differential scanning calorimetry (DSC). ° C or higher, may be 50 ° C or higher.
- the melting temperature of the ethylene/alpha-olefin copolymer of the present invention is within the above range, it exhibits excellent thermal stability and does not exhibit a decrease in light transmittance due to a high crystalline region having a high melting temperature, so the light transmittance is realized at an excellent level.
- the melting temperature is measured using differential scanning calorimetry (DSC). Specifically, the copolymer is heated to 150°C, maintained for 5 minutes, lowered to 20°C, and the temperature is increased again. At this time, the rate of rise and fall of the temperature is adjusted to 10 ° C./min, respectively, and the result measured in the section where the second temperature rises can be measured as the melting temperature.
- DSC differential scanning calorimetry
- the ethylene/alpha-olefin copolymer of the present invention is a low-density polymer having a density ranging from 0.85 to 0.89 g/cc, wherein the density may mean a density measured according to ASTM D-792. Specifically, the density may be 0.850 g/cc or more, 0.860 g/cc or more, or 0.870 g/cc or more, or 0.874 g/cc or more, and 0.890 g/cc or less, or 0.880 g/cc or less, 0.878 g/cc or less. cc or less.
- the ethylene/alpha-olefin copolymer of the present invention has a density within the above range, it can be usefully used as an insulating material because physical properties such as volume resistance and light transmittance are not deteriorated while exhibiting excellent crosslinkability.
- the ethylene/alpha-olefin copolymer of the present invention has a melt index (MI, 190°C, 2.16 kg load conditions) of 1 to 30 dg/min.
- the melt index may be 1 dg/min or more, 2 dg/min or more, 3 dg/min or more, or 4 dg/min or more, and 30 dg/min or less, 20 dg/min or less, or 15 dg/min or less. min or less.
- the ethylene/alpha-olefin copolymer of the present invention has a melt index within the above range, it can be usefully used as an insulating material because of its excellent volume resistance and light transmittance while exhibiting an appropriate production rate.
- the ethylene/alpha-olefin copolymer of the present invention has a melt flow rate (MFRR, Melt Flow Rate Ratio, MI 10 /MI 2.16 ) may be 8.0 or less, specifically 4.0 or more, 4.2 or more, 4.5 or more, 8.0 or less, or 7.5 or less.
- the melt flow index is an index of the degree of long-chain branching of the copolymer, and the ethylene/alpha-olefin copolymer of the present invention satisfies the melt flow index along with the above-described properties, and is suitable for solar cell encapsulant compositions with excellent physical properties can be applied
- the ethylene/alpha-olefin copolymer of the present invention when it has a low melt index of 1 to 100 dg/min as described above, it may have a low melt flow index of 8.0 or less as described above. Since the copolymer of the present invention has such a low melt index and melt flow index, the copolymer has a high molecular weight and a low long-chain branch content, so it has an excellent degree of crosslinking.
- the ethylene/alpha-olefin copolymer of the present invention is prepared by copolymerizing ethylene and an alpha-olefin monomer, wherein the alpha-olefin, which means the part derived from the alpha-olefin monomer in the copolymer, is C4 to C20 of alpha-olefins, specifically propylene, 1-butene, 1-pentene, 4-methyl-1-pentene, 1-hexene, 1-heptene, 1-octene, 1-decene, 1-undecene, 1-dodecene , 1-tetradecene, 1-hexadecene, 1-eicosene, and the like, and one of them may be used alone or in a mixture of two or more.
- the alpha-olefin may be 1-butene, 1-hexene or 1-octene, preferably 1-butene, 1-hexene or a combination thereof.
- the content of alpha-olefin in the ethylene / alpha-olefin copolymer may be appropriately selected within a range that satisfies the above physical property requirements, specifically, more than 0 and 99 mol%, 10 mol% or more, 50 It may be mol% or less, but is not limited thereto.
- the ethylene/alpha-olefin copolymer of the present invention is prepared by a manufacturing method comprising introducing a transition metal compound, a cocatalyst, ethylene and an alpha-olefin monomer into a polymerization reactor, and polymerizing the copolymer.
- a method for polymerizing the ethylene and alpha-olefin monomers is not particularly limited, and conventional methods widely used in the art may be appropriately used.
- the alpha-olefin monomers are propylene, 1-butene, 1-pentene, 4-methyl-1-pentene, 1-hexene, 1-heptene, 1-octene, 1-decene, 1-undecene, It may be at least one selected from the group consisting of 1-dodecene, 1-tetradecene, 1-hexadecene, and 1-eicosene, but is not limited thereto.
- the alpha-olefin monomer may be 1-butene, 1-hexene or 1-octene.
- the molar ratio of ethylene and alpha-olefin monomers is 1:1.14 to 1:3.00, specifically 1:1.14 to 1:2.00, 1:1.14 to 1:1.50, 1:1.14 to 1:1.30, or 1:1.14 to 1:1.25.
- the molar ratio of ethylene and alpha-olefin monomers is within the above range, an ethylene/alpha-olefin copolymer having a high proportion of amorphous regions due to a large number of alpha-olefin monomers is produced, and at the same time, alpha-olefin monomers are too high. If it is used a lot, the crystalline region is too low, making it difficult to process due to film sagging during film production, and the rigidity of the film is lowered after production, and it is sticky on the surface, making it difficult to store.
- transition metal compound used for polymerization may be a compound represented by Formula 1 below, a compound represented by Formula 2 below, or a combination thereof, but is not limited thereto.
- R 1 is hydrogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; alkenyl of 2 to 20 carbon atoms; alkoxy having 1 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; arylalkoxy having 7 to 20 carbon atoms; Alkylaryl having 7 to 20 carbon atoms; Or an arylalkyl having 7 to 20 carbon atoms,
- R 2 and R 3 are each independently hydrogen; halogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; alkenyl of 2 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; Alkylaryl having 7 to 20 carbon atoms; arylalkyl having 7 to 20 carbon atoms; Alkylamido having 1 to 20 carbon atoms; or an arylamido having 6 to 20 carbon atoms;
- R 4 and R 5 are each independently hydrogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; or alkenyl having 2 to 20 carbon atoms;
- R 6 to R 9 are each independently hydrogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; or alkenyl having 2 to 20 carbon atoms;
- Two or more of R 6 to R 9 adjacent to each other may be connected to each other to form a ring
- Q 1 is Si, C, N, P or S
- M 1 is Ti, Hf or Zr
- X 1 and X 2 are each independently hydrogen; halogen; Alkyl having 1 to 20 carbon atoms; alkenyl of 2 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; Alkylaryl having 7 to 20 carbon atoms; arylalkyl having 7 to 20 carbon atoms; Alkylamino having 1 to 20 carbon atoms; or arylamino having 6 to 20 carbon atoms;
- R 10 is hydrogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; alkenyl of 2 to 20 carbon atoms; alkoxy having 1 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; arylalkoxy having 7 to 20 carbon atoms; Alkylaryl having 7 to 20 carbon atoms; Or an arylalkyl having 7 to 20 carbon atoms,
- R 11a to R 11e are each independently hydrogen; halogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; alkenyl of 2 to 20 carbon atoms; alkoxy having 1 to 20 carbon atoms; or an aryl having 6 to 20 carbon atoms;
- R 12 is hydrogen; halogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; alkenyl of 2 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; Alkylaryl having 7 to 20 carbon atoms; arylalkyl having 7 to 20 carbon atoms; Alkylamido having 1 to 20 carbon atoms; or an arylamido having 6 to 20 carbon atoms;
- R 13 and R 14 are each independently hydrogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; or alkenyl having 2 to 20 carbon atoms;
- R 15 to R 18 are each independently hydrogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; or alkenyl having 2 to 20 carbon atoms;
- Two or more of R 15 to R 18 adjacent to each other may be connected to each other to form a ring
- Q 2 is Si, C, N, P or S
- M 2 is Ti, Hf or Zr
- X 3 and X 4 are each independently hydrogen; halogen; Alkyl having 1 to 20 carbon atoms; alkenyl of 2 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; Alkylaryl having 7 to 20 carbon atoms; arylalkyl having 7 to 20 carbon atoms; Alkylamino having 1 to 20 carbon atoms; or arylamino having 6 to 20 carbon atoms.
- the transition metal compound represented by Formula 1 and the transition metal compound represented by Formula 2 are cyclopentadiene in which benzothiophene is fused by a cyclic bond, and an amido group (NR 1 , NR 10 ) It is stably cross-linked by Q 1 or Q 2 and forms a structure in which Group 4 transition metals are coordinated.
- the transition metal compound represented by Formula 1 When the transition metal compound represented by Formula 1 is used as a catalyst for polymerization of ethylene and alpha-olefin monomers, it is possible to prepare copolymers with high activity, high molecular weight, and high copolymerizability even at high polymerization temperatures. do. In particular, due to the structural characteristics of the catalyst, it is difficult to introduce an alpha-olefin monomer, and a high-density copolymer tends to be produced. On the other hand, since a large amount of alpha-olefin can be introduced into the transition metal compound of Chemical Formula 2, a polymer (elastomer) of an ultra-low density region can also be prepared.
- the transition metal compound prepared by Formula 1 or 2 used in the present invention is mixed and used in the catalyst composition.
- an alpha-olefin monomer Since the copolymerizability of incorporating is different, when a copolymer is prepared by mixing them, a copolymer having both a low-density region in which a large amount of alpha-olefin monomer is incorporated and a high-density region in which a small amount of alpha-olefin monomer is incorporated can be prepared.
- the free volume is low due to the high crystallinity distribution of the copolymer, and thus, since the charge mobility is low, it exhibits excellent physical properties with high electrical insulation properties.
- the molar ratio of the transition metal compound represented by Formula 1 and Formula 2 is 1:1.2 to 1:10, or 1:1.5 to 1:9, or 1:1.5 to 1:7, 1:2 to 1 :7, 1:2 to 1:5, or 1:2 to 1:3.
- transition metal compound represented by Formula 1 When the transition metal compound represented by Formula 1 is used alone, or when the transition metal compound represented by Formula 1 is excessive outside the molar ratio, or when the transition metal compound represented by Formula 2 is used alone, or outside the molar ratio When the transition metal compound represented by Chemical Formula 2 is excessive, a copolymer having poor electrical insulation properties due to low crystallinity distribution may be produced.
- the polymerization reaction may be carried out by continuously polymerizing ethylene and alpha-olefin monomers by continuously adding hydrogen in the presence of the catalyst composition, and specifically, while introducing hydrogen at 10 to 100 cc/min may be performed.
- the hydrogen gas suppresses a rapid reaction of the transition metal compound at the initial stage of polymerization and serves to terminate the polymerization reaction. Accordingly, an ethylene/alpha-olefin copolymer having a narrow molecular weight distribution can be effectively produced by using such hydrogen gas and adjusting the amount thereof.
- the hydrogen may be introduced at 10 cc/min or more, or 15 cc/min or more, or 19 cc/min or more, or 22 cc/min or more, and at the same time, 100 cc/min or less, or 50 cc/min or less. min or less, or 45 cc/min or less, or 35 cc/min or less, or 29 cc/min or less.
- the produced ethylene/alpha-olefin polymer can realize the physical properties in the present invention.
- the polymerization reaction is not uniformly terminated, making it difficult to prepare an ethylene/alpha-olefin copolymer having desired properties.
- the termination reaction occurs too quickly, and there is a concern that an ethylene/alpha-olefin copolymer having a very low molecular weight may be produced.
- the polymerization reaction can be carried out at 100 to 200 ° C., and the number of unsaturated functional groups and molecular weight distribution in the ethylene/alpha-olefin copolymer can be more easily controlled by controlling the polymerization temperature together with the amount of hydrogen input.
- the polymerization reaction may be carried out at 100 to 200 °C, 120 to 180 °C, 130 to 170 °C, 135 to 150 °C.
- R 1 is hydrogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; alkenyl of 2 to 20 carbon atoms; alkoxy having 1 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; arylalkoxy having 7 to 20 carbon atoms; Alkylaryl having 7 to 20 carbon atoms; or arylalkyl having 7 to 20 carbon atoms, more specifically, R 1 is methyl, ethyl, propyl, butyl, isobutyl, tbutyl, isopropyl, cyclohexyl, benzyl, phenyl, methoxyphenyl, ethoxyphenyl, fluorine phenyl, bromophenyl, chlorophenyl, dimethylphenyl or diethylphenyl.
- R 2 and R 3 are each independently hydrogen; halogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; alkenyl of 2 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; Alkylaryl having 7 to 20 carbon atoms; arylalkyl having 7 to 20 carbon atoms; Alkylamido having 1 to 20 carbon atoms; Or an arylamido having 6 to 20 carbon atoms, and more specifically, the R 2 and R 3 are each independently hydrogen; Alkyl having 1 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; Alkylaryl having 6 to 20 carbon atoms; or arylalkyl having 7 to 20 carbon atoms.
- R 4 and R 5 are the same as or different from each other, and each independently hydrogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; or alkenyl having 2 to 20 carbon atoms, and more specifically, alkyl having 1 to 6 carbon atoms. More specifically, the R 4 and R 5 may be methyl, ethyl or propyl.
- R 6 to R 9 are the same as or different from each other, and each independently hydrogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; or alkenyl of 2 to 20 carbon atoms. More specifically, R 6 to R 9 are the same as or different from each other, and each independently may be hydrogen or methyl.
- R 6 to R 9 adjacent to each other may be connected to each other to form an aliphatic ring having 5 to 20 carbon atoms or an aromatic ring having 6 to 20 carbon atoms, and the aliphatic ring or aromatic ring may be a halogen or a carbon atom 1 to 20. It may be substituted with an alkyl of 20 carbon atoms, an alkenyl of 2 to 20 carbon atoms or an aryl of 6 to 20 carbon atoms.
- Q 1 may be Si, C, N, P, or S, and more specifically, Q 1 may be Si.
- M 1 may be Ti, Hf, or Zr.
- X 1 and X 2 are the same as or different from each other, and each independently hydrogen; halogen; Alkyl having 1 to 20 carbon atoms; alkenyl of 2 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; Alkylaryl having 7 to 20 carbon atoms; arylalkyl having 7 to 20 carbon atoms; Alkylamino having 1 to 20 carbon atoms; or arylamino having 6 to 20 carbon atoms.
- the compound represented by Formula 1 may be a compound represented by any one of the following formulas.
- R 10 is hydrogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; alkenyl of 2 to 20 carbon atoms; alkoxy having 1 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; arylalkoxy having 7 to 20 carbon atoms; Alkylaryl having 7 to 20 carbon atoms; or an arylalkyl having 7 to 20 carbon atoms, and more specifically, R 10 is hydrogen; alkyl having 1 to 20 carbon atoms or 1 to 12 carbon atoms; alkoxy having 1 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; arylalkoxy having 7 to 20 carbon atoms; Alkylaryl having 7 to 20 carbon atoms; or arylalkyl having 7 to 20 carbon atoms.
- R 11a to R 11e are each independently hydrogen; halogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; alkenyl of 2 to 20 carbon atoms; alkoxy having 1 to 20 carbon atoms; Or an aryl having 6 to 20 carbon atoms, more specifically, hydrogen; halogen; Alkyl having 1 to 12 carbon atoms; Cycloalkyl having 3 to 12 carbon atoms; alkenyl having 2 to 12 carbon atoms; alkoxy having 1 to 12 carbon atoms; or phenyl.
- R 12 is hydrogen; halogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; alkenyl of 2 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; Alkylaryl having 7 to 20 carbon atoms; arylalkyl having 7 to 20 carbon atoms; Alkylamido having 1 to 20 carbon atoms; Or an arylamido having 6 to 20 carbon atoms, more specifically, hydrogen; halogen; Alkyl having 1 to 12 carbon atoms; Cycloalkyl having 3 to 12 carbon atoms; alkenyl having 2 to 12 carbon atoms; or phenyl.
- R 13 and R 14 are each independently hydrogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; or alkenyl having 2 to 20 carbon atoms, more specifically, hydrogen; or an alkyl having 1 to 12 carbon atoms.
- R 15 to R 18 are each independently hydrogen; Alkyl having 1 to 20 carbon atoms; Cycloalkyl having 3 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; or alkenyl having 2 to 20 carbon atoms, more specifically, hydrogen; Alkyl having 1 to 12 carbon atoms; or cycloalkyl of 3 to 12 carbon atoms, or hydrogen; or methyl.
- two or more of R 15 to R 18 adjacent to each other may be connected to each other to form a ring.
- Q 2 may be Si, C, N, P or S, and more specifically, Q 2 may be Si.
- X 3 and X 4 are each independently hydrogen; halogen; Alkyl having 1 to 20 carbon atoms; alkenyl of 2 to 20 carbon atoms; aryl of 6 to 20 carbon atoms; Alkylaryl having 7 to 20 carbon atoms; arylalkyl having 7 to 20 carbon atoms; Alkylamino having 1 to 20 carbon atoms; or arylamino having 6 to 20 carbon atoms, specifically, hydrogen; halogen; Alkyl having 1 to 12 carbon atoms; Cycloalkyl having 3 to 12 carbon atoms; Or it may be an alkenyl having 2 to 12 carbon atoms, more specifically, hydrogen; or an alkyl having 1 to 12 carbon atoms.
- the compound represented by Chemical Formula 2 may be specifically any one of the compounds represented by Chemical Formulas 2-1 to 2-10.
- the alpha-olefin monomer which is a comonomer
- the alpha-olefin monomer may be an olefin monomer having 4 to 20 carbon atoms.
- Specific examples include propylene, 1-butene, 1-pentene, 4-methyl-1-pentene, 1-hexene, 1-heptene, 1-octene, 1-decene, 1-undecene, 1-dodecene, 1-tetra decene, 1-hexadecene, or 1-eicosene, and the like, and one of them alone or a mixture of two or more may be used.
- the alpha-olefin monomer may be 1-butene, 1-hexene or 1-octene, and most preferably 1-butene.
- the content of the alpha-olefin-based monomer may be appropriately selected within a range that satisfies the above physical property requirements, and specifically may be greater than 0 and 99 mol% or less, or 10 to 50 mol%.
- the present invention provides a composition for an encapsulant film comprising the ethylene/alpha-olefin copolymer.
- a modified resin composition for example, a silane-modified resin composition or an amino-silane-modified resin composition, may be prepared using the composition for an encapsulant film.
- the composition for the encapsulant film may include a known crosslinking agent, a crosslinking aid, a silane coupling agent, and the like, in addition to the above-described ethylene/alpha-olefin copolymer.
- the crosslinking agent is a radical initiator in the step of preparing the silane-modified resin composition, and may serve to initiate a reaction in which an unsaturated silane compound is grafted into the resin composition.
- a cross-linking between the silane-modified resin composition or between the silane-modified resin composition and the non-modified resin composition in the step of lamination in the manufacture of an opto-electronic device heat resistance and durability of a final product, such as an encapsulant sheet, can be improved. there is.
- crosslinking agent is a crosslinkable compound capable of initiating radical polymerization of a vinyl group or forming a crosslinking bond
- various crosslinking agents known in the art may be used, for example, organic peroxides, hydroperoxides and azo compounds One or two or more selected from the group consisting of may be used.
- the organic peroxide may be an organic peroxide having a 1-hour half-life temperature of 120 to 135°C, for example, 120 to 130°C, 120 to 125°C, preferably 121°C.
- the "1-hour half-life temperature” means a temperature at which the half-life of the crosslinking agent is 1 hour.
- the temperature at which the radical initiation reaction efficiently occurs is different, and therefore, when an organic peroxide having a 1-hour half-life temperature in the above range is used as a crosslinking agent, a lamination process temperature for manufacturing an optoelectronic device
- a radical initiation reaction, that is, a crosslinking reaction can proceed effectively.
- the crosslinking agent is included in an amount of 0.01 to 1 part by weight, for example, 0.05 to 0.55, 0.1 to 0.5, or 0.15 to 0.45 part by weight, based on 100 parts by weight of the composition for the encapsulant film, and the crosslinking agent is less than 0.01 part by weight.
- the effect of improving heat resistance properties is insignificant, and when included in an amount exceeding 1 part by weight, the formability of the encapsulant sheet is reduced, which may cause a problem in that process restrictions occur, and may affect the physical properties of the encapsulant.
- the resin composition may include a crosslinking aid in addition to the crosslinking agent.
- a crosslinking assistant in addition to the crosslinking agent, the degree of crosslinking between the resin compositions by the above-described crosslinking agent can be increased, and accordingly, heat resistance and durability of a final product, for example, an encapsulant sheet, can be further improved.
- crosslinking aid various crosslinking aids known in the art may be used.
- a compound containing at least one unsaturated group such as an allyl group or a (meth)acryloxy group may be used.
- allyl group-containing compound examples include polyallyl compounds such as triallyl isocyanurate (TAIC), triallyl cyanurate, diallyl phthalate, diallyl fumarate, or diallyl maleate.
- the compound containing the (meth)acryloxy group may be, for example, poly(meth)acryloxy compounds such as ethylene glycol diacrylate, ethylene glycol dimethacrylate, and trimethylolpropane trimethacrylate. However, it is not particularly limited thereto.
- the crosslinking aid is included in an amount of 0.01 to 0.5 parts by weight, for example, 0.01 to 0.3, 0.015 to 0.2 or 0.016 to 0.16 parts by weight, based on 100 parts by weight of the composition for the encapsulant film, and the crosslinking aid is 0.01 parts by weight
- the effect of improving heat resistance properties is insignificant, when included in excess of 0.5 parts by weight, a problem affecting the physical properties of a final product, for example, an encapsulant sheet may occur and production cost may increase.
- composition for the encapsulant film may further include a silane coupling agent in addition to the ethylene/alpha-olefin copolymer, the crosslinking agent, and the crosslinking aid.
- silane coupling agent examples include N-( ⁇ -aminoethyl)- ⁇ -aminopropyltrimethoxysilane, N-( ⁇ -aminoethyl)- ⁇ -aminopropylmethyldimethoxysilane, and ⁇ -amino At least one selected from the group consisting of propyltriethoxysilane, ⁇ -glycidoxypropyltrimethoxysilane, and ⁇ -methacryloxypropyltrimethoxysilane (MEMO) may be used.
- the silane coupling agent may be included in an amount of 0.1 to 0.4 parts by weight based on 100 parts by weight of the composition for an encapsulant film. When used less than 0.3, adhesion to glass is poor during solar module manufacturing, making it easy to absorb water, so long-term performance of the module cannot be guaranteed.
- composition for the encapsulant film may further include an unsaturated silane compound or an amino silane compound.
- the unsaturated silane compound may be grafted onto the main chain including the polymerization unit of the copolymer of the present invention in the presence of a radical initiator, etc., and included in a silane-modified resin composition or an amino silane-modified resin composition in a polymerized form.
- the unsaturated silane compound is vinyltrimethoxy silane, vinyltriethoxy silane, vinyltripropoxy silane, vinyltriisopropoxy silane, vinyltributoxy silane, vinyltripentoxy silane, vinyltriphenoxy silane, or vinyl It may be triacetoxy silane or the like, and as an example, vinyltrimethoxy silane or vinyltriethoxy silane may be used, but is not limited thereto.
- the amino silane compound is an unsaturated silane compound grafted on the main chain of the copolymer in the step of grafting modification of the ethylene/alpha-olefin copolymer, for example, a hydroxyl group that converts a reactive functional group such as an alkoxy group of vinyltriethoxysilane into a hydroxyl group.
- a hydroxyl group that converts a reactive functional group such as an alkoxy group of vinyltriethoxysilane into a hydroxyl group.
- the amino silane compound may also participate as a reactant in the direct copolymerization reaction, thereby providing a moiety having an amine functional group to the amino silane-modified resin composition.
- the amino silane compound is a silane compound containing an amine group, and is not particularly limited as long as it is a primary amine or a secondary amine.
- amino silane compound aminotrialkoxysilane, aminodialkoxysilane, etc. may be used. Examples include 3-aminopropyltrimethoxysilane (APTMS) and 3-aminopropyltriethoxysilane.
- the content of the unsaturated silane compound and/or amino silane compound is not particularly limited.
- composition for the encapsulant film may further include one or more additives selected from a light stabilizer, a UV absorber, and a heat stabilizer, if necessary.
- the light stabilizer may serve to prevent photooxidation by capturing active species at the onset of photodegradation of the resin, depending on the application of the composition.
- the type of light stabilizer that can be used is not particularly limited, and known compounds such as hindered amine-based compounds or hindered piperidine-based compounds can be used.
- the UV absorber may absorb ultraviolet rays from sunlight and convert them into harmless thermal energy in molecules according to the use of the composition, thereby preventing the excitation of active species for initiating photodegradation in the resin composition.
- Specific types of UV absorbers that can be used are not particularly limited, and examples include inorganic UV absorbers such as benzophenone, benzotriazole, acrylonitrile, metal complex salts, hindered amines, ultrafine titanium oxide or ultrafine zinc oxide.
- inorganic UV absorbers such as benzophenone, benzotriazole, acrylonitrile, metal complex salts, hindered amines, ultrafine titanium oxide or ultrafine zinc oxide.
- One type or a mixture of two or more types of absorbents and the like can be used.
- thermal stabilizer examples include tris (2,4-di-tert-butylphenyl) phosphite, bis [2,4-bis (1,1-dimethylethyl) -6-methylphenyl] ethyl ester phosphorous acid, tetrakis (2,4-di-tert-butylphenyl)[1,1-biphenyl]-4,4'-diylbisphosphonate and bis(2,4-di-tert-butylphenyl)pentaerythritol diphosphite, etc.
- phosphorus-based heat stabilizers such as reaction products of 8-hydroxy-5,7-di-tert-butyl-furan-2-one and o-xylene. One or two or more of these may be used. there is.
- the content of the light stabilizer, UV absorber and/or heat stabilizer is not particularly limited. That is, the content of the additive may be appropriately selected in consideration of the use of the resin composition, the shape or density of the additive, and is usually within the range of 0.01 to 5 parts by weight based on 100 parts by weight of the total solid content of the composition for an encapsulant film. can be properly adjusted.
- composition for an encapsulant film of the present invention may appropriately additionally include various additives known in the related art according to the application to which the resin component is applied in addition to the above components.
- composition for the encapsulant film can be molded by injection, extrusion, etc. and used as various molded products, and specifically, as an encapsulant for encapsulating elements in various optoelectronic devices, such as solar cells. It can be used, for example, it can also be used as an industrial material applied to an elevated temperature lamination process, but the use is not limited thereto.
- the ligand compound (1.06g, 3.22mmol/1.0eq) and MTBE 16.0mL (0.2M) were put in a 50ml Schlenk flask and stirred first. At -40°C, n-BuLi (2.64ml, 6.60mmol/2.05eq, 2.5M in THF) was added and reacted overnight at room temperature. Then, after slowly adding MeMgBr (2.68ml, 8.05 mmol/2.5eq, 3.0M in diethyl ether) dropwise at -40°C, TiCl 4 (2.68ml, 3.22 mmol/1.0eq, 1.0M in toluene) was added in that order. It was reacted overnight at room temperature. The reaction mixture was then filtered through Celite using hexane. After solvent drying, a brown solid was obtained in a yield of 1.07 g (82%).
- the stirred Li-complex THF solution was cannulated into a Schlenk flask containing 8.1 mL (1.0 eq, 49.925 mmol) of dichloro(methyl)(phenyl)silane and 70 mL of THF at -78°C, followed by stirring at room temperature overnight. After stirring and vacuum drying, the mixture was extracted with 100 mL of hexane.
- An ethylene/alpha-olefin copolymer was prepared in the same manner as in Example 1, except that polymerization conditions were changed as shown in Table 1 below.
- Example 1 0.150 0.30 0.045 0.87 1.09 7.0 20 135
- Example 2 0.145 0.29 0.050 0.87 1.02 7.0 18 135
- Example 3 0.150 0.30 0.050 0.87 1.05 7.0 18 135
- Example 4 0.150 0.30 0.045 0.87 1.00 7.0 11 134
- Comparative Example 1 0.150 0.30 0.050 0.87 0.85 7.0 16 136
- Comparative Example 2 0.150 0.30 0.050 0.87 0.90 7.0 17 135
- Comparative Example 3 0.150 0.30 0.050 0.87 0.97 7.0 18 134
- Comparative Example 4 0.145 0.29 0.045 0.87 0.95 7.0 10 135 Comparative Example 5 0.150 0.30 0.055 0.87 0.97 7.0 8 138
- MI 10 190 °C, 10 kg load condition
- MI 2.16 190 °C, 2.16 kg load condition
- DSC 6000 Differential Scanning Calorimeter manufactured by PerkinElmer. Specifically, by using DSC, the temperature of the copolymer is increased to 150 ° C. under a nitrogen atmosphere and maintained for 1 minute, The DSC curve was observed while cooling to -100°C and then increasing the temperature to 150°C. At this time, the heating rate and cooling rate were each set to 10°C/min.
- the ethylene/alpha-olefin copolymer was placed in a 1T square frame, and the front and rear surfaces were covered with 3T steel plates, and then put into a high-temperature press. 190 °C, 25 N / cm 2 for 240 seconds, 6 times reduced pressure / pressure degassing 190 °C, 151 N / cm 2 for 240 seconds continuously, then cooled to 30 °C while lowering 15 °C per minute, at this time The pressure was maintained at 151 N/cm 2 . 30 °C, 151 N / cm 2 maintained for 300 seconds to complete the preparation of the specimen.
- q is a scattering vector
- ⁇ is a value of 1/2 the scattering angle
- ⁇ is the wavelength of the irradiated X-ray.
- the distance of the crystal domain was analyzed by measuring the scattering intensity (I(q)) according to the scattering vector (q) obtained through SAXS.
- the measured scattering intensity (I(q)) is multiplied by the square of the scattering vector (q), and a peak is observed in a graph of I(q) ⁇ q 2 according to the scattering vector (q).
- a distance (d-spacing) between crystal domains was obtained using the scattering vector value (q*) of the observed peak.
- the q* represents the scattering vector value at the peak of the graph of I(q) ⁇ q 2 according to the scattering vector (q).
- Xenocs’ model name Xeuss 2.0 X-ray scattering equipment was used to transmit X-rays through the sample, and the scattering intensity according to the scattering vector (q) (I(q)) was measured.
- the sample was placed about 0.7 m away from the detector and measured by incident X-rays, and a Pilatus3 300K (2D detector) was used as the detector.
- WAXS is a parallel beam method, which measures the interference of X-rays generated by colliding with a sample during transmission. By assigning peaks resulting from the crystal structure, it is possible to determine how much the area of the crystalline peak occupies compared to the total area. Calculate the degree of crystallinity.
- the scattering or diffraction intensity (I(q)) according to the scattering vector (q) obtained through WAXS was measured and analyzed. From the obtained scattering or diffraction intensity, the diffraction peaks by Amorphous halo (Ia(q)), Mesophase (Im(q)), and Crystal (Ic(q)) were deconvolved. Specifically, the deconvolution of the diffraction peak was performed using Gaussian and Lorentzian functions. were combined and defined according to the following method.
- Amorphous halo (1 in FIG. 1) is defined as the sum of three Gaussian functions (2 in FIG. 1).
- the three Gaussian functions have peak centers at scattering vectors of 0.943 ⁇ -1 , 1.369 ⁇ -1 , and 1.812 ⁇ -1 , respectively.
- Ia is an amorphous halo peak.
- the ethylene/alpha-olefin copolymer was placed in a 3T square frame, and the front and rear surfaces were covered with 3T steel plates, and then put into a high-temperature press. 190 °C, 25 N / cm 2 (240) seconds, reduced pressure / pressure degassing 6 times, 190 °C 151 N / cm 2 continuously treated for 240 seconds, then cooled to 30 °C while lowering 15 °C per minute, at this time The pressure was maintained at 151 N/cm 2 . 30 °C, 151 N / cm 2 maintained for 300 seconds to complete the preparation of the specimen.
- Shore A hardness was measured according to ASTM D2240 using a portable hardness tester. At this time, since the sample temperature changes when the specimen is taken out of the oven, it was measured in a 40 ° C chamber for accurate measurement.
- Example 1 0.8716 16.1 6.8 57.5 12.3 9.4 62.2
- Example 2 0.8738 14.9 6.9 60.6 12.1 9.6 64.7
- Example 3 0.8731 14.7 6.9 59.3 12.2 9.8 63.9
- Example 4 0.8740 5.0 7.3 58.8 12.1 12.0 64.9
- Comparative Example 1 0.8770 12.9 6.8 65.1 11.5 15.1 68.4
- Comparative Example 2 0.8759 13.2 6.9 63.5 11.6 13.4 67.2
- Comparative Example 3 0.8745 14.4 6.8 61.4 12.0 12.7 65.5
- Comparative Example 4 0.8750 4.9 6.9 61.0 11.9 12.5 66.1 Comparative Example 5 0.8755 5.4 7.4 61.8 11.6 14.2 64.9
- the ethylene/alpha-olefin copolymer according to the present invention has a d-spacing of 12 nm or more, a crystallinity of 14%, a shore A hardness of 65 or less, and a melting temperature of 70 ° C or less. did
- a Planetary Mixer from Thermo Electron (Karlsruhe) GmbH was used for impregnation of the crosslinking agent.
- TBEC t-butyl 1-(2-ethylhexyl)monoperoxycarbonate
- TVSS tetrakis(vinyldimethylsiloxy)silane
- MEMO methacryloxypropyltrimethoxysilane
- the crosslinking agent Before the crosslinking agent is absorbed into the ethylene/alpha-olefin copolymer, it acts as a lubricant and maintains a low Torque value, but when the crosslinking agent is absorbed, the Torque value increases. .
- an encapsulant film having an average thickness of 550 ⁇ m was prepared using a microextruder at a low temperature (extruder barrel temperature of 100° C. or less) to the extent that high temperature crosslinking does not occur.
- the crosslinking degree was evaluated based on CPIA (China Photovoltaic Industry Association) standards and ASTM D2765. After cutting the prepared encapsulant film into 10 cm ⁇ 10 cm, vacuum lamination was performed at 150° C. for 20 minutes (vacuum for 5 minutes / pressure for 1 minute / pressure for 14 minutes) to obtain crosslinked specimens.
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Abstract
Description
Cat. | Cocat. | Tibal | C2 | 1-C4 | C6 | 수소 | 온도 | |
μmol/min | μmol/min | kg/h | kg/h | kg/h | cc/min | cc/min | ℃ | |
실시예 1 | 0.150 | 0.30 | 0.045 | 0.87 | 1.09 | 7.0 | 20 | 135 |
실시예 2 | 0.145 | 0.29 | 0.050 | 0.87 | 1.02 | 7.0 | 18 | 135 |
실시예 3 | 0.150 | 0.30 | 0.050 | 0.87 | 1.05 | 7.0 | 18 | 135 |
실시예 4 | 0.150 | 0.30 | 0.045 | 0.87 | 1.00 | 7.0 | 11 | 134 |
비교예 1 | 0.150 | 0.30 | 0.050 | 0.87 | 0.85 | 7.0 | 16 | 136 |
비교예 2 | 0.150 | 0.30 | 0.050 | 0.87 | 0.90 | 7.0 | 17 | 135 |
비교예 3 | 0.150 | 0.30 | 0.050 | 0.87 | 0.97 | 7.0 | 18 | 134 |
비교예 4 | 0.145 | 0.29 | 0.045 | 0.87 | 0.95 | 7.0 | 10 | 135 |
비교예 5 | 0.150 | 0.30 | 0.055 | 0.87 | 0.97 | 7.0 | 8 | 138 |
밀도(g/cc) | MI(dg/min) | MFRR | Tm(℃) | d-spacing(nm) | 결정화도(%) | 경도(shore A) |
|
실시예 1 | 0.8716 | 16.1 | 6.8 | 57.5 | 12.3 | 9.4 | 62.2 |
실시예 2 | 0.8738 | 14.9 | 6.9 | 60.6 | 12.1 | 9.6 | 64.7 |
실시예 3 | 0.8731 | 14.7 | 6.9 | 59.3 | 12.2 | 9.8 | 63.9 |
실시예 4 | 0.8740 | 5.0 | 7.3 | 58.8 | 12.1 | 12.0 | 64.9 |
비교예 1 | 0.8770 | 12.9 | 6.8 | 65.1 | 11.5 | 15.1 | 68.4 |
비교예 2 | 0.8759 | 13.2 | 6.9 | 63.5 | 11.6 | 13.4 | 67.2 |
비교예 3 | 0.8745 | 14.4 | 6.8 | 61.4 | 12.0 | 12.7 | 65.5 |
비교예 4 | 0.8750 | 4.9 | 6.9 | 61.0 | 11.9 | 12.5 | 66.1 |
비교예 5 | 0.8755 | 5.4 | 7.4 | 61.8 | 11.6 | 14.2 | 64.9 |
함침 완료 시간(분) | 가교도(%) | |
실시예 1 | 35 | 78.1 |
실시예 2 | 37 | 79.2 |
실시예 3 | 35 | 79.4 |
실시예 4 | 38 | 87.5 |
비교예 1 | 58 | 79.8 |
비교예 2 | 48 | 78.9 |
비교예 3 | 45 | 78.5 |
비교예 4 | 43 | 87.0 |
비교예 5 | 42 | 86.5 |
Claims (10)
- 하기 (a) 내지 (d) 조건을 충족하는 에틸렌/알파-올레핀 공중합체:(a) SAXS(Small-Angle X-Ray Scattering)로 측정한 d-spacing: 12 nm 이상;(b) WAXS(Wide-Angle X-ray Scattering)로 측정한 결정화도: 14% 이하;(c) 40℃ 조건에서 측정한 경도(shore A): 65 이하; 및(d) DSC(Differential Scanning calorimetry)로 측정한 용융 온도: 70℃ 이하.
- 청구항 1에 있어서,상기 결정화도는 13% 이하인 에틸렌/알파-올레핀 공중합체.
- 청구항 1에 있어서,상기 경도(shore A)는 63 이하인 에틸렌/알파-올레핀 공중합체.
- 청구항 1에 있어서,상기 용융 온도는 50 내지 65℃인 에틸렌/알파-올레핀 공중합체.
- 청구항 1에 있어서,밀도가 0.85 내지 0.89 g/cc인 에틸렌/알파-올레핀 공중합체.
- 청구항 1에 있어서,용융 지수(Melt Index, MI, 190℃, 2.16 kg 하중 조건)가 1 내지 100 dg/min인 에틸렌/알파-올레핀 공중합체.
- 청구항 1에 있어서,용융 지수(MI2.16, 190℃, 2.16 kg 하중 조건)에 대한 용융 지수(MI10, 190℃, 10 kg 하중 조건) 값인 용융 유동 지수(MFRR, Melt Flow Rate Ratio, MI10/MI2.16)가 8.0 이하인 에틸렌/알파-올레핀 공중합체.
- 청구항 1에 있어서,상기 알파-올레핀은 프로필렌, 1-부텐, 1-펜텐, 4-메틸-1-펜텐, 1-헥센, 1-헵텐, 1-옥텐, 1-데센, 1-운데센, 1-도데센, 1-테트라데센, 1-헥사데센 및 1-에이코센으로 이루어진 군에서 선택된 1종 이상을 포함하는 것인 에틸렌/알파-올레핀 공중합체.
- 청구항 1에 있어서,상기 알파-올레핀은 에틸렌/알파-올레핀 공중합체 기준 0 초과 99 이하 몰%로 포함되는 에틸렌/알파-올레핀 공중합체.
- 청구항 1 내지 9 중 어느 한 항의 에틸렌/알파-올레핀 공중합체를 포함하는 봉지재 필름용 조성물.
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EP22887696.7A EP4265655A1 (en) | 2021-11-01 | 2022-10-28 | Ethylene/alpha-olefin copolymer and composition for sealant film comprising same |
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JP2012126909A (ja) * | 2004-12-28 | 2012-07-05 | Mitsui Chemicals Tohcello Inc | 太陽電池封止材 |
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KR20210128325A (ko) * | 2020-04-16 | 2021-10-26 | 주식회사 엘지화학 | 전기 절연성이 우수한 에틸렌/알파-올레핀 공중합체 |
KR20210128319A (ko) * | 2020-04-16 | 2021-10-26 | 주식회사 엘지화학 | 전기 절연성이 우수한 에틸렌/알파-올레핀 공중합체 |
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CN117567961A (zh) * | 2024-01-15 | 2024-02-20 | 万华化学集团股份有限公司 | 一种光伏胶膜用乙烯/α-烯烃无规共聚物及其应用 |
CN117567961B (zh) * | 2024-01-15 | 2024-04-09 | 万华化学集团股份有限公司 | 一种光伏胶膜用乙烯/α-烯烃无规共聚物及其应用 |
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