JP7475139B2 - 特性が改善されたインフレーションフィルム - Google Patents
特性が改善されたインフレーションフィルム Download PDFInfo
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- JP7475139B2 JP7475139B2 JP2019515242A JP2019515242A JP7475139B2 JP 7475139 B2 JP7475139 B2 JP 7475139B2 JP 2019515242 A JP2019515242 A JP 2019515242A JP 2019515242 A JP2019515242 A JP 2019515242A JP 7475139 B2 JP7475139 B2 JP 7475139B2
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- Prior art keywords
- ethylene
- film
- composition
- melt index
- polyethylene
- Prior art date
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- 239000000203 mixture Substances 0.000 claims description 143
- -1 polyethylene Polymers 0.000 claims description 123
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 121
- 239000005977 Ethylene Substances 0.000 claims description 121
- 229920000642 polymer Polymers 0.000 claims description 84
- 239000004698 Polyethylene Substances 0.000 claims description 80
- 229920000573 polyethylene Polymers 0.000 claims description 78
- 239000004711 α-olefin Substances 0.000 claims description 34
- 238000009826 distribution Methods 0.000 claims description 33
- 239000000155 melt Substances 0.000 claims description 28
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 26
- 229920002554 vinyl polymer Polymers 0.000 claims description 26
- 125000004432 carbon atom Chemical group C* 0.000 claims description 13
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 230000001747 exhibiting effect Effects 0.000 claims 1
- 239000010410 layer Substances 0.000 description 64
- 239000003054 catalyst Substances 0.000 description 53
- 238000000034 method Methods 0.000 description 37
- 239000002904 solvent Substances 0.000 description 37
- 229910052751 metal Inorganic materials 0.000 description 32
- 239000002184 metal Substances 0.000 description 32
- 239000011777 magnesium Substances 0.000 description 29
- 235000001055 magnesium Nutrition 0.000 description 29
- 229910052749 magnesium Inorganic materials 0.000 description 28
- 238000006243 chemical reaction Methods 0.000 description 24
- 239000000178 monomer Substances 0.000 description 23
- 239000010936 titanium Substances 0.000 description 23
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- 238000010828 elution Methods 0.000 description 20
- 238000006116 polymerization reaction Methods 0.000 description 19
- 239000000523 sample Substances 0.000 description 18
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 17
- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 description 16
- 125000001183 hydrocarbyl group Chemical group 0.000 description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 15
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- 238000012360 testing method Methods 0.000 description 14
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 13
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- 125000003118 aryl group Chemical group 0.000 description 10
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- 239000001257 hydrogen Substances 0.000 description 9
- 150000002739 metals Chemical class 0.000 description 9
- RFFLAFLAYFXFSW-UHFFFAOYSA-N 1,2-dichlorobenzene Chemical compound ClC1=CC=CC=C1Cl RFFLAFLAYFXFSW-UHFFFAOYSA-N 0.000 description 8
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- 150000002901 organomagnesium compounds Chemical class 0.000 description 8
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- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 8
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 8
- 239000004322 Butylated hydroxytoluene Substances 0.000 description 7
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 7
- 238000005481 NMR spectroscopy Methods 0.000 description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 7
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 7
- 229940095259 butylated hydroxytoluene Drugs 0.000 description 7
- 229920001577 copolymer Polymers 0.000 description 7
- 229910052736 halogen Inorganic materials 0.000 description 7
- 150000002367 halogens Chemical group 0.000 description 7
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 7
- 239000003446 ligand Substances 0.000 description 7
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 7
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 7
- 230000007935 neutral effect Effects 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- PBKONEOXTCPAFI-UHFFFAOYSA-N 1,2,4-trichlorobenzene Chemical compound ClC1=CC=C(Cl)C(Cl)=C1 PBKONEOXTCPAFI-UHFFFAOYSA-N 0.000 description 6
- 229920000089 Cyclic olefin copolymer Polymers 0.000 description 6
- 239000002841 Lewis acid Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000004913 activation Effects 0.000 description 6
- 125000003710 aryl alkyl group Chemical group 0.000 description 6
- UORVGPXVDQYIDP-UHFFFAOYSA-N borane Chemical compound B UORVGPXVDQYIDP-UHFFFAOYSA-N 0.000 description 6
- 230000001143 conditioned effect Effects 0.000 description 6
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 description 6
- 235000013305 food Nutrition 0.000 description 6
- CBFCDTFDPHXCNY-UHFFFAOYSA-N icosane Chemical compound CCCCCCCCCCCCCCCCCCCC CBFCDTFDPHXCNY-UHFFFAOYSA-N 0.000 description 6
- 150000007517 lewis acids Chemical class 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- JRZJOMJEPLMPRA-UHFFFAOYSA-N 1-nonene Chemical compound CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 5
- 238000007792 addition Methods 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 239000003963 antioxidant agent Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000002425 crystallisation Methods 0.000 description 5
- 230000008025 crystallization Effects 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 5
- 229910001507 metal halide Inorganic materials 0.000 description 5
- 150000005309 metal halides Chemical class 0.000 description 5
- 238000004806 packaging method and process Methods 0.000 description 5
- 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 5
- 239000002685 polymerization catalyst Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 229910052723 transition metal Inorganic materials 0.000 description 5
- 150000003623 transition metal compounds Chemical class 0.000 description 5
- 150000003624 transition metals Chemical class 0.000 description 5
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 5
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 description 5
- 229910052726 zirconium Inorganic materials 0.000 description 5
- 125000006659 (C1-C20) hydrocarbyl group Chemical group 0.000 description 4
- QVLAWKAXOMEXPM-DICFDUPASA-N 1,1,1,2-tetrachloro-2,2-dideuterioethane Chemical compound [2H]C([2H])(Cl)C(Cl)(Cl)Cl QVLAWKAXOMEXPM-DICFDUPASA-N 0.000 description 4
- ZGEGCLOFRBLKSE-UHFFFAOYSA-N 1-Heptene Chemical compound CCCCCC=C ZGEGCLOFRBLKSE-UHFFFAOYSA-N 0.000 description 4
- AFFLGGQVNFXPEV-UHFFFAOYSA-N 1-decene Chemical compound CCCCCCCCC=C AFFLGGQVNFXPEV-UHFFFAOYSA-N 0.000 description 4
- 238000001644 13C nuclear magnetic resonance spectroscopy Methods 0.000 description 4
- WSSSPWUEQFSQQG-UHFFFAOYSA-N 4-methyl-1-pentene Chemical compound CC(C)CC=C WSSSPWUEQFSQQG-UHFFFAOYSA-N 0.000 description 4
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical compound [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000012644 addition polymerization Methods 0.000 description 4
- 238000004364 calculation method Methods 0.000 description 4
- 238000004587 chromatography analysis Methods 0.000 description 4
- 238000013480 data collection Methods 0.000 description 4
- 125000005678 ethenylene group Chemical group [H]C([*:1])=C([H])[*:2] 0.000 description 4
- UAIZDWNSWGTKFZ-UHFFFAOYSA-L ethylaluminum(2+);dichloride Chemical compound CC[Al](Cl)Cl UAIZDWNSWGTKFZ-UHFFFAOYSA-L 0.000 description 4
- 229910021482 group 13 metal Inorganic materials 0.000 description 4
- 229910052735 hafnium Inorganic materials 0.000 description 4
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 4
- 238000012417 linear regression Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 150000002736 metal compounds Chemical class 0.000 description 4
- CPOFMOWDMVWCLF-UHFFFAOYSA-N methyl(oxo)alumane Chemical compound C[Al]=O CPOFMOWDMVWCLF-UHFFFAOYSA-N 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 4
- 238000000079 presaturation Methods 0.000 description 4
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- 229920006300 shrink film Polymers 0.000 description 4
- 239000004460 silage Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- OBAJXDYVZBHCGT-UHFFFAOYSA-N tris(pentafluorophenyl)borane Chemical class FC1=C(F)C(F)=C(F)C(F)=C1B(C=1C(=C(F)C(F)=C(F)C=1F)F)C1=C(F)C(F)=C(F)C(F)=C1F OBAJXDYVZBHCGT-UHFFFAOYSA-N 0.000 description 4
- 229910052720 vanadium Inorganic materials 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 3
- 101100494773 Caenorhabditis elegans ctl-2 gene Proteins 0.000 description 3
- 101100112369 Fasciola hepatica Cat-1 gene Proteins 0.000 description 3
- 101100005271 Neurospora crassa (strain ATCC 24698 / 74-OR23-1A / CBS 708.71 / DSM 1257 / FGSC 987) cat-1 gene Proteins 0.000 description 3
- 239000007983 Tris buffer Substances 0.000 description 3
- 150000001412 amines Chemical class 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
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- QXALIERKYGCHHA-UHFFFAOYSA-N (2,3,4,5,6-pentafluorophenyl)borane Chemical compound BC1=C(F)C(F)=C(F)C(F)=C1F QXALIERKYGCHHA-UHFFFAOYSA-N 0.000 description 2
- QEGNUYASOUJEHD-UHFFFAOYSA-N 1,1-dimethylcyclohexane Chemical compound CC1(C)CCCCC1 QEGNUYASOUJEHD-UHFFFAOYSA-N 0.000 description 2
- YRAJNWYBUCUFBD-UHFFFAOYSA-N 2,2,6,6-tetramethylheptane-3,5-dione Chemical compound CC(C)(C)C(=O)CC(=O)C(C)(C)C YRAJNWYBUCUFBD-UHFFFAOYSA-N 0.000 description 2
- OSDWBNJEKMUWAV-UHFFFAOYSA-N Allyl chloride Chemical compound ClCC=C OSDWBNJEKMUWAV-UHFFFAOYSA-N 0.000 description 2
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- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- YNQLUTRBYVCPMQ-UHFFFAOYSA-N Ethylbenzene Chemical compound CCC1=CC=CC=C1 YNQLUTRBYVCPMQ-UHFFFAOYSA-N 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 2
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- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 2
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- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 2
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- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 150000003609 titanium compounds Chemical class 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
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- 239000010937 tungsten Substances 0.000 description 2
- 125000006273 (C1-C3) alkyl group Chemical group 0.000 description 1
- QPFMBZIOSGYJDE-QDNHWIQGSA-N 1,1,2,2-tetrachlorethane-d2 Chemical compound [2H]C(Cl)(Cl)C([2H])(Cl)Cl QPFMBZIOSGYJDE-QDNHWIQGSA-N 0.000 description 1
- CRRUGYDDEMGVDY-UHFFFAOYSA-N 1-bromoethylbenzene Chemical compound CC(Br)C1=CC=CC=C1 CRRUGYDDEMGVDY-UHFFFAOYSA-N 0.000 description 1
- 125000004134 1-norbornyl group Chemical group [H]C1([H])C([H])([H])C2(*)C([H])([H])C([H])([H])C1([H])C2([H])[H] 0.000 description 1
- AFTBJQDQENGCPC-UHFFFAOYSA-N 2,5-ditert-butyl-4-methylphenol Chemical compound CC1=CC(C(C)(C)C)=C(O)C=C1C(C)(C)C AFTBJQDQENGCPC-UHFFFAOYSA-N 0.000 description 1
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Description
内層は、エチレン系組成物を含む。本明細書で使用される「エチレン系組成物」という用語は、(ポリマーの総重量に基づいて)過半量の重合エチレンモノマーを含み、任意で、少なくとも1つの重合コモノマーを含み得るポリマーを指す。内層は、内層に存在するポリマーの総重量に基づいて、50~100重量%、または65~100重量%、または75~100重量%、または80~100重量%のエチレン系組成物を含み得る。いくつかの実施形態では、内層は、内層に存在するポリマーの総重量に基づいて、70重量%以上、または80重量%以上、または90重量%以上、または95重量%以上、または98重量%のエチレン系組成物を含む。
Mは、それぞれ独立して、+2、+3、または+4の形式酸化状態にあるチタン、ジルコニウム、またはハフニウムであり、いくつかの実施形態では、Mはハフニウムであり、
nは0~3の整数であり、nが0のとき、Xは存在せず、
各Xは、独立して、中性、モノアニオン性、またはジアニオン性の単座配位子であるか、または2つのXが一緒になって、中性、モノアニオン性、またはジアニオン性である二座配位子を形成し、
Xおよびnは、式(I)の金属-配位子錯体が全体として中性であるように選択され、
各Zは、独立して、O、S、N(C1-C40)ヒドロカルビル、またはP(C1-C40)ヒドロカルビルであり、
Z-L-Zフラグメントは、式(1)からなり:
第1の外層および第2の外層は、独立してポリエチレン組成物を含む。第1の外層および第2の外層は、独立して、それぞれ第1の外層または第2の外層に存在するポリマーの総重量に基づいて、50~100重量%、または65~100重量%、または75~100重量%、または80~100重量%のポリエチレン組成物を含み得る。いくつかの実施形態では、第1の外層および第2の外層は、それぞれ第1の外層または第2の外層に存在するポリマーの総重量に基づいて、70重量%以上、または80重量%以上、または90重量%以上、または95重量%以上、または98重量%以上のポリエチレン組成物を含む。
本明細書に記載される多層インフレーションフィルムは、種々の技術によって作製することができる。例えば、多層インフレーションフィルムを作製する方法は、米国特許第6,521,338号(Maka)に記載されており、その全体が参照により本明細書に組み込まれる。例えば、いくつかの実施形態では、多層インフレーションフィルムは、押出機内で内層組成物を第1の外層組成物および第2の外層組成物と共押出しして、内層、第1の外層、および第2の外層を有する筒を形成し、この筒を冷却して多層インフレーションフィルムを形成することによって作製することができる。
密度
密度は、ASTM D-792に従って測定され得る。
メルトインデックス(I2)は、ASTM D 1238、手順B(条件190℃/2.16kg)に従って測定することができる。メルトインデックス(I10)は、ASTM D 1238、手順B(条件190℃/10.0kg)に従って測定することができる。
PolymerChar(スペイン、バレンシア)のGPC-IR高温クロマトグラフィーシステムには、Precision Detectors(マサチューセッツ州、アマースト)の2角度レーザー光散乱検出器モデル2040と、ともにPolymerCharのIR5赤外線検出器および4毛細管粘度計とが備わっていた。データ収集は、PolymerChar Instrument Controlソフトウェアおよびデータ収集インターフェースを使用して実施した。このシステムには、Agilent Technologies(カリフォルニア州、サンタクララ)のオンラインの溶媒脱ガスデバイスおよびポンプシステムが備わっていた。
Mポリエチレン=Ax(Mポリエチレン)B(式1)、
式中、Mは分子量であり、Aは0.4316に等しく、Bは1.0に等しい。
ゼロ剪断粘度は、「直径25mm」の平行板を使用して190℃でAR-G2応力制御レオメーター(TA Instruments、New Castle,Del)で実施したクリープ試験により得た。固定具をゼロにする前に、レオメーターオーブンを少なくとも30分間試験温度に設定した。その試験温度で、圧縮成形された試料ディスクをプレート間に挿入し、5分間平衡にした。次いで、上側プレートを所望の試験間隙(1.5mm)より50μm(機器設定)まで下げた。余分な材料をトリミングして除去し、上側プレートを所望の間隙まで下げた。測定は、5L/分の流速で、窒素パージ下で行った。デフォルトのクリープ時間を2時間に設定した。各試料は、空気中で、10MPaの圧力下で、5分間、177℃で「2mmの厚さ×25mmの直径」の円形プラークに圧縮成形した。次いで、試料を圧縮機から取り出し、カウンターに配置して、冷却した。
原液(3.26g)を10mmのNMR管中の「0.133gのポリマー試料」に添加した。原液は、テトラクロロエタン-d2(TCE)およびペルクロロエチレン(50:50、w:w)と0.001MのCr3+との混合物であった。管内の溶液を5分間N2でパージして酸素量を減らした。蓋をした試料管を室温で一晩放置してポリマー試料を膨潤させた。試料を110℃で周期的にボルテックス混合しながら溶解した。試料は、不飽和の一因となり得る添加剤、例えばエルカミドなどの滑剤を含まなかった。各1H NMR分析は、Bruker AVANCE 400MHz分光計で120℃において10mmの凍結プローブを用いて実行した。
NCH2=I合計/2 (式1A)。
Nビニレン=Iビニレン/2 (式2A)、
Nトリ置換=Iトリ置換(式3A)、
Nビニル=Iビニル/2 (式4A)、
Nビニリデン=Iビニリデン/2(式5A)。
Nビニレン/1,000C=(Nビニレン/NCH2)*1,000 ((式6A)、
Nトリ置換/1,000C=(Nトリ置換/NCH2)*1000 (式7A)、
Nビニル/1000C=(Nビニル/NCH2)*1000 (式8A)、
Nビニリデン/1000C=(Nビニリデン/NCH2)*1000 (式9A)、
約3.5グラムのペレットを予め洗浄した2ドラムポリエチレンバイアルに移すことによって、2組の複製試料を調製した。試験された各金属に対して、NIST追跡可能標準溶液(SPEXからのCerti.pure)から2ドラムポリエチレンバイアル内で標準を調製した。milli-Q純水を用いてそれらを6mlに希釈し、バイアルをヒートシールした。次いで、Mark I TRIGA原子炉を使用して、これらの元素について試料および標準を分析した。これらの元素に使用された反応および実験条件を、以下の表に要約する。ガンマ分光法を行う前に、試料を非照射バイアルに移した。元素濃度は、CANBERRAソフトウェアおよび標準的比較技術を用いて計算した。表1は、金属決定のための測定パラメータを示す。
PolymerChar(Valencia,Spain)製のGPC-IR高温クロマトグラフィーシステムは、精密検出器(Amherst,MA)2角度レーザー光散乱検出器モデル2040、ならびにIR5赤外線検出器(GPC-IR)および4キャピラリー粘度計(いずれもPolymerChar製)が備えられていた。光散乱検出器の「15度の角度」を計算目的に使用した。データ収集は、PolymerChar Instrument Controlソフトウェアおよびデータ収集インターフェースを使用して実施した。このシステムには、Agilent Technologies(カリフォルニア州、サンタクララ)のオンラインの溶媒脱ガスデバイスおよびポンプシステムが備わっていた。
Mポリエチレン=Ax(Mポリエチレン)B(式1B)、
式中、Mは分子量であり、Aはおよそ0.40の値を有し、Bは1.0に等しい。NBS1475A(NIST)線状ポリエチレンの重量平均分子量が以下の式3Bによって計算して52,000g/モルに相当するように、A値を0.385と0.425との間で調節した(特定のカラムセット効率に依存する)。
SCB/1000合計C=A0+[A1×(IR5メチルチャネル領域/IR5測定チャネル領域)](式4B)、
式中、A0はゼロの「IR5領域比」における「SCB/1000合計C」の切片であり、A1は「SCB/1000合計C」対「IR5領域比」の傾きであり、「IR5領域比」の関数としての「SCB/1000合計C」の増加を表す。
モルパーセントコモノマー={SCBf/[SCBf+((1000-SCBf*コモノマーの長さ)/2)]}*100(式5B)、
式中、「SCBf」は、「1000合計C当たりのSCB」であり、「コモノマーの長さ」=オクテンの場合8、ヘキセンの場合6などである。
樹脂を空気中1500psiの圧力下で5分間、350°Fで「3mm厚×1インチ」の円形プラークに圧縮成形した。次いで、試料を圧縮機から取り出し、カウンターに配置して、冷却した。
結晶化溶出分画(CEF)技術を、Monrabalら,Macromol.Symp.257,71-79(2007)に従って実施した。CEF機は、IR-4またはIR-5検出器(例えば、PolymerChar,Spainから市販されているもの)および2角度光散乱検出器モデル2040(例えば、Precision Detectorsから市販されているもの)を備える。50mm×4.6mmの10マイクロメートルガードカラム(例えば、PolymerLabsから市販されているもの)を、IR-4またはIR-5検出器の前に検出器オーブン中に取り付ける。オルトジクロロベンゼン(ODCB、99%の無水等級)および2,5-ジ-tert-ブチル-4-メチルフェノール(BHT)(例えば、Sigma-Aldrichから市販されているもの)を入手した。シリカゲル40(粒径0.2~0.5mm)(例えば、EMD Chemicalsから市販されているもの)も入手した。シリカゲルを、使用前に真空オーブンで、160℃で少なくとも2時間乾燥させる。ODCBを、使用前に乾燥窒素(N2)で1時間スパージする。乾燥窒素は、CaCO3および5Å分子篩上に<90psigで窒素を通すことによって得る。ODCBを、5グラムの乾燥シリカを2リットルのODCBに添加することによって、または0.1ml/分~1.0ml/分で、乾燥シリカを充填したカラム(単数または複数)を通してポンピングすることによって、さらに乾燥させる。N2等の不活性ガスを、サンプルバイアルをパージするのに使用しない場合、800ミリグラムのBHTを、2リットルのODCBに添加する。BHTの有無にかかわらず乾燥ODCBを、以下「ODCB-m」と称する。試料溶液を、オートサンプラーを使用して、160℃で2時間、振盪下で、4mg/mlで、ODCB-m中にポリマー試料を溶解することによって調製する。300μLのサンプル溶液をカラムに注入する。CEFの温度プロファイルは、次のとおりである:110℃から30℃に3℃/分で結晶化、30℃で5分間の熱平衡(2分に設定した可溶性画分溶出時間を含む)、および30℃から140℃に3℃/分で溶出。結晶化中の流速は、0.052ml/分である。溶出中の流速は、0.50ml/分である。IR-4またはIR-5信号データは、1データポイント/秒で収集する。
CDBIを、CEFから得たデータからWO/93/03093に記載される方法を使用して算出する。CDBIは、平均総モル当たりのコモノマー含有量の50パーセント以内のコモノマー含有量を有するポリマー分子の重量パーセントと定義される。これは、ベルヌーイ分布を除いたコモノマー分布と、ポリマー中のコモノマー分布との比較を表す。
製造されたフィルムについて以下の物理的性質を測定した(実験の節を参照)。
フィルムは、ASTM D-2457に従って測定し、光沢単位で表し得る。
内部ヘイズおよび全体の(全)ヘイズについて測定された試料をサンプリングし、ASTM D1003に従って調製した。内部ヘイズは、フィルムの両面に鉱油を使用して屈折率を合わせることによって得た。試験にはHazegard Plus(BYK-Gardner USA、Columbia、MD)を使用した。表面ヘイズは、全ヘイズと内部ヘイズとの差として決定した。全ヘイズは、5回の測定の平均として報告した。
フィルムをASTM D1922、縦方向にタイプB(MD引裂)に従って測定し、グラム-力で表す。試験前に、フィルム試験片の厚さを試料中心で測定した。フィルム方向当たり合計15個の試験片を試験し、平均引裂強度および平均厚さを報告した。平均引裂強度は、平均厚さに対して正規化した。
フィルムは、ASTM D1709に従って測定し、グラムで表す。
約6,718kgの0.20M MgCl2スラリーに219kgのEADC溶液(ヘプタン中15重量%)を添加し、続いて8時間撹拌した。次いで、6%のTiCl4/VOCl3(それぞれ239Kgおよび155Kg)の混合物を添加し、続いてIsopar E中のZr(TMHD)4の6%溶液275Kgを添加した。これら2回の添加は、互いに3時間以内に連続して行った。得られた触媒プレミックスを、使用前にさらに8時間撹拌しながら熟成させた。
触媒1は以下のように調製される:約109kgの0.20M MgCl2スラリーに7.76kgの(C2H5)AlCl2(EADC)溶液(ヘプタン中15重量%)を添加し、続いて8時間撹拌した。次いで、TiCl4/VOCl3の混合物(それぞれ85mLおよび146mL)を添加し、続いてZr(TMHD)4(ジルコニウムテトラキス(2,2,6,6-テトラメチル-3,5-ヘプタンジオネート)の溶液(Isopar E中0.30M溶液0.320kg)を添加した。これら2回の添加は、互いに1時間以内に順次行った。得られた触媒プレミックスを、使用前にさらに8時間撹拌しながら熟成を行った。次いで、触媒1を使用して、下記のように本発明の樹脂2を調製する。
樹脂3は、以下に記載するように、第1の反応器中に第1の触媒系の存在下で、および以下に記載するように、第2の反応器中に第2の触媒系の存在下で、溶液重合により、米国特許第5,977,251号(この特許の図2参照)に従った二重直列ループ反応器システムで調製した。
以下の表6でさらに概説されるA層およびB層によるA/B/A構造を有する3層インフレーションフィルム(本発明のフィルム1~3および比較フィルム1~10)である1ミルのフィルム厚を製造した。3層インフレーションフィルムは、7つの50mm押出機、30/1L/D溝付きフィード押出機、混合セクションを有する中程度の剪断障壁スクリューを有する7層アルパインインフレーションフィルムラインを使用して製造した。フィルム製作条件は、以下の通りであった:2.5のブローアップ比(BUR)、78.7ミルのダイギャップ、9.84インチ(250mm)のダイサイズ、31.4のドローダウン比、および36インチのフロストライン高さ(FLH)。フィルム特性を表6に報告する。
[1] 内層、第1の外層、および第2の外層を有する多層インフレーションフィルムであって、
前記内層が、少なくとも1つのエチレン系ポリマーを含むエチレン系組成物を含み、前記エチレン系組成物が、0.9超のMWCDI値および以下の式:I10/I2≧7.0-1.2×log(I2)を満たすメルトインデックス比(I10/I2)を有し、
前記第1の外層および前記第2の外層が、独立してエチレンと、任意に1つ以上のアルファオレフィンコモノマーとの反応生成物を含むポリエチレン組成物を含み、前記ポリエチレン組成物が、以下の特性:
(a)0.1~2.0g/10分のメルトインデックス(I2 )、
(b)0.910~0.930g/ccの密度、
(c)6.0~7.6のメルトインデックス比(I10/I2 )、および
(d)2.5~4.0の分子量分布(Mw/Mn)によって特徴付けられる、多層インフレーションフィルム。
[2] 前記エチレン系組成物が、10.0以下のMWCDI値を有する、上記[1]に記載のフィルム。
[3] 前記エチレン系組成物が、1.2~3.0のZSVR値を有する、上記[1]または [2]に記載のフィルム。
[4] 前記エチレン系組成物が、9.2以下のメルトインデックス比(I10/I2)を有する、上記[1]~[3]のいずれか1項に記載のフィルム。
[5] 前記エチレン系組成物が、1,000,000合計炭素当たり10超のビニルのビニル不飽和レベルを有する、上記[1]~[4]のいずれか1項に記載のフィルム。
[6] 前記エチレン系組成物が、0.905~0.935g/ccの密度を有する、上記 [1]~[5]のいずれか1項に記載のフィルム。
[7] 前記内層が、前記内層中のポリマーの総量に基づいて、少なくとも75重量%の前記エチレン系組成物を含む、上記[1]~[6]のいずれか1項に記載のフィルム。
[8] 前記ポリエチレン組成物が、1000炭素原子当たり0.12超のビニルのビニル不飽和を有する、上記[1]~[7]のいずれか1項に記載のフィルム。
[9] 前記ポリエチレン組成物が、少なくとも1つの反応器中で溶液重合により多元金属プロ触媒を含む触媒組成物の存在下で形成される、上記[1]~[8]のいずれか1項に記載のフィルム。
[10] 前記溶液重合が、単一の反応器中で生じる、上記[9]に記載のフィルム。
[11] 前記フィルムが、0.3~5ミルの厚さを有する、上記[1]~[10]のいずれか1項に記載のフィルム。
[12] 前記フィルムが、1ミルの厚さを有するインフレーションフィルムに対して12%未満の全ヘイズを示す、上記[1]~[10]のいずれか1項に記載のフィルム。
[13] 前記フィルムが、65超の光沢単位の45°光沢を示す、上記[1]~[10]に記載のフィルム。
本明細書に開示される寸法および値は、記述された正確な数値に厳密に限定されるものとして理解されるべきではない。代わりに、他に特定されない限り、そのような各寸法は、記述された値およびその値を取り巻く機能的に同等の範囲の両方を意味することが意図されている。例えば、「40mm」として開示された寸法は、「約40mm」を意味することが意図されている。
Claims (10)
- 内層、第1の外層、および第2の外層を有する多層インフレーションフィルムであって、
前記内層が、少なくとも1つのエチレン系ポリマーを含むエチレン系組成物を含み、前記エチレン系組成物が、0.9超のMWCDI値、0.5~1.0g/10分のメルトインデックス(I 2 )および以下の式:I10/I2≧7.0-1.2×log(I2)を満たすメルトインデックス比(I10/I2)を有し、
前記第1の外層および前記第2の外層が、独立して、エチレンと、任意に1つ以上のアルファオレフィンコモノマーとの反応生成物を含むポリエチレン組成物を含み、前記ポリエチレン組成物が、以下の特性:
(a)0.5~1.0g/10分のメルトインデックス(I2 )、
(b)0.910~0.930g/ccの密度、
(c)6.0~7.6のメルトインデックス比(I10/I2 )および
(d)2.5~4.0の分子量分布(Mw/Mn)
によって特徴付けられ、
1ミルの厚さを有するインフレーションフィルムに対して12%未満の全ヘイズを示す、多層インフレーションフィルム。 - 前記エチレン系組成物が、10.0以下のMWCDI値を有する、請求項1に記載のフィルム。
- 前記エチレン系組成物が、1.2~3.0のZSVR値を有する、請求項1または2に記載のフィルム。
- 前記エチレン系組成物が、9.2以下のメルトインデックス比(I10/I2)を有する、請求項1~3のいずれか1項に記載のフィルム。
- 前記エチレン系組成物が、1,000,000合計炭素当たり10超のビニルのビニル不飽和レベルを有する、請求項1~4のいずれか1項に記載のフィルム。
- 前記エチレン系組成物が、0.905~0.935g/ccの密度を有する、請求項1~5のいずれか1項に記載のフィルム。
- 前記内層が、前記内層中のポリマーの総量に基づいて、少なくとも75重量%の前記エチレン系組成物を含む、請求項1~6のいずれか1項に記載のフィルム。
- 前記ポリエチレン組成物が、1000炭素原子当たり0.12超のビニルのビニル不飽和を有する、請求項1~7のいずれか1項に記載のフィルム。
- 前記フィルムが、0.3~5ミルの厚さを有する、請求項1~8のいずれか1項に記載のフィルム。
- 前記フィルムが、65超の光沢単位の45°光沢を示す、請求項1~8のいずれか1項に記載のフィルム。
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