JP2016506988A - ポリオレフィンの調製 - Google Patents
ポリオレフィンの調製 Download PDFInfo
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- JP2016506988A JP2016506988A JP2015556933A JP2015556933A JP2016506988A JP 2016506988 A JP2016506988 A JP 2016506988A JP 2015556933 A JP2015556933 A JP 2015556933A JP 2015556933 A JP2015556933 A JP 2015556933A JP 2016506988 A JP2016506988 A JP 2016506988A
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- 229920000098 polyolefin Polymers 0.000 title description 5
- 238000002360 preparation method Methods 0.000 title description 2
- 239000003054 catalyst Substances 0.000 claims abstract description 234
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 144
- 239000002245 particle Substances 0.000 claims abstract description 97
- 238000000034 method Methods 0.000 claims abstract description 50
- 239000012968 metallocene catalyst Substances 0.000 claims abstract description 30
- 238000009826 distribution Methods 0.000 claims abstract description 27
- 239000012190 activator Substances 0.000 claims abstract description 24
- 239000002685 polymerization catalyst Substances 0.000 claims abstract description 23
- -1 polyethylene Polymers 0.000 claims description 113
- 150000001875 compounds Chemical class 0.000 claims description 65
- 229920000642 polymer Polymers 0.000 claims description 63
- 239000000377 silicon dioxide Substances 0.000 claims description 62
- 239000001257 hydrogen Substances 0.000 claims description 43
- 229910052739 hydrogen Inorganic materials 0.000 claims description 43
- 229920005989 resin Polymers 0.000 claims description 39
- 239000011347 resin Substances 0.000 claims description 39
- 230000004044 response Effects 0.000 claims description 38
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 34
- 125000004429 atom Chemical group 0.000 claims description 32
- 239000003446 ligand Substances 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 27
- 239000004698 Polyethylene Substances 0.000 claims description 26
- 229920000573 polyethylene Polymers 0.000 claims description 26
- CPOFMOWDMVWCLF-UHFFFAOYSA-N methyl(oxo)alumane Chemical compound C[Al]=O CPOFMOWDMVWCLF-UHFFFAOYSA-N 0.000 claims description 25
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 24
- 239000005977 Ethylene Substances 0.000 claims description 24
- 125000005842 heteroatom Chemical group 0.000 claims description 24
- 125000001183 hydrocarbyl group Chemical group 0.000 claims description 24
- 238000006116 polymerization reaction Methods 0.000 claims description 24
- 239000007789 gas Substances 0.000 claims description 20
- 239000000155 melt Substances 0.000 claims description 20
- 230000008569 process Effects 0.000 claims description 19
- 229910052735 hafnium Inorganic materials 0.000 claims description 16
- 239000002002 slurry Substances 0.000 claims description 14
- SVBLJDGZIHTZBY-UHFFFAOYSA-N C(CC)C1(C=CC=C1)[Hf]C1(C=CC=C1)CCC Chemical compound C(CC)C1(C=CC=C1)[Hf]C1(C=CC=C1)CCC SVBLJDGZIHTZBY-UHFFFAOYSA-N 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 13
- 125000000058 cyclopentadienyl group Chemical group C1(=CC=CC1)* 0.000 claims description 12
- ZSWFCLXCOIISFI-UHFFFAOYSA-N endo-cyclopentadiene Natural products C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 claims description 12
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 6
- 125000006659 (C1-C20) hydrocarbyl group Chemical group 0.000 claims description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 125000005595 acetylacetonate group Chemical group 0.000 claims description 2
- 150000004703 alkoxides Chemical class 0.000 claims description 2
- 125000004946 alkenylalkyl group Chemical group 0.000 claims 1
- 150000001734 carboxylic acid salts Chemical class 0.000 claims 1
- 230000000704 physical effect Effects 0.000 claims 1
- 229920003023 plastic Polymers 0.000 claims 1
- 239000004033 plastic Substances 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 description 27
- 239000002184 metal Substances 0.000 description 26
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 23
- 125000000217 alkyl group Chemical group 0.000 description 22
- 239000000463 material Substances 0.000 description 22
- 125000004122 cyclic group Chemical group 0.000 description 20
- 238000004519 manufacturing process Methods 0.000 description 18
- 239000000178 monomer Substances 0.000 description 18
- 229910052757 nitrogen Inorganic materials 0.000 description 17
- 238000006243 chemical reaction Methods 0.000 description 16
- 125000004432 carbon atom Chemical group C* 0.000 description 15
- 239000003795 chemical substances by application Substances 0.000 description 15
- 125000001424 substituent group Chemical group 0.000 description 14
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- 125000003118 aryl group Chemical group 0.000 description 12
- 229910052736 halogen Inorganic materials 0.000 description 12
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 12
- 230000003068 static effect Effects 0.000 description 12
- LIKMAJRDDDTEIG-UHFFFAOYSA-N 1-hexene Chemical compound CCCCC=C LIKMAJRDDDTEIG-UHFFFAOYSA-N 0.000 description 11
- 239000004305 biphenyl Substances 0.000 description 11
- 235000010290 biphenyl Nutrition 0.000 description 11
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 11
- 150000003254 radicals Chemical class 0.000 description 11
- 229910052799 carbon Inorganic materials 0.000 description 10
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 10
- 229910052710 silicon Inorganic materials 0.000 description 10
- 239000000654 additive Substances 0.000 description 9
- 229910052732 germanium Inorganic materials 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 125000001181 organosilyl group Chemical group [SiH3]* 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 9
- 239000007983 Tris buffer Substances 0.000 description 8
- 239000000969 carrier Substances 0.000 description 8
- 239000010408 film Substances 0.000 description 8
- 229930195733 hydrocarbon Natural products 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 229910052726 zirconium Inorganic materials 0.000 description 8
- 229920002873 Polyethylenimine Polymers 0.000 description 7
- 150000001412 amines Chemical class 0.000 description 7
- 150000002367 halogens Chemical class 0.000 description 7
- 150000004678 hydrides Chemical class 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 7
- 230000000670 limiting effect Effects 0.000 description 7
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 229910052717 sulfur Inorganic materials 0.000 description 7
- 239000004215 Carbon black (E152) Substances 0.000 description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- 125000002877 alkyl aryl group Chemical group 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 description 6
- QWTDNUCVQCZILF-UHFFFAOYSA-N isopentane Chemical compound CCC(C)C QWTDNUCVQCZILF-UHFFFAOYSA-N 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 229910052698 phosphorus Inorganic materials 0.000 description 6
- 239000011574 phosphorus Substances 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 230000000996 additive effect Effects 0.000 description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 5
- 235000010210 aluminium Nutrition 0.000 description 5
- 229940083916 aluminum distearate Drugs 0.000 description 5
- RDIVANOKKPKCTO-UHFFFAOYSA-K aluminum;octadecanoate;hydroxide Chemical compound [OH-].[Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O RDIVANOKKPKCTO-UHFFFAOYSA-K 0.000 description 5
- 229910052796 boron Inorganic materials 0.000 description 5
- 150000007942 carboxylates Chemical class 0.000 description 5
- 239000003085 diluting agent Substances 0.000 description 5
- 238000011020 pilot scale process Methods 0.000 description 5
- AFFLGGQVNFXPEV-UHFFFAOYSA-N 1-decene Chemical compound CCCCCCCCC=C AFFLGGQVNFXPEV-UHFFFAOYSA-N 0.000 description 4
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 4
- 125000003710 aryl alkyl group Chemical group 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 125000000623 heterocyclic group Chemical group 0.000 description 4
- 229910052809 inorganic oxide Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 230000036961 partial effect Effects 0.000 description 4
- 229950010765 pivalate Drugs 0.000 description 4
- IUGYQRQAERSCNH-UHFFFAOYSA-N pivalic acid Chemical compound CC(C)(C)C(O)=O IUGYQRQAERSCNH-UHFFFAOYSA-N 0.000 description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 125000003944 tolyl group Chemical group 0.000 description 4
- 125000002023 trifluoromethyl group Chemical group FC(F)(F)* 0.000 description 4
- 125000006710 (C2-C12) alkenyl group Chemical group 0.000 description 3
- YBYIRNPNPLQARY-UHFFFAOYSA-N 1H-indene Natural products C1=CC=C2CC=CC2=C1 YBYIRNPNPLQARY-UHFFFAOYSA-N 0.000 description 3
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 3
- JAKYKQHNJUDFCT-UHFFFAOYSA-N C1=CC=C2C([Zr])C=CC2=C1 Chemical compound C1=CC=C2C([Zr])C=CC2=C1 JAKYKQHNJUDFCT-UHFFFAOYSA-N 0.000 description 3
- 125000000882 C2-C6 alkenyl group Chemical group 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical group [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 3
- AFABGHUZZDYHJO-UHFFFAOYSA-N dimethyl butane Natural products CCCC(C)C AFABGHUZZDYHJO-UHFFFAOYSA-N 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 125000003983 fluorenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 description 3
- 125000004216 fluoromethyl group Chemical group [H]C([H])(F)* 0.000 description 3
- 238000012685 gas phase polymerization Methods 0.000 description 3
- 150000002366 halogen compounds Chemical class 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- 125000003454 indenyl group Chemical group C1(C=CC2=CC=CC=C12)* 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 229910052752 metalloid Inorganic materials 0.000 description 3
- 150000002738 metalloids Chemical class 0.000 description 3
- 150000002739 metals Chemical class 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 125000000538 pentafluorophenyl group Chemical group FC1=C(F)C(F)=C(*)C(F)=C1F 0.000 description 3
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- 150000003839 salts Chemical class 0.000 description 3
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- 238000006467 substitution reaction Methods 0.000 description 3
- 229910052723 transition metal Inorganic materials 0.000 description 3
- 150000003624 transition metals Chemical class 0.000 description 3
- MCULRUJILOGHCJ-UHFFFAOYSA-N triisobutylaluminium Chemical compound CC(C)C[Al](CC(C)C)CC(C)C MCULRUJILOGHCJ-UHFFFAOYSA-N 0.000 description 3
- 125000003161 (C1-C6) alkylene group Chemical group 0.000 description 2
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 2
- ZGEGCLOFRBLKSE-UHFFFAOYSA-N 1-Heptene Chemical compound CCCCCC=C ZGEGCLOFRBLKSE-UHFFFAOYSA-N 0.000 description 2
- GQEZCXVZFLOKMC-UHFFFAOYSA-N 1-hexadecene Chemical compound CCCCCCCCCCCCCCC=C GQEZCXVZFLOKMC-UHFFFAOYSA-N 0.000 description 2
- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical compound CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 description 2
- WSSSPWUEQFSQQG-UHFFFAOYSA-N 4-methyl-1-pentene Chemical compound CC(C)CC=C WSSSPWUEQFSQQG-UHFFFAOYSA-N 0.000 description 2
- HBAQYPYDRFILMT-UHFFFAOYSA-N 8-[3-(1-cyclopropylpyrazol-4-yl)-1H-pyrazolo[4,3-d]pyrimidin-5-yl]-3-methyl-3,8-diazabicyclo[3.2.1]octan-2-one Chemical class C1(CC1)N1N=CC(=C1)C1=NNC2=C1N=C(N=C2)N1C2C(N(CC1CC2)C)=O HBAQYPYDRFILMT-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 239000011954 Ziegler–Natta catalyst Substances 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- RBQGALRSGWYFMO-UHFFFAOYSA-L [Cl-].[Cl-].C1(C=CC=C1)[Zr+2]C1=CC=CC=2C3=CC=CC=C3CC1=2 Chemical compound [Cl-].[Cl-].C1(C=CC=C1)[Zr+2]C1=CC=CC=2C3=CC=CC=C3CC1=2 RBQGALRSGWYFMO-UHFFFAOYSA-L 0.000 description 2
- JFWBIRAGFWPMTI-UHFFFAOYSA-N [Zr].[CH]1C=CC=C1 Chemical compound [Zr].[CH]1C=CC=C1 JFWBIRAGFWPMTI-UHFFFAOYSA-N 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 125000005234 alkyl aluminium group Chemical group 0.000 description 2
- 125000005248 alkyl aryloxy group Chemical group 0.000 description 2
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- 125000004104 aryloxy group Chemical group 0.000 description 2
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 125000005619 boric acid group Chemical group 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 125000001309 chloro group Chemical group Cl* 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 2
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 2
- 238000005243 fluidization Methods 0.000 description 2
- 150000002222 fluorine compounds Chemical class 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 229920001519 homopolymer Polymers 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 238000009616 inductively coupled plasma Methods 0.000 description 2
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 2
- 239000002480 mineral oil Substances 0.000 description 2
- 235000010446 mineral oil Nutrition 0.000 description 2
- APRJFNLVTJWEPP-UHFFFAOYSA-M n,n-diethylcarbamate Chemical compound CCN(CC)C([O-])=O APRJFNLVTJWEPP-UHFFFAOYSA-M 0.000 description 2
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 125000004433 nitrogen atom Chemical group N* 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 125000004430 oxygen atom Chemical group O* 0.000 description 2
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 2
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 description 2
- 125000004437 phosphorous atom Chemical group 0.000 description 2
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- 239000002243 precursor Substances 0.000 description 2
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
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- 238000003756 stirring Methods 0.000 description 2
- 125000000547 substituted alkyl group Chemical group 0.000 description 2
- 125000003107 substituted aryl group Chemical group 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
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- 239000000725 suspension Substances 0.000 description 2
- 229910052718 tin Inorganic materials 0.000 description 2
- GBXQPDCOMJJCMJ-UHFFFAOYSA-M trimethyl-[6-(trimethylazaniumyl)hexyl]azanium;bromide Chemical compound [Br-].C[N+](C)(C)CCCCCC[N+](C)(C)C GBXQPDCOMJJCMJ-UHFFFAOYSA-M 0.000 description 2
- JLTRXTDYQLMHGR-UHFFFAOYSA-N trimethylaluminium Chemical compound C[Al](C)C JLTRXTDYQLMHGR-UHFFFAOYSA-N 0.000 description 2
- 150000003755 zirconium compounds Chemical class 0.000 description 2
- WCFQIFDACWBNJT-UHFFFAOYSA-N $l^{1}-alumanyloxy(2-methylpropyl)aluminum Chemical compound CC(C)C[Al]O[Al] WCFQIFDACWBNJT-UHFFFAOYSA-N 0.000 description 1
- 125000004642 (C1-C12) alkoxy group Chemical group 0.000 description 1
- 125000002733 (C1-C6) fluoroalkyl group Chemical group 0.000 description 1
- 125000006755 (C2-C20) alkyl group Chemical group 0.000 description 1
- CRSBERNSMYQZNG-UHFFFAOYSA-N 1 -dodecene Natural products CCCCCCCCCCC=C CRSBERNSMYQZNG-UHFFFAOYSA-N 0.000 description 1
- QCEOZLISXJGWSW-UHFFFAOYSA-K 1,2,3,4,5-pentamethylcyclopentane;trichlorotitanium Chemical compound [Cl-].[Cl-].[Cl-].CC1=C(C)C(C)([Ti+3])C(C)=C1C QCEOZLISXJGWSW-UHFFFAOYSA-K 0.000 description 1
- CORHDXNAYKUXRI-UHFFFAOYSA-N 1h-cyclopenta[12]annulene Chemical compound C1=CC=CC=CC=CC=CC2=C1CC=C2 CORHDXNAYKUXRI-UHFFFAOYSA-N 0.000 description 1
- FXNDIJDIPNCZQJ-UHFFFAOYSA-N 2,4,4-trimethylpent-1-ene Chemical compound CC(=C)CC(C)(C)C FXNDIJDIPNCZQJ-UHFFFAOYSA-N 0.000 description 1
- YVSMQHYREUQGRX-UHFFFAOYSA-N 2-ethyloxaluminane Chemical compound CC[Al]1CCCCO1 YVSMQHYREUQGRX-UHFFFAOYSA-N 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 125000004975 3-butenyl group Chemical group C(CC=C)* 0.000 description 1
- 125000006043 5-hexenyl group Chemical group 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
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- 125000001028 difluoromethyl group Chemical group [H]C(F)(F)* 0.000 description 1
- URSLCTBXQMKCFE-UHFFFAOYSA-N dihydrogenborate Chemical compound OB(O)[O-] URSLCTBXQMKCFE-UHFFFAOYSA-N 0.000 description 1
- QKIUAMUSENSFQQ-UHFFFAOYSA-N dimethylazanide Chemical compound C[N-]C QKIUAMUSENSFQQ-UHFFFAOYSA-N 0.000 description 1
- ZTJBELXDHFJJEU-UHFFFAOYSA-N dimethylboron Chemical compound C[B]C ZTJBELXDHFJJEU-UHFFFAOYSA-N 0.000 description 1
- YOTZYFSGUCFUKA-UHFFFAOYSA-N dimethylphosphine Chemical compound CPC YOTZYFSGUCFUKA-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229940069096 dodecene Drugs 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004993 emission spectroscopy Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- GCPCLEKQVMKXJM-UHFFFAOYSA-N ethoxy(diethyl)alumane Chemical compound CCO[Al](CC)CC GCPCLEKQVMKXJM-UHFFFAOYSA-N 0.000 description 1
- 125000000219 ethylidene group Chemical group [H]C(=[*])C([H])([H])[H] 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 125000003709 fluoroalkyl group Chemical group 0.000 description 1
- 125000004407 fluoroaryl group Chemical group 0.000 description 1
- 125000003784 fluoroethyl group Chemical group [H]C([H])(F)C([H])([H])* 0.000 description 1
- 125000001207 fluorophenyl group Chemical group 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 235000013611 frozen food Nutrition 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000004746 geotextile Substances 0.000 description 1
- WHYHZFHCWGGCOP-UHFFFAOYSA-N germyl Chemical compound [GeH3] WHYHZFHCWGGCOP-UHFFFAOYSA-N 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 150000002363 hafnium compounds Chemical class 0.000 description 1
- FIFKZAWQYNAOPH-UHFFFAOYSA-L hafnium(4+);dichloride Chemical compound [Cl-].[Cl-].[Hf+4] FIFKZAWQYNAOPH-UHFFFAOYSA-L 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 229910001504 inorganic chloride Inorganic materials 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 239000001282 iso-butane Substances 0.000 description 1
- 238000002356 laser light scattering Methods 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 150000007527 lewis bases Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- MHERPFVRWOTBSF-UHFFFAOYSA-N methyl(phenyl)phosphane Chemical compound CPC1=CC=CC=C1 MHERPFVRWOTBSF-UHFFFAOYSA-N 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 1
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 125000001624 naphthyl group Chemical group 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000001037 p-tolyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1*)C([H])([H])[H] 0.000 description 1
- 229920006280 packaging film Polymers 0.000 description 1
- 239000012785 packaging film Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 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
- 125000001147 pentyl group Chemical group C(CCCC)* 0.000 description 1
- 150000003003 phosphines Chemical class 0.000 description 1
- 238000007745 plasma electrolytic oxidation reaction Methods 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 239000012041 precatalyst Substances 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229920006300 shrink film Polymers 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- OLRJXMHANKMLTD-UHFFFAOYSA-N silyl Chemical compound [SiH3] OLRJXMHANKMLTD-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 235000011888 snacks Nutrition 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- VSEOIQRHQSIHRZ-UHFFFAOYSA-L titanium(4+);dichloride Chemical compound Cl[Ti+2]Cl VSEOIQRHQSIHRZ-UHFFFAOYSA-L 0.000 description 1
- 150000003623 transition metal compounds Chemical class 0.000 description 1
- SQBBHCOIQXKPHL-UHFFFAOYSA-N tributylalumane Chemical compound CCCC[Al](CCCC)CCCC SQBBHCOIQXKPHL-UHFFFAOYSA-N 0.000 description 1
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 description 1
- VOITXYVAKOUIBA-UHFFFAOYSA-N triethylaluminium Chemical compound CC[Al](CC)CC VOITXYVAKOUIBA-UHFFFAOYSA-N 0.000 description 1
- ORYGRKHDLWYTKX-UHFFFAOYSA-N trihexylalumane Chemical compound CCCCCC[Al](CCCCCC)CCCCCC ORYGRKHDLWYTKX-UHFFFAOYSA-N 0.000 description 1
- 125000000026 trimethylsilyl group Chemical group [H]C([H])([H])[Si]([*])(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- LFXVBWRMVZPLFK-UHFFFAOYSA-N trioctylalumane Chemical compound CCCCCCCC[Al](CCCCCCCC)CCCCCCCC LFXVBWRMVZPLFK-UHFFFAOYSA-N 0.000 description 1
- CNWZYDSEVLFSMS-UHFFFAOYSA-N tripropylalumane Chemical compound CCC[Al](CCC)CCC CNWZYDSEVLFSMS-UHFFFAOYSA-N 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- VPGLGRNSAYHXPY-UHFFFAOYSA-L zirconium(2+);dichloride Chemical compound Cl[Zr]Cl VPGLGRNSAYHXPY-UHFFFAOYSA-L 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
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Abstract
Description
メタロセン触媒化合物
一般に、メタロセン触媒化合物について、例えば、1及び2メタロセンベースのポリオレフィン(John Scheirs&W.Kaminsky eds.,John Wiley&Sons,Ltd.2000)、G.G.Hlatky in 181 COORDINATION CHEM.REV.243−296(1999)に記載され、特に、使用については、1メタロセンベースのポリオレフィンS261−377におけるポリエチレンの合成(2000)に記載される。メタロセン触媒化合物は、少なくとも3〜12族の金属原子のうちの1つに結合する1つ以上のCp配位子(シクロペンタジエニル及びシクロペンタジエニルへの配位子アイソローバル)、及び、少なくとも1つの金属原子に結合する1つ以上の脱離器を有する「ハーフサンドイッチ」及び/または「フルサンドイッチ」化合物を含むことができる。本明細書中で使用するように、周期表(周期表(Periodic Table of the Elements))及びその族への全参照は、HAWLEY’S CONDENSED CHEMICAL DICTIONARYの第13版(IUPACの許可の下再版された)、John Wiley & Sons,Inc.,(1997)で発表された、新たな表記法(NEW NOTATION)に対するものであるが、これは、参照が、ローマ数字で記載される以前のIUPAC形式(またはその形式内に表記されるもの)に対して行われない場合、または、別途指示されない場合に限る。
CpACpBMXn (I)
式(I)中、Mは上記の通りであり、各XはMに化学的に結合し、各Cp基はMに化学的に結合し、nは0または1〜4の整数である。いくつかの実施形態では、nは1または2であってよい。式(I)中CpA及びCpBによって示される配位子は、同じまたは異なるシクロペンタジエニル配位子、またはシクロペンタジエニルへの配位子アイソローバルであってよく、それらのいずれかまたはいずれもがヘテロ原子を含み得て、それらのいずれかまたはいずれもがR族によって置換され得る。少なくとも1つの特定の実施形態において、CpA及びCpBは、シクロペンタジエニル、インデニル、テトラヒドロインデニル、フルオレニル、及びそれぞれの置換誘導体からなる群から独立して選択される。
CpA(A)CpBMXn (II)
触媒系は、1つ以上の15族の金属を含む触媒化合物を含むことができる。15族の金属を含む触媒化合物は一般に、3〜14族の金属原子と、3〜7族または4〜6族の金属原子と、を含む。多くの実施形態では、15族の金属を含む化合物は、少なくとも1つの脱離基及び少なくとも2つの15族の原子にも結合し、それらのうちの少なくとも1つが、別の基を介して15または16族の原子にも結合する、4族の金属原子を含む。
本明細書中で使用されるように、担体という用語は、タルク、無機酸化物、及び無機塩化物等の多孔性担体物質を示す。触媒原料使用される触媒化合物は、活性剤とともに同じ担体上に担持され得る、または活性剤を非担持形態で使用することができる、あるいは活性剤を単一サイトの触媒化合物、またはそれらの組み合わせとは異なる担体に堆積させることができる。これを当該業界で一般的に使用される任意の技術によって実現することができる。当該業界には、単一サイトの触媒化合物を担持するための他の様々な方法が存在する。例えば、単一サイトの触媒化合物は、例えば、米国特許第5,473,202号及び同第5,770,755号に記載のポリマー結合配位子を含むことができる。単一サイトの触媒化合物は、例えば、米国特許第5,648,310号に記載のように、噴霧乾燥体であってよい。単一サイトの触媒化合物と使用する担体は、欧州特許第0 802 203号に記載されるように、官能性であってよい、または米国特許第5,688,880号に記載のように、少なくとも1つの置換基または脱離基が選択される。
本明細書中で使用されるように、用語「活性剤」は、単一サイトの触媒化合物または成分を、例えば、触媒成分のカチオン種を生成することすることによって活性化することができる、担持されたまたは非担持の任意の化合物または化合物の組み合わせを示す。例えば、これには、少なくとも1つの脱離基(本明細書中に記載の単一サイトの触媒化合物の「X」族)の、単一サイトの触媒化合物/成分の金属中心からの引き抜きが含まれ得る。また、活性剤は、「共触媒」として示され得る。
本明細書中に開示された気相ポリエチレン生成プロセスでは、1つ以上の静電制御剤を付加的に使用し、反応器内の静水位を調節することが望ましい。本明細書中で使用されるように、静電制御剤は、流動反応器内に流入された際に、流動床で静電荷(負に、正に、)に影響を及ぼし得る、または、または0まで)それを駆動し得る化学成分である。使用される特定の静電制御剤は、正電荷の特質によって決定し得、生成されるポリマー及び使用される単一サイトの触媒化合物によって、選択される静電制御剤が異なり得る。例えば、静電制御剤の使用は欧州特許第0229368号、及び米国特許第4,803,251号、同第4,555,370号、及び同第5,283,278号、ならびにそれらで引用される参照に開示されている。
-(CH2-CH2-NH)n-
式中、nは約10〜約10,000であってよい。ポリエチレンイミンは、直鎖、分岐、または超分岐(例えば、樹状または樹枝状ポリマー構造を形成する)であってよい。それらは、エチレンイミンのホモポリマーまたはコポリマー、もしくはそれらの混合(以下、ポリエチレンイミンと称される)であってよい。化学式−−[CH2−CH2−NH]-によって示される直鎖ポリマーを、ポリエチレンイミンとして使用することができ、また、第1、第2、及び第3分岐を使用することもできる。
本明細書中に記載される触媒系を使用して1つ以上のオレフィンを重合させ、それらから1つ以上のポリマー生成物を生成することができる。気相、スラリー、高圧力、及び/または、溶液重合プロセスを含むがそれらに限定されない、任意の好適な重合プロセスを使用することができる。様々な実施形態では、流動床反応器を利用し、ポリオレフィンポリマーを気相重合プロセスで生成する。
FBD=(ΔP*S)/(S1*H) 式1
Eqn.1で、ΔPは、下部と中間タップとの間の圧力降下(lbs/in2)を示し、Sは反応器のD断面積(in2)を示し、S1は反応器の断面積(ft2)を示し、Hは、下部と中間タップとの間の距離(ft)を示し、この方程式によって計算されたFBD値は、反応器の圧力、温度、及び気体密度に基づいて実測値に修正される。
パイロットプラントのためにES70シリカを用いてHfPを形成するための工程は混合タンクに及ぶ
EP70シリカ上でHfP触媒を形成するために使用される材料には、およそビス(n−プロピルシクロペンタジエニル)ハフニウムジメチル(HfP)、875℃で脱水されたES70シリカ、及びトルエン中のメチルアルミノキサン(MAO)が10%である溶液が含まれた。Al:Hfモル比は、約80:1〜130:1であった。触媒組成物を調製するための方法は、例えば、米国特許第6,242,545号に開示されている。担持工程で使用される混合タンクは、動作前に、浄化され、乾燥され、圧力検査される。混合タンクは、二重らせん性のリボン翼を用いて撹拌される。
表1は、生産中に調製された15の樹脂試料のリストを有する。対照触媒が含まれていない、ES757用に作製された3つの触媒バッチ、Davison 955用に作製された2つのバッチ、PQ ES70用に作製された2つのバッチであり、及びDavison 2408の1つのバッチが存在した。これらの全触媒バッチは、同じ触媒形成(HfPベース)を有するが、使用する担体のタイプのみが異なる。これらの触媒バッチの評価は、エチレン流量に基づいて、200psiaのエチレン分圧、およそ2時間の滞留時間、2〜3モル%のイソペンタンレベル、及び30ppmwの連続添加剤のレベルで実行された。
Claims (29)
- 担持重合触媒を作製するための方法であって、
ハウニウムを含む触媒化合物を形成することと、
前記触媒を活性剤と混合して触媒錯体を形成することと、
前記触媒錯体をシリカ担体と合わせて、担持触媒を形成することと、
前記担持触媒を乾燥させて、前記触媒錯体を前記シリカ担体に結合させることと、を含み、前記担持触媒が、約0.660mm(0.0260in)を超える平均粒径と、約7000gの樹脂/g(触媒)を超える平均生産性と、を有し、約20%の樹脂粒子が、約1mmより大きい粒径を有する樹脂粒径の分布を形成するポリマーを生成する、前記方法。 - 前記担持重合触媒が、重合が実質的に同じ反応器条件で行われたときに、他のシリカ担体上に担持される前記触媒化合物から形成された樹脂粒子の流動化かさ密度対安定かさ密度比(FBD/SBD)の平均より、少なくとも約4%高い、平均流動化かさ密度対安定かさ密度比(FBD/SBD)を有する樹脂粒子を形成する、請求項1に記載の前記方法。
- 実質的に同じ反応器条件において、前記担持触媒が、約25μmの平均粒径を有する触媒のメルトフロー比応答の3ユニット内であるメルトフロー比応答で、ポリマーを形成する、請求項1に記載の前記方法。
- ビス(n−プロピルシクロペンタジエニル)ハフニウム(CH3)2、ビス(n−プロピルシクロペンタジエニル)ハフニウムF2、ビス(n−プロピルシクロペンタジエニル)ハフニウムCl2、またはそれらの任意の組み合わせを含む触媒化合物を形成することを含む、請求項1に記載の前記方法。
- 前記触媒をメチルアルミノキサン(MAO)活性剤と混合することを含む、請求項1に記載の前記方法。
- 担持重合触媒を作製するための方法であって、
ビス(n−プロピルシクロペンタジエニル)ハフニウム(CH3)2を含む触媒を形成することと、
前記触媒をメチルアルミノキサンと混合して、触媒錯体を形成することと、
前記触媒錯体をシリカ担体と合わせて、担持触媒を形成することと、
前記担持触媒を乾燥させて、前記触媒錯体を前記シリカ担体と結合させることと、を含み、前記担持触媒が、約0.762mm(0.03in)を超える平均粒径と、約7000gの樹脂/g(触媒)を超える平均生産性と、を有し、約20%が、約1mmより大きい粒径を有する樹脂粒子の分布を形成するポリマーを生成する、前記方法。 - 前記担持重合触媒が、少なくとも約0.570の平均流動化かさ密度対安定かさ密度比(FBD/SBD)を有する樹脂粒子を形成する、請求項6に記載の前記方法。
- ポリマーを形成するための方法であって、
1gの触媒につき少なくとも約7000gのポリマーの生産性を有する担持ハフニウム触媒を形成することと、
前記担持触媒を流動床反応器内で少なくともエチレンと反応させて、樹脂粒子を形成することと、を含み、前記樹脂粒子が、
少なくとも約0.762mm(0.0300in)の平均ポリマー粒径と、
直径1mmを少なくとも約20%超える粒径分布と、
約0.570を超える流動化かさ密度対安定かさ密度比(FBD/SBD)と、を有する、前記方法。 - 実質的に同じ反応器条件において、前記担持触媒が、約25μmの平均粒径を有する触媒のメルトフロー比応答の3ユニット内であるメルトフロー比応答で、ポリマーを形成する、請求項8に記載の前記方法。
- 前記担持触媒形成することが、
ビス(n−プロピルシクロペンタジエニル)ハフニウム(CH3)2をメチルアルミノキサンと混合して、触媒錯体を形成することと、
前記触媒錯体をシリカ担体と合わせて、担持触媒を形成することと、
前記担持触媒を乾燥させて、前記触媒錯体を前記シリカ担体に結合させることと、を含む、請求項8に記載の前記方法。 - コモノマーを前記流動床反応器に添加し、前記樹脂粒子の密度を制御することを含む、請求項8に記載の前記方法。
- 前記担持触媒が、少なくとも約77℃の温度で、約0.7dg/分のMI、約0.912g/cm3の密度、及び約26のMFRを有するポリマーを、流動床反応器内で形成する、請求項8に記載の前記方法。
- 前記担持触媒が、少なくとも約75℃の温度で、約1dg/分のMI、約0.918g/cm3の密度、及び約28のMFRを有するポリマーを、流動床反応器内で形成する、請求項8に記載の前記方法。
- 水素を前記流動床反応器に添加し、前記樹脂粒子のメルトインデックスを制御することを含む、請求項8に記載の前記方法。
- 流動床気相反応器内で前記担持触媒からポリマーを形成することを含む、請求項8に記載の前記方法。
- スラリーループ反応器内で、前記担持触媒からポリマーを形成することを含む、請求項1に記載の前記方法。
- 樹脂粒子のサンプルを測定し、初期生成物特性を得ることと、
前記初期生成物特性に少なくとも部分的に基づいて、プロセスパラメータを変更して、第2の生成物を得ることと、を含む、請求項8に記載の前記方法。 - 試料を測定することが、プラスチック試料の物理的特性を判定することを含む、請求項17に記載の前記方法。
- 試料を測定することが、フローインデックス、メルトインデックス、密度、分子量分布、コモノマー含有量、またはそれらの任意の組み合わせのうちの少なくとも1つを判定することを含む、請求項17に記載の前記方法。
- 重合反応器内でコモノマー対エチレンの比率を調整して、ポリエチレンの組成分布、前記分子量分布、及び前記メルトインデックス(I2)のうちの少なくとも1つを制御することを含む、請求項17に記載の前記方法。
- 重合反応器内で水素対エチレンの比率を調整して、ポリエチレンの組成分布、前記分子量分布、及び前記メルトインデックス(I2)のうちの少なくとも1つを制御することを含む、請求項17に記載の前記方法。
- ポリエチレンコポリマーを形成するための重合触媒であって、
複数のシリカ粒子と、
前記複数のシリカ粒子上に担持されるメタロセン触媒と、
前記複数のシリカ粒子上に担持される活性剤と、を含み、
前記重合触媒が、前記粒子の約10%が約17〜約23マイクロメートル未満の粒径を有し、前記粒子の約50%が約40〜約45マイクロメートル未満の粒径を有し、前記粒子の約90%が約72〜約77マイクロメートル未満の粒径を有する粒径分布を有し、
前記重合触媒が、約77℃での約26のメルトフロー比応答と、
前記重合触媒が、約75℃での約28のメルトフロー比応答と、を有する、前記重合触媒。 - 前記活性剤がメチルアルミノキサンを含む、請求項22に記載の前記触媒。
- 触媒担体に含浸した前記触媒が、ビス(n−プロピルシクロペンタジエニル)ハフニウム(CH3)2、ビス(n−プロピルシクロペンタジエニル)ハフニウムF2、ビス(n−プロピルシクロペンタジエニル)ハフニウムCl2、またはそれらの任意の組み合わせを含む、請求項22に記載の前記触媒。
- 前記担体に含浸した触媒が、式
CpACpBMXn、または、CpA(A)CpBMXn、
を有し、
式中、Mは、第4、5、または6族の原子であり、CpA及びCpBはそれぞれMに結合し、シクロペンタジエニル配位子、置換シクロペンタジエニル配位子、シクロペンタジエニルへの配位子アイソローバル、及びシクロペンタジエニルへの置換配位子アイソローバルからなる群から独立して選択され、(A)は、CpA及びCpBのいずれにも結合し、二価のC1〜C20のヒドロカルビル、及び、ヒドロカルビルを含むC1〜C20のヘテロ原子からなる群から選択される二価の架橋基であり、ヒドロカルビルを含む前記ヘテロ原子は1〜3のヘテロ原子を含み、Xは、塩化物イオン、臭化物イオン、C1〜C10のアルキル及びC2〜C12のアルケニル、カルボン酸塩、アセチルアセトネート及びアルコキシドからなる群から選択される脱離基であり、nは1〜3の整数である、請求項22に記載の前記触媒。 - 前記重合触媒が、約0.570を超える流動化かさ密度対安定かさ密度(FBD/SBD)の比率を有するポリマーを形成する、請求項22に記載の前記触媒。
- ポリエチレンコポリマーを形成するための重合触媒であって、
複数のシリカ粒子と、
前記複数のシリカ粒子上に担持されるハフニウム触媒と、
前記複数のシリカ粒子上に担持される活性剤と、
を含み、約10%の前記粒子が約17〜約23マイクロメートル未満の粒径を有し、約50%の前記粒子が約40〜約45マイクロメートル未満の粒径を有し、約90%の前記粒子が約72〜約77マイクロメートル未満の粒径を有する粒径分布を有し、約0.570を超える流動化かさ密度対安定かさ密度(FBD/SBD)の比率を有するポリマー床を形成する、前記重合触媒。 - 前記重合触媒が少なくとも約77℃の温度で、0.7dg/分のMI、0.912g/cm3の密度、及び26のMFRを有するポリマーを流動床反応器内で形成するメルトフロー応答と、前記触媒が少なくとも約75℃の温度で、1dg/分のMI、0.918g/cm3の密度、及び28のMFRを有するポリマーを流動床反応器内で形成するメルトフロー応答と、を有する、請求項27に記載の前記重合触媒。
- 前記触媒担体に含浸する前記触媒が、ビス(n−プロピルシクロペンタジエニル)ハフニウム(CH3)2、ビス(n−プロピルシクロペンタジエニル)ハフニウムF2、ビス(n−プロピルシクロペンタジエニル)ハフニウムCl2、またはそれらの任意の組み合わせである、請求項27に記載の前記システム。
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