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European Patent Office Europäisches Patentamt *EP000942006B1* (19) European Patent Office Office européen des brevets (11) EP 0 942 006 B1 (12) EUROPEAN PATENT SPECIFICATION (45) Date of publication and mention (51) Int Cl.7: C08F 4/602, C08F 4/606, of the grant of the patent: C08F 10/00 04.06.2003 Bulletin 2003/23 (21) Application number: 99301730.0 (22) Date of filing: 08.03.1999 (54) Catalyst for olefin polymer production and process for olefin polymer production employing the catalyst Katalysator für Olefinpolymerisation und Verfahren zur Herstellung von Olefinpolymer unter Verwendung desselben Catalyseur de polymérisation d’oléfines et procédé de production de polymère d’oléfines utilisant celui-ci (84) Designated Contracting States: (74) Representative: Copsey, Timothy Graham et al DE FR NL Kilburn & Strode, 20 Red Lion Street (30) Priority: 09.03.1998 JP 5658598 London WC1R 4PJ (GB) 11.01.1999 JP 380399 (56) References cited: (43) Date of publication of application: EP-A- 0 658 576 15.09.1999 Bulletin 1999/37 • CHEMICAL ABSTRACTS, vol. 123, no. 20, 13 (73) Proprietor: TOSOH CORPORATION November 1995 (1995-11-13) Columbus, Ohio, Shinnanyo-shi, Yamaguchi-ken (JP) US; abstract no. 274205, GOLUB, A. S. ET AL: "Formation of intercalation compounds of MoS2 (72) Inventors: with alkali metal and alkylammonium cations • Yamada, Satoru from a monolayer dispersion of molybdenum Mie-gun, Mie (JP) disulfide" XP002133340 & IZV. AKAD. NAUK, • Yano, Akihiro SER. KHIM. (1993), (4), 672-4 , Yokkaichi-shi, Mie (JP) Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition shall be filed in a written reasoned statement. It shall not be deemed to have been filed until the opposition fee has been paid. (Art. 99(1) European Patent Convention). EP 0 942 006 B1 Printed by Jouve, 75001 PARIS (FR) EP 0 942 006 B1 Description Background of the Invention: 5 Field of the Invention: [0001] The present invention relates to a catalyst for olefin polymer production comprising a metallocene compound, a reaction product of topotactic reduction by electron transfer, and an organoaluminum compound, and a process for producing an olefin polymer employing the catalyst. 10 [0002] The present invention relates also to a catalyst for olefin polymer production comprising a metallocene com- pound, a product of a topotactic reduction reaction by electron transfer, an organoaluminum compound, and organo- alkaline earth metal compound or an organozinc compound, and a process for producing an olefin polymer employing the catalyst. 15 Description of the Related Art: [0003] A catalyst composed of a metallocene compound and an organoaluminum compound, and another catalyst composed of a metallocene compound, an organoaluminum compound, and an organomagnesium compound are disclosed as the catalyst for producing an olefin polymer (JP-A-3-197513, and JP-A-3-290408). However, these cat- 20 alysts are not satisfactory in the catalyst activity. [0004] Active catalysts for olefin polymer production are disclosed which are composed of a metallocene compound and a methylaluminoxane (JP-A-58-19309, and JP-A-60-35007). These catalyst employs a large amount of expensive aluminoxane to produce a polymer having industrially useful properties, which causes problems of high catalyst cost and residual aluminum. 25 [0005] Highly active olefin polymerization catalysts not containing the methylaluminoxane are disclosed which com- prises a metallocene compound, a boron compound, and an organoaluminum compound (Kohyo 1-501950, and Kohyo 1-502036). However, the boron compound for this catalyst is complicated and expensive, disadvantageously. Summary of the Invention: 30 [0006] The present invention intends to solve the above technical problems, and to provide a catalyst for olefin polymer production with high catalyst activity without using an expensive catalyst component. The present invention provides also a process for producing an olefin polymer with the catalyst. [0007] The olefin polymerization catalyst of the present invention comprises [A] a metallocene compound containing 35 a transition metal selected from Groups 3, 4, 5, and 6 of Periodic Table, [B] a reaction product of topotactic reduction with electron transfer, and [C] an organoaluminum compound. [0008] The olefin polymerization catalyst of another embodiment of the present invention comprises [A] a metallocene compound containing a transition metal selected from Groups 3, 4, 5, and 6 of Periodic Table, [B] a reaction product of topotactic reduction by electron transfer, [C] an organoaluminum compound, and [D] an organoalkaline earth metal 40 compound or an organozinc compound. [0009] The process for producing an olefin polymer of the present invention uses the above catalyst. Detailed Description of the Preferred Embodiment: 45 [0010] The topotactic reduction with electron transfer in the present invention is a reaction, as defined by R. Schöll- horn: Angew. Chem. Int. Ed. Eng., 19, 983-1003 (1980), in which a host compound is reduced by electrons and guest cations are introduced into vacant lattice sites of the host compound to balance the electric charges without change of the structure and composition of the host compound by the reaction. This reaction is represented by General Formula (35) below: 50 + - + x- xE + xe + h[Q] - (E )x [Q] (35) where [Q] is the host compound, h is a vacant lattice site of [Q], e- is an electron, x is a number of reduction, and E+ 55 is a monovalent guest cation. [0011] The component [B] in the present invention is a reaction product of the above electron-transferring topotactic reduction, and is represented by General Formula (36): 2 EP 0 942 006 B1 n+ 2 k- E(k/n)(L )h[Q] (36) where [Q] is a host compound, k is a number of reduction, En+ is an n-valent guest cation, L2 is a Lewis base, and h 5 is a number of the Lewis base. [0012] The host compound [Q] includes host compounds of three-dimensional structure, host compounds of two- dimensional structure, host compounds of one-dimensional structure, and host compounds of a molecular solid. [0013] The host compounds of three-dimensional structure include hexamolybdenum octasulfide, hexamolybdenum octaselenide, trimolybdenum tetrasulfide, trititanium tetrasulfide, hexatitanium octaselenide, triniobium tetrasulfide, 10 hexavanadium octasulfide, pentavanadium octasulfide, divanadium pentaoxide, tungsten trioxide, titanium dioxide, vanadium dioxide, chromium dioxide, manganese dioxide, tungsten dioxide, ruthenium dioxide, osmium dioxide, and iridium dioxide. [0014] The host compounds of two-dimensional structure include titanium disulfide, zirconium disulfide, hafnium disulfide, vanadium disulfide, niobium disulfide, tantalum disulfide, chromium disulfide, molybdenum disulfide, tungsten 15 disulfide, rhenium disulfide, platinum disulfide, tin disulfide, lead disulfide, titanium diselenide, zirconium diselenide, hafnium diselenide, vanadium diselenide, niobium diselenide, tantalum diselenide, chromium diselenide, molybdenum diselenide, tungsten diselenide, rhenium diselenide, platinum diselenide, tin diselenide, lead diselenide, titanium ditel- luride, zirconium ditelluride, hafnium ditelluride, vanadium ditelluride, niobium ditelluride, tantalum ditelluride, chromium ditelluride, molybdenum ditelluride, tungsten ditelluride, rhenium ditelluride, platinum ditelluride, tin ditelluride, lead 20 ditelluride, magnesium phosphorus trisulfide, calcium phosphorus trisulfide, vanadium phosphorus trisulfide, manga- nese phosphorus trisulfide, iron phosphorus trisulfide, cobalt phosphorus trisulfide, nickel phosphorus trisulfide, palla- dium phosphorus trisulfide, zinc phosphorus trisulfide, cadmium phosphorus trisulfide, mercury phosphorus trisulfide, tin phosphorus trisulfide, magnesium phosphorus triselenide, calcium phosphorus triselenide, vanadium phosphorus triselenide, manganese phosphorus triselenide, iron phosphorus triselenide, cobalt phosphorus triselenide, nickel 25 phosphorus triselenide, palladium phosphorus triselenide, zinc phosphorus triselenide, cadmium phosphorus trisele- nide, mercury phosphorus triselenide, tin phosphorus triselenide, chromium phosphorus tetrasulfide, tantalum sulfide carbide, molybdenum trioxide, octadecamolybdenum dopentacontaoxide (18-molubdenum 52-oxide), divanadium pentaoxide gel, iron oxychloride, titanium oxychloride, vanadium oxychloride, chromium oxychloride, aluminum oxy- chloride, bismuth oxychloride, α-zirconium nitride chloride, β-zirconium nitride chloride, α-zirconium nitride bromide, 30 β-zirconium nitride bromide, zirconium nitride iodide, titanium nitride chloride, titanium nitride bromide, titanium nitride iodide, graphite, and polyacene. [0015] The host compounds of one-dimensional structure include titanium trisulfide, niobium triselenide, potassium iron disulfide, polyacetylene, polyaniline, polypyrrole, polythiophene, poly(p-phenylene), poly(triphenylene), polyazu- lene, polyfluorene, polynaphthalene, polyanthracene, polyfuran, polycarbazole, tetrathiafulvalene-substituted polysty- 35 rene, ferrocene-substituted polyethylene, carbazole-substituted polyethylene, and polyoxyphenazine. [0016] The host compounds of a molecular solid include tetracyanoquinodimethane, and tetrathiafulvalene. [0017] The host compound [Q] may be a mixture of two or more of the above host compounds. [0018] The number of reduction, k, is preferably in the range of 0 < k ≤ 3, more preferably
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