PDF《TEPZZ_58B_T》

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75001 PARIS (FR) (19) EP

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525 B1 TEPZZ_58?5?5B_T (11) EP

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525 B1 (12) EUROPEAN PATENT SPECIFICATION (45) Date of publication and mention of the grant of the patent: 17.12.2014 Bulletin 2014/51 (21) Application number: 05007953.2 (22) Date of filing: 19.12.1997 (51) Int Cl.: C07F 5/02 (2006.01) B01J 37/00 (2006.01) C08F 4/643 (2006.01) C08F 210/16 (2006.01) C08F 4/6592 (2006.01) C01B 35/06 (2006.01) B01J 31/14 (2006.01) B01J 35/02 (2006.01) (54) Boron compound in the form of fine particles, component of catalyst for olefin polymerization comprising the same and method for producing the same Borverbindung in Form feiner Teilchen, Katalysatorkomponente für die Olefinpolymerisation, die diese enthalten und Verfahren zu dessen Herstellung Composé au bore sous forme de fines particules, constituant catalyseur pour polymérisation d'

oléfines à base dudit composé, et procédé de production de celui-ci (84) Designated Contracting States: DE (30) Priority: 20.12.1996 JP

34198896 14.01.1997 JP

503397 14.01.1997 JP

503497 04.07.1997 JP

17969397 (43) Date of publication of application: 05.10.2005 Bulletin 2005/40 (60) Divisional application: 10012390.0 /

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918 (62) Document number(s) of the earlier application(s) in accordance with Art.

76 EPC: 97949174.3 /

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062 (73) Proprietor: Sumitomo Chemical Company, Limited Tokyo 104-8260 (JP) (72) Inventors: ? Sato, Hideki Chiba, 299-0017 Japan (JP) ? Katayama, Hiroaki Chiba, 275-0017 Japan (JP) ? Wakamatsu, Kazuki Chiba, 299-0246 Japan (JP) (74) Representative: Vossius &

Partner Siebertstrasse

4 81675 München (DE) (56) References cited: EP-A-

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781 ? DATABASE WPI Section Ch, Week

199427 Derwent Publications Ltd., London, GB;

Class A23, AN 1994-222075 XP002377547 &

JP

06 157782 A (TEIJIN LTD)

7 June

1994 (1994-06-07) EP

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50 55 Description [0001] The present application discloses a method for feeding a specific boron compound to a reactor, a boron compound having a controlled particle diameter useful as a component of a catalyst for polymerization of an olefin and a method for producing the same. More par- ticularly, it discloses a method for continuously feeding a boron compound useful as a component of a catalyst for polymerization of an olefin to a reactor, particularly an apparatus for preparing a catalyst or a reactor for po- lymerization of an olefin, said boron compound having a controlled particle diameter, and a method for producing said boron compound. [0002] Many reports have already been presented on methods for producing olefin polymers with catalysts for olefin polymerization, which uses a transition metal com- pound (e.g. a metallocene complex or non-metallocene complex) and a specific boron compound. Said boron compound, whichisalsocommerciallyavailable inrecent years, is usually a solid containing large size particles having a particle diameter of several hundreds microm- eters to several millimeters , and while it is soluble in toluene to some extent, it has a low solubility in most, solvents including saturated hydrocarbons. Therefore, conventionally it has been used in a solution having not so high concentration or used by adding undissolved part of said boron compound remaining in solid form into a vessel. [0003] For example, In Japanese Patent Publication (Kohyo) No. Hei 1-502036 discloses a method for pro- ducing an olefin polymer in which tri-n-butylammonium tetrakis(phenyl)borate is suspended in toluene, bis(pen- tamethylcyclopentadienyl) zirconium dimethyl is added thereto, Cp*2Zr(C6H4)B(C6H5)3 ?wherein Cp* repre- sentsη5-pentamethylcyclopentadienylgroup?isisolated and used as a catalyst for polymerization of an olefin. In thismethod, tri-n-butylammonium tetrakis(phenyl)borate is provided in advance in the form of a suspension in toluene in a reactor for preparing a catalyst, and the cat- alyst isprepared by adding a metallocene complex there- to. [0004] In addition, inU.S. Patent Specification No. 5, 408, 017, it is disclosed that a method for producing an olefin polymer in a high-pressure polymerization appa- ratus at 1,300 bar, in which method N,N-dimethylanilin- ium tetrakis(pentafluorophenyl)borate and dimethylsilyl- bis(4,5,6,7-tetrahydroindenyl) zirconium dimethyl are mixed in toluene to prepare a homogeneous catalyst so- lution, which is used as a catalyst for polymerization of an olefin. In this method, while a solid N,N-dimethylanilin- ium tetrakis(pentafluorophenyl)borate is used for the preparation of the catalyst, a homogeneous catalyst so- lution is provided before use for polymerization by mixing it with the metallocene complex in toluene, and then said solution is continuously fed to a polymerization reactor with a high-pressure pump. [0005] Furthermore, Japanese Patent Publication (Kokai) No. Hei 7-157508 discloses a method in which a solution of triisobutyl aluminum in toluene is added to a solution of diphenylmethylene(cyclopentadienyl) (fluore- nyl) zirconium dichloride in toluene in a separate vessel before use for polymerization, and further, a solution of N,N-dimethylanilinium tetrakis(pentafluorophenyl)bo- rate intoluene isadded toobtainahomogeneouscatalyst solution, then said solution is fed to a high-temperature high-pressure polymerization reactor. [0006] Conventionally, as described above, when said boron compound is continuously fed to a reactor, a dis- continuous procedure for preparing a homogeneous cat- alyst solution in a separate vessel, was adopted or a so- lution having not so high concentration was used. [0007] In Published Specification No. WO94/00459, there is described a method for producing said boron compound and a method for purifying a produced crude boron compound that is colored. According to said meth- od for purification, a method is disclosed in which the produced crude boron compound dissolved in ethers........