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    1.
    发明专利
    未知

    公开(公告)号：DE3144312A1

    公开(公告)日：1983-05-19

    申请号：DE3144312

    申请日：1981-11-07

    Applicant: BASF AG

    Inventor： JAGGARD JAMES F R DIPL CHEM DR ,  SCHWEIER GUENTHER DIPL CHEM DR ,  KLAERNER PETER DIPL CHEM DR

    IPC: C08F297/08 ,  C08F293/00

    Abstract: Propylene/ethylene block copolymers are prepared by a process in which, in an agitated bed comprising small polymer particles, first (I) propylene is homopolymerized from the gas phase, in a first polymerization zone, by feeding in a Ziegler-Natta catalyst comprising (1) a titanium(III) component and (2) a dialkyl-aluminum chloride component, with or without (3) a further catalyst component, and then (II) the product obtained in the first polymerization zone is fed into a second polymerization zone, where a mixture of propylene and ethylene is polymerized with the propylene homopolymer present in this product. In this process, the Ziegler-Natta catalyst employed contains a titanium(III) component (1) which is prepared by subjecting (1.1) a titanium-containing compound (a) of the formula TiCl3. nAlCl3 and (1.2) an electron donor (b), consisting of (b1) an ester of a particular class or (b2) a phosphorus-containing compound of a particular class, to a special milling procedure, the particular features of which are special metering and temperature conditions, suspending the resulting intermediate in a mixture of a liquid hydrocarbon (c) and an oxygen-containing compound (d), comprising (d1) an ether of a certain class and/or (d2) an ester of a certain class, and then heating the suspension obtained. The solid remaining in suspension is the titanium(III) component (1) which is to be employed for the polymerization. The polymer obtained has improved morphological properties.

    Trivalent titanium component prepn. for Ziegler-Natta catalyst system - by grinding titanium tri:chloride complex with phosphorus cpd. and reacting with ether and/or ester
    2.
    发明专利
    Trivalent titanium component prepn. for Ziegler-Natta catalyst system - by grinding titanium tri:chloride complex with phosphorus cpd. and reacting with ether and/or ester 未知

    公开(公告)号：DE3021296A1

    公开(公告)日：1982-01-07

    申请号：DE3021296

    申请日：1980-06-06

    Applicant: BASF AG

    Inventor： JAGGARD JAMES F R DIPL CHEM DR ,  KLAERNER PETER DIPL CHEM DR ,  STAIGER GERHARD DIPL CHEM DR

    IPC: C08F4/64 ,  C08F10/00

    Abstract: In the prepn. of a new Ti(III)-component (1) for Ziegler-Natta catalyst systems, a Ti-contg. cpd. having TiCl3.nAlCl3, (A), (where n is 0.01-1) is ground with a P-contg. cpd. having formula OmP(R1)3, (B), (where m is 0 or 1 ; R1 is R2, OR2 or N(R2)2 and R2 is 1-24C alkyl, aryl, alkaryl or aralkyl). Specific grinding conditions are used. (B) is added to (A) in quantities corresponding to molar ratio Ti in (A) : (B) 1 : 0.01 to 1 : 1. A suspension of (i) 1 pt.wt. of prod.; (ii) 0.5-20 pts.wt. hydrocarbon, (C), liq. under normal conditions and boiling below 150 deg.C; and (iii) an O-contg. cpd. (D) is prepd. (D) can be a 4-30C ether of formula R8-O-R8' (where R8 and R8' are 1-15C alkyl, Ph or 7-14C alkyl-phenyl) and/or a 2-34C ester having formula R9'-O-CO-R9 or R9'-O-CO-CR9=CHR9 (where R9 is H, 1-12C alkyl, 7-14C phenyl-alkyl in which Ph is opt. mono-alkyl substd., Ph or 7-14C alkyl-phenyl ; R9' is 1-8C alkyl, Ph or 7-14C phenyl-alkyl). (D)-quantities are such that molar ratio Ti in (A) to (D) is 1 : 0.01 to 1 : 2. The suspension is strongly stirred 5-120 min. at 40-140 deg. C and cooled to 15-25 deg.C. The solid separated from the suspension is opt. washed with a hydrocarbon, liq. under normal conditions and boiling below 150 deg.C and dried to recover the new Ti(III)-componentt (1). The catalyst systems are used in 2-6C alpha-mono-olefin (co)polymerisation. Stereoregular polymers are obtd. in high yields. The prods. have a low fine grain proportion.

    Trivalent titanium component prepn. for Ziegler-Natta catalyst system - by grinding titanium tri:chloride complex with ester and reacting with alcohol
    3.
    发明专利
    Trivalent titanium component prepn. for Ziegler-Natta catalyst system - by grinding titanium tri:chloride complex with ester and reacting with alcohol 未知

    公开(公告)号：DE3021297A1

    公开(公告)日：1982-01-07

    申请号：DE3021297

    申请日：1980-06-06

    Applicant: BASF AG

    Inventor： JAGGARD JAMES F R DIPL CHEM DR ,  KLAERNER PETER DIPL CHEM DR ,  STAIGER GERHARD DIPL CHEM DR

    IPC: C08F4/64 ,  C08F10/00

    Abstract: In the prepn. of a new Ti(III)-component, (1), for Ziegler-Natta catalyst systems, a Ti-contg. cpd., (A), having formula TiCl3.nAlCl3 (where n is 0.01-1) is ground with a 2-34C ester, (B), having formula R1-O-CO-R2 or R1-O-CO-CR2=CHR2 (where R1 is 1-16C alkyl or 7-23C phenyl-alkyl in which the Ph gp. is opt. substd. by up to 5 1-4C alkyl gps.; R2 is H, 1-18C alkyl, 7-23C phenyl- alkyl or 7-23C alkyl-phenyl in which Pb is opt. substd. by up to 5 1-4C alkyl gps.). Specific grinding conditions are used. (B) is added to (A) in quantities corresponding to molar ratio Ti in (A) : (B) 1 : 1.5 to 1 : 0.01. A suspension of (i) 1 pt.wt. prod.; (ii) 0.5-20 pts.wt. hydrocarbon, (C), liq. under normal conditions and boiling below 150 deg.C; and (iii) a 1-20C alcohol, (D), having formula X(OH)y (where y is 1 or 2 and X is an aromatic, satd. aliphatic or cycloaliphatic hydrocarbyl gp.) is prepd. D-quantity is such as to set up molar ratio Ti in (A) : (D) 1 : 0.01 to 1 : 2. The suspension is then strongly stirred 5-120 min. at 40-140 deg.C and then cooled to 15-25 deg.C. The suspension is opt. mixed with an Al-contg cpd. (E) having formula Al(R8)x(Y)3-x (where x is 1-3; Y is Cl or R8; R8 is 1-12C alkyl). Quantities are such as to set up molar ratio OH gps. from (D) : alkyl gps. in (E) 1 : 0.005 to 1 : 2. The solid sepd. from the suspension is opt. washed with a hydrocarbon, liq. under normal conditions and boiling below 150 deg.C, and dried, to recover (I). The catalyst systems are used in 2-6C alpha-mono-olefin (co)polymerisation. Stereoregular polymers are obtd. in high yields. Fine grain proportion is reduced.

    8.
    发明专利
    未知

    公开(公告)号：DE3018113A1

    公开(公告)日：1981-11-19

    申请号：DE3018113

    申请日：1980-05-12

    Applicant: BASF AG

    Inventor： JAGGARD JAMES F R DIPL CHEM DR ,  KLAERNER PETER DIPL CHEM DR ,  SCHWEIER GUENTHER DIPL CHEM DR

    IPC: C08F4/64 ,  C08F10/00

    Abstract: A process for the preparation of homopolymers and copolymers of alpha -monoolefins by means of a Ziegler-Natta catalyst system comprising (1) a titanium-III component, which is prepared by subjecting (1.1) a titanium trichloride/aluminum trichloride compound (a) and (1.2) an ester (b) to a certain type of milling treatment in which (A) a vibratory ball mill providing a relatively high milling acceleration is used, (B) the mill is first charged with the titanium-containing compound (a) and, if appropriate, is run for a certain period, thereafter (C) the ester (b) is added at a certain rate while milling the charge, thereupon (D) the charge is kept at +15 DEG C. or above for a certain period, while continuing the milling, hereupon (E), if appropriate, the product obtained from (D) is milled further for a certain period at +5 DEG C. or below, then (F), if appropriate, but advantageously so, the product obtained from (D) or (E) is kept at +20 DEG C. or above for a certain period, without milling, and thereafter (G), if appropriate, the product obtained from (F) is milled further for a certain period at +5 DEG C. or below, (2) an aluminum-alkyl component containing a chlorine bonded to the aluminum, and (3), if appropriate, a phenolic compound of a certain category, in which process a titanium-III component (1) is employed, in the preparation of which additionally -(H) a suspension is prepared from (H1) the product obtained according to (D), (E), (F) or (G), (H2) a liquid hydrocarbon (c) and (H3) an oxygen-containing compound (d), consisting of (d1) an ether of a certain category and/or (d2) an ester of a certain category, thereafter (I) the suspension obtained according to (H) is kept at an elevated temperature for a certain period, with vigorous agitation, and is then cooled, hereupon (J), if appropriate, the solid is isolated from the suspension obtained according to (I), and, if desired, is washed with a liquid hydrocarbon and dried, the novel titanium-III component (1) being the solid, in suspended form, obtained according to (I) or the solid, in isolated form, obtained according to (J). Using this Ziegler-Natta catalyst system, polymers with relatively high stereo-regularity and advantageous morphological properties can be obtained in relatively high yield.

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