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公开(公告)号：DE3130304A1
公开(公告)日：1983-02-17
申请号：DE3130304
申请日：1981-07-31
Applicant: BASF AG
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公开(公告)号：DE3019493A1
公开(公告)日：1981-11-26
申请号：DE3019493
申请日：1980-05-22
Applicant: BASF AG
Abstract: Catalyst compsn. contg. Ti and used for Ziegler catalysts is mfd. by firstly grinding together (i) a Ti cpd. having the formula TiCl3.zAlCl3 or ClmTiOB4m, where z is 0-0.5, m is 0-3, and B represents a 1-18C alkyl residue; (ii) a magnesium alcoholate (II) having the formula MgOD2, where D is a univalent 1-18C satd. aliphatic and/or aromatic hydrocarbon residue; and (iii) a metal chloride, i.e. AlCl3 or ZnCl2 or MnCl2. The wt. ratio of Ti cpd. to Mg alcoholate is 1:0.2-200 and the wt. ratio of Ti cpd. to ME chloride ranges from 1:0-20. Grinding is effected over 1-200 hrs. at 30-70 m/sec/sec. The prod. (IV) is then mixed with 1:0.01 to 1:1 pts. wt. of a 1-12C alkanol and 1:1 to 1:1000 of a 5-12C alkane to form a suspension (VII) and continuous mixing is effected over 0.5-60 mins. at 0-195 deg.C. The suspension is then treated with a metal cpd. having the formula Mt G-s-t Et, where Mt is Al, Si or Ti, G is a 1-12C residue, E is Cl, Br, H or an -OR residue, R is a 1-12C hydrocarbon residue, s is the highest valency of Mt, and t is a number from 0 to s-1 if Al, 0-4 if Si, or the number 4 if Ti. The suspension is maintained until the Mg content w.r.t. solids metal cpd. lies within the range of 1:0.1 to 1:20. The resulting solids compsn. is the catalyst contg. the Ti. Used pref. in the prodn. of ethylene homopolymers but can also be used for the prodn. of ethylene copolymers. Use of the catalyst reduces the amt. of halogen introduced into the polymer and achieves uniform polymer grain size and/or a redn. of fine-grain prod. and/or high bulk wt.
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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
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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公开(公告)号：DE2914190A1
公开(公告)日：1980-10-30
申请号：DE2914190
申请日：1979-04-07
Applicant: BASF AG
Abstract: A Ti-contg. catalyst component for Ziegler catalysts is prepd. by grinding (I) a solid Ti cpd. chosen from (oxy)chlorides or 1-8C alkoxy chlorides of tri- to tetravalent Ti or TiCl3.Z(AlCl3) (where Z is 0.5) and (II) a halogen cpd. prepd. by heating a cpd. of formula (MII)6(MeIII)2(OH16)(CO3)(1(H2O)4 (where MeIII is Al or Cr and MII is Mg, Ca, Zn or Mn) for 1-100 hrs at 150-600 degrees C and then chlorinating to a Cl content of 40-76 wt.%. (I) and (II) are ground in a wt. ratio of (I):(II) of 1:200-1:2 for 5-100 hrs. at a grinding speed of 4-6 m/s2. The process is characterised by forming a suspension of the above prod. (III), a 1-12C alkanol (IV) and a 5-12C alkane (V) in a wt. ratio of (III):(IV) of 1:0.01-1:1 and wt. ratio of (III):(IV) of 1:1-1:1000, mixing the suspension continuously for 0.5-60 min. at 0-195 degrees C and reacting an acyl halide (VI) RCOX (where R is a satd. 1-18C hydrocarbon gp. which can be opt. substd. by up to 3 Cl or Br atoms and X is Cl, Br, F or I), with the suspension until the atom ratio of Ti in the suspension to halogen in (VI) is 1:0.01-1:100. The catalyst has overall improved properties.
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公开(公告)号：DE2914168A1
公开(公告)日：1980-10-23
申请号：DE2914168
申请日：1979-04-07
Applicant: BASF AG
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Patent Agency Ranking
公开(公告)号：DE2841646A1
公开(公告)日：1980-04-03
申请号：DE2841646
申请日：1978-09-25
Applicant: BASF AG
Inventor： JAGGARD JAMES F R DIPL CHEM DR , HENNENBERGER PETER DIPL CHEM D , STAIGER GERHARD DIPL CHEM DR , KLAERNER PETER DIPL CHEM DR
Abstract: The process involves stopping and restarting the homo- or co-polymerisation 2-6C alpha-monoolefins at 40-120 degrees C. and 1-100 bar using a Ziegler-Natta catalyst of (a) a TiCl3 cocrystallisate of the formula TiCl3.nAlCl3 (in which n = 0.31-0.35), opt. modified with an electron donor, and (b) an Al cpd. of the formula R2AlX (in which R is 1-6C alkyl; X is Cl or R) in an (a):(b) molar ratio of 1:1-100. Polymerisation is stopped by introducing CO and/or CO2 to a concn. of min. 0.5 mmole/l. reactor vol. under 2 min. and restarted by replacing the CO/CO2 with fresh monomer. Overheating and the danger of explosion can be avoided easily and economically. Introduction of the stopper can be controlled automatically by a safety system.
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公开(公告)号：DE2838989A1
公开(公告)日：1980-03-27
申请号：DE2838989
申请日：1978-09-07
Applicant: BASF AG
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公开(公告)号：DE2616587A1
公开(公告)日：1977-11-03
申请号：DE2616587
申请日：1976-04-14
Applicant: BASF AG
Inventor： KLAERNER PETER DIPL CHEM DR , SANDER BRUNO DIPL CHEM DR , KEPPLER HANS GEORG DIPL ING DR , BRONSTERT KLAUS DIPL CHEM DR , GAUSEPOHL HERMANN DIPL CHEM DR
Abstract: Purificn. of waste liquor (I) from the prodn. of styrene bead polymers in the presence of vinylpyrrolidone polymers or vinyl alcohol polymers as suspension stabilisers involves addn. of precipitant and sepn. of the sediment formed 100 pts. (I) are treated with 0.05-3 esp. 0.1-1 pts. water-soluble amide-ammonium or diammonium salt (II) of styrene/maleic anhydride copolymer contg. max. 50 mole% maleic, anhydride, having a Staudinger index of 5-150, pref. 10-60 cm3/g in dimethylformamide at 25 degrees C. An inorganic acid is then added to pH below 3. The improvement comprises the use of (II) contg. 2-40, pref. 5-20 wt.% copolymerised (meth)acrylic acid. The treated liquor is clearer. (II) is added in the form of a 0.1-20 pref. 1-20 wt.% aq. soln. or dispersion. In an example, the addn. of (II) to (I) and adjustment to pH2 reduced the total organic C content of the filtrate from 59,200 to 110 mg C/l and the chemical oxygen demand from 103,200 to 380 mg O2/l.
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公开(公告)号：DE3136254A1
公开(公告)日：1983-03-31
申请号：DE3136254
申请日：1981-09-12
Applicant: BASF AG
Abstract: The invention relates to a process for the preparation of finely divided polymers of alpha -monoolefins by polymerisation in liquid i-butane - in which the monomer to be polymerised is in dissolved form and the finely divided polymer formed is in suspended form - by means of a Ziegler catalyst system comprising 1) a vanadium-containing catalyst component and 2) a metal compound carrying hydrocarbon groups, characterised in that the vanadium-containing catalyst component 1) is the solid-phase product (VII) obtained by 1.1) first bringing 1.1.1) a finely divided, porous, inorganic oxide (I) having a certain specification and 1.1.2) a solution (II) as obtained on combining (IIa) a lower alcohol and (IIb) a vanadium trihalide, into contact with one another to form a dispersion (III), and evaporating this dispersion to a dry consistency - formation of a solid-phase intermediate (IV) - and 1.2) then 1.2.1) bringing the solid-phase intermediate (IV) obtained from step 1.1) and 1.1.2) an aluminium compound (V) having hydrocarbon groups dissolved in an organic solvent into contact with one another to form a dispersion (VI), and in this way isolating, with the solid-phase product (VII) resulting as the dispersed components, the novel vanadium-containing catalyst component 1). This is distinguished, inter alia, by the fact that it is capable of giving polymers having particularly good morphological properties.
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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
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.
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