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    Ziegler type catalyst for (alpha)-olefin (co)polymerisation - giving good control of polymerisation and polymers
    23.
    发明专利
    Ziegler type catalyst for (alpha)-olefin (co)polymerisation - giving good control of polymerisation and polymers 未知

    公开(公告)号：DE2543272A1

    公开(公告)日：1977-04-07

    申请号：DE2543272

    申请日：1975-09-27

    Applicant: BASF AG

    Inventor： SCHWEIER GUENTHER DIPL CHEM DR ,  BACHL ROBERT DIPL CHEM DR ,  MUELLER-TAMM HEINZ DIPL CHEM D ,  FRIELINGSDORF HANS DIPL ING DR ,  GRUBER WOLFGANG DIPL CHEM DR ,  KOLK ERICH DIPL CHEM DR

    IPC: C08F4/62 ,  C08F10/00 ,  C08F4/64

    Abstract: (Co)polymerisation of 2-10C alpha-mono-olefins at 30-200 degrees C/0.1-200 bars press., is effected in the presence of a Ziegler type catalyst system composed of (1) a fraction contg. Ti and/or V (component A) and (2) a metallic cpd. (component B) of formula (I): (Me-Am-nXn (I) (where Me is Al, Mg or Zn or their mixt.; A is 1-12, pref. 2-8C hydrocarbon radical; X is Cl, Br, I or H; m = valency of Me; n is a value between 0 and m-1, pref. 0 or 1). The respective proportions of A and B are such that the atomic ratio between the transition metal of A and the metal Me of B is 1:0.1-1:500, pref. 1:0.2-1:200. The novel component A is a solid prod. prepd. by (a) mixing finely particulate porous SiO2 (prod. I) of particle size 1-1000 u, pref. 1-400 u, a pre vol. of 0.3-3, pref. 1-2.5 cm3/g and an active surface area of 100-1000 pref. 200-400 m2/g with a Mg cpd. (prod. II) dissolved in an organic solvent, in such proportions that the wt. ratio between SiO2 and the Mg cpd. is 1:0.01-1:0.25, pref. 1:0.05-1:0.2, (b) mixing the solid prod. from (a) prod. (III) with a deriv. of Ti and/or V (prod. Iv), in the solid or liq. state or dissolved in an organic solvent, in such proportions that the wt. ratio between prod. III and the transition metal of prod. IV is 1:0.01-1:20, the resulting solid prod. V comprising A. Used for e.g. propene, butene, hexene-1, etc. with component (A), the initiation of the polymerisation is relatively slow and its max. activity is reached progressively, thus allowing control of the polymerisation reaction. The polymers obtd. e.g. polyethylene, have morphologically properties.

    Polymerisation of olefins catalysed by silicic acid xerogels - contg. chromium oxide, leaving low catalyst residues in the polymer
    24.
    发明专利
    Polymerisation of olefins catalysed by silicic acid xerogels - contg. chromium oxide, leaving low catalyst residues in the polymer 未知

    公开(公告)号：DE2540276A1

    公开(公告)日：1977-03-24

    申请号：DE2540276

    申请日：1975-09-10

    Applicant: BASF AG

    Inventor： MUELLER-TAMM HEINZ DIPL CHEM D ,  FRIELINGSDORF HANS DIPL ING DR ,  GONSIOR LEONHARD DIPL CHEM DR ,  GRUBER WOLFGANG DIPL CHEM DR

    IPC: C08F10/00

    Abstract: Olefin polymers are prepd. by polymerising 2-8C monoolefins at 60-100 degrees C and olefin pressures of 0.5-40 bars using a catalyst obtd. by (A) preparing a silicic acid-xerogel by (i) extracting >=60% (pref. >=90%) of the water contained in a silicic acid hydrogel contg. 10-25% (esp. 14-20%) solids (calc. as SiO2) with a 1-4C alcohol and/or 3-5C alkanone; (ii) drying the gel from (ii) at 180 degrees C/10 torr/30 mins. to contact wt. (xerogel formation); (iii) comminuting the xerogel to a dia. of 20-2000 (pref. 40-300) ; (B) admixing the xerogel with solid, finely divided chromium trioxide at 100-300 degrees C/0.001-250 torr until the xerogel takes up 0.1-10% (calc. on the xerogel and as Cr) chromium trioxide; (C) maintaining the prod. from (B) in a gas stream free from water and contg. >10 vol. % O2 at 400-1000 degrees C/10-100 mins. The hydrogel used in (A) comprises spherical, particles at dia. 1-8 mm., pref. 2-6mm. and is prepd. by (i) introducing a soln. of Na or K silicate along the length and also tangentially to a spiralling stream of an aq. inorganic acid; (ii) spraying the resulting silicic acid hydrogel into a gaseous medium dropwise; (iii) allowing the sprayed hydrogel to solidify in the gaseous medium; (iv) washing the resulting spherical hydrogel without prior ageing to remove salts. Used esp. for ethylene polymerisation. The catalyst gives high productivity, and the catalyst content of the polymer is so small that it need not be removed.

    Ziegler catalyst for alpha:mono:olefin (co)polymerisation - has solid titanium component treated with acyl halide, facilitating mol. wt. control
    27.
    发明专利
    Ziegler catalyst for alpha:mono:olefin (co)polymerisation - has solid titanium component treated with acyl halide, facilitating mol. wt. control 未知

    公开(公告)号：DE2829623A1

    公开(公告)日：1980-01-24

    申请号：DE2829623

    申请日：1978-07-06

    Applicant: BASF AG

    Inventor： BACHL ROBERT DIPL CHEM DR ,  EHLERS EHLER ING GRAD ,  FRIELINGSDORF HANS DIPL ING DR ,  SCHWEIER GUENTHER DIPL CHEM DR

    IPC: C08F4/64 ,  C08F10/00

    Abstract: Ziegler catalyst for the (co)polymerisation of 2-6 C alpha-monoolefins at 30-200 degrees C. and 0.1-200 bar consists of a Ti-contg. component (I) and a metal cpd. (II) of formula MAm-nXn (in which M is Al, Mg, and/or Zn. A is a 1-12C hydrocarbyl gp. X is Cl, Br, I and/or H. m is the valency of M. n is 0 to m-1), the Ti:M atomic ratio being 1:0.1-500. The novelty is that (I) is a solid phase prod. obtd. as follows. A finely-divided porous SiO2.aAl2O3 (III) (a = 0-2) with a particle dia. of 1-1000 mu m, pore vol. of 0.3-3 cm.3/g. and a surface area of 100-1000 m.2/g. is dispersed in a soln. (IV) contg. 100 (wt.) pts. alcohol Z-OH (in which Z is a satd. 1-8C hydrocarbyl gp.). 0.06-1 pts. (as Ti) of TiX'o (in which X' is Cl and/or Br) and 0.01-4 pts. (as Mg) of a Mg cpd. (V) of formula Mg6Alw(OH)xYy(B-OH)z (in which Y is Cl or Br. B is a satd. 1-8C hydrocarbyl gp. w is 0-3, x is 0-8, y = 12+3w-z and z is 0-36), which is soluble in Z-OH, to give a wt. ratio of (III):Ti in TiX'3 of 1:0.001-0.2 and of (III):Mg in (V) of 1:0.01-0.25. The dispersion is evapd. to dryness at 200 degrees C. and above the m.pt. of Z-OH. The solid intermediate obtd. is suspended in an acyl halide opt. dissolved in an organic solvent, to give a wt. ratio of Ti in the intermediate : R-CO-X of 1 : 0.01-100, giving a suspension of (I). Good mol. wt. control is attainable with less mol.wt. regulator than usual and the polymers have much better morphological properties (bulk density and flow). Polymerisation can be carried out (dis)continuously by the suspension, soln., or dry phase process.

    Ziegler catalyst component contg. titanium - is prepd. by combining carrier, titanium tri:halide and magnesium cpd. in alcohol and mixing prod. with aluminium- or silicon cpd.
    28.
    发明专利
    Ziegler catalyst component contg. titanium - is prepd. by combining carrier, titanium tri:halide and magnesium cpd. in alcohol and mixing prod. with aluminium- or silicon cpd. 未知

    公开(公告)号：DE2721094A1

    公开(公告)日：1978-11-23

    申请号：DE2721094

    申请日：1977-05-11

    Applicant: BASF AG

    Inventor： SCHWEIER GUENTHER DIPL CHEM DR ,  BACHL ROBERT DIPL CHEM DR ,  KOLK ERICH DIPL CHEM DR ,  KLAERNER PETER DIPL CHEM DR ,  FRIELINGSDORF HANS DIPL ING DR

    IPC: C08F4/64 ,  C08F10/00

    Abstract: catalyst component is prepd. by (1) contacting a finely divided carrier (I), with a soln. (II), prepd. by mixing (IIa) 100 pts. wt. alcohol having formula Z-OH (where Z is a satd. 1-8C hydrocarbyl (IIb) 0.01-6 pts. wt. (calculated as Ti) of a Ti trihalide (where halogen is Cl and/or Br) and (IIc) 0.01-4 pts. wt. (calculated as Mg) of an Mg cpd. soluble in (IIa), to form a dispersion (III). Wt. ratio (I):Ti in (IIb) is 1:0.01 to 1:0.2. Wt. ratio (I):Mg in (IIc) is 1:0.01 to 1:0.25. The dispersion (III) is evaporated to dryness, below 200 degrees C but above m.pt. of (IIa), to form a solid-phase intermediate prod. (IV). this is followed by (2) contacting with a metal cpd. (V) dissolved in an organic solvent, to form a dispersion. (V) has formula MtGs-tEt (where Mt is Al or Si; G is 1-12C hydrocarbyl; E is Cl, Br, I, H or -OD; D is a 1-12C hydrocarbyl; s is valency of Mt and t is I to s-1 when Mt is Al or 0.4 when Mt is Si). Wt. ratio (IV):(V) is 1:0.05 to 1:2. The resulting dispersed solid-phase prod. (VI) is the Ti-contg. catalyst component. The Ziegler catalyst systems are used in homo- and copolymerisation of 2-6C monolefins at 30-200 degrees C and 0.1-200 bar. Constant specific polymer yields are obtd. Polymer particles where high bulk wt. and fluidity. Polymer dust particle content is very small. Productivity, measured as polymer quantity/Ti, is high. Ti and halogen proportions in polymer are so small as to obviate a purifying step.

    Catalyst for polymerisation of olefins - using a chromium and an alkyl metal cpd. on a silicate type carrier
    29.
    发明专利
    Catalyst for polymerisation of olefins - using a chromium and an alkyl metal cpd. on a silicate type carrier 未知

    公开(公告)号：DE2604551A1

    公开(公告)日：1977-08-11

    申请号：DE2604551

    申请日：1976-02-06

    Applicant: BASF AG

    Inventor： GRUBER WOLFGANG DIPL CHEM DR ,  FRIELINGSDORF HANS DIPL ING DR ,  MUELLER-TAMM HEINZ DIPL CHEM D ,  MERZ GERHARD DIPL CHEM DR ,  GONSIOR LEONARD DIPL CHEM DR

    IPC: C08F4/24 ,  C08F10/00 ,  C08F4/62

    Abstract: Prepn. of a catalyst for the polymerisation of olefins, the catalyst being obtd. from a Si contg. material (a), and alkyl gp. contg. metal organic cpd. (b), and a Cr cpd. (c) (1)(i) an Alcogel (a) of the empirical formula SiO2.-mAl2O3. nROH (m=0-2, n=a number which gives 1-85% ROH, R=3-8C alkyl) and (ii) an alkyl gp. contg. Al Cpd. (b) of formula R'pAl(OR")3-p (R'=1-8C alkyl, R"=1-8C open chain alkyl ro a ring closed 5-8C alkyl, p=1-3) are well mixed to form a solid phse reaction prod. (2) The prod. from (1) and a soln. of a Cr cpd. (c) (CrO3 or a cpd. convertible to CrO3 in stage (3)) are well mixed and the solvent evaporated. (3) The stage (2) prod. is held in a gas stream contg. >=10 vol. % of 0 for 10-400 minues at 600-1000 degrees C. In the catalyst, for 100 pts. wt. of (a) as SiO2, there are 0.1-10 pts. wt. of (b) as Al and 0.3-10 pts. wt. of (c) as CrO3. The prods. of stage (1) and (2) are dried and ground before further processing so that they show no wt. loss in 30 minutes at 100 degrees C and 10 Torr press., and have a particle diam. of 20-2000 mu m. The catalysts can be modified to allow properties of the polymer e.g. density melt index, G modulus, to be varied and they need not be removed from the polymers. The polymes are esp. suitable for the prepn. of small hollow body mouldings without melt fracture and weld lines and with a high stress crack corrosion resistance.

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