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    Polymerisation of olefins catalysed by silicic acid xerogels - contg. chromium oxide, leaving low catalyst residues in the polymer
    2.
    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.

    Olefin polymn catalyst - made by heating silicic acid xerogel with solid chromium trioxide
    4.
    发明专利
    Olefin polymn catalyst - made by heating silicic acid xerogel with solid chromium trioxide 未知

    公开(公告)号：DE2411711A1

    公开(公告)日：1975-09-25

    申请号：DE2411711

    申请日：1974-03-12

    Applicant: BASF AG

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

    IPC: C08F4/22 ,  C08F10/00

    Abstract: Polyolefins are made by polymerising 2-8 C alpha-mono-olefins at 60-160 degrees C and olefin pressures of 0.5-40 bar using silicic acid xerogel/CR2O3 catalysts made by (1) forming a finely divided silica xerogel with a particle size of 10 to 2000 mu m by (a) making a 10-25 wt. % solids (as SiO2) silicic acid hydrogel, (b) extracting water from the hydrogel with a 1-4 C alkanol and/or a 3-5 C alkanone until the org. liq. takes up no more water and (c) drying the dewatered gel, saturated with the org. liq. until no further wt. loss occurs on heating at 180 degrees C/10 Torr for 30 mins.; (2) mixing the resulting xerogel with solid, finely divided CR2O3 and heating at 100-300 degrees C/0.01-250 Torr until the xerogel has taken up 0.1-10 wt. % CR2O3 (calculated as Cr) and (3) treating the prod. for 10-1000 min. at 40-1100 degrees C in a moisture-free gas stream contg. >10 vol. % O2. The catalysts give high yields and high productivity, and the resulting polymers have relatively narrow particle size distribution, low fines content and a sufficiently high melt index when made in the absence of mol. wt. regulators.

    Olefin polymn. catalyst prodn. - by forming silicic acid-xerogel and charging with chromium trioxide
    6.
    发明专利
    Olefin polymn. catalyst prodn. - by forming silicic acid-xerogel and charging with chromium trioxide 未知

    公开(公告)号：DE2455557A1

    公开(公告)日：1976-05-26

    申请号：DE2455557

    申请日：1974-11-23

    Applicant: BASF AG

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

    IPC: C08F10/00 ,  C08F4/24

    Abstract: Silicic acid-xerogel/Cr2O3 catalyst for polymsn. of olefins is obtd. by (1) first forming a finely divided (10-200 mu-m. dia.) silicic acid xerogel, (2) charging the xerogel with 0.1-10wt.% (w.r.t. the xerogel and calc. as Cr) of Cr2O3 or a Cr cpd. which forms Cr2O3 in step (3), and (3) holding the resulting prodt. in a water-free gas stream contg. >10vol.% 02, for 10-1000 mins. at 400-1100 degrees C, the silicic acid-xerogel being produced by (1.ue starting from a 0.1-20wt.% solids (calc. as SiO2) contg. aq. soln. of water glass, (1.2) exchanging the Na+ ion in the soln. for H+ with an ion exchanger until the Na content (calc. as Na2O) in the silicic acid xerogel amts. to is not >0.2wt.%, (1.3) adding to the soln. a water-sol Al salt (and opt. water) of such a kind that a wt. ratio water:silicic acid (calc. as SiO2) of 100:0.05-100:24 as well as a wt. ratio SiO2:Al2O3 of 100:100-100: 2 is obtd., (1.4) opt. bringing the resulting soln. to a pH of 0.1-3.5 with an aq.inorganic acid soln. of such a kind that the wt.ratio water:silicic acid and SiO2:Al2O3 remain as in (1.3), (1.5) bring the resulting soln. to a pH of 4-12 with a water-sol. neutralising nitrogen base, (1.6) extracting the resulting solid phase prodt. (silicic acid hydrogel) using a 1-4C alkanol and/or 3-5C alkanone until the organic liq. takes up no more water, and finally (1.7) drying the dehydrated gel, which is satd. with organic liq. until at 120 degrees C no further wt. loss occurs (xerogel-formation). The resulting catalyst can be used for polymsn. of olefins in the absence of M.W- regulators or in presence of a comparatively small amt. of M.W. regulator.

    Olefin polymn catalyst - made by heating silicic acid xerogel with solid chromium trioxide
    7.
    发明专利
    Olefin polymn catalyst - made by heating silicic acid xerogel with solid chromium trioxide 未知

    公开(公告)号：DE2411734A1

    公开(公告)日：1975-09-25

    申请号：DE2411734

    申请日：1974-03-12

    Applicant: BASF AG

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

    IPC: C08F4/24 ,  C08F10/00

    Abstract: Olefin polymsn. catalysts are made by (1) forming a finely divided silica xerogel with a particle size of 10 to 2000 mu m by (a) making a 10-25 wt. % solids (as SiO2) silicic acid hydrogel, (b) extracting water from the hydrogel with a 1-4 C alkanol and/or a 3-5 C alkanone until the org. liq. takes up no more water and (c) drying the dewatered gel, satd. with the org. liq. until no further wt. loss occurs on heating at 180 degrees C/10 Torr for 30 mins.; (2) mixing the resulting xerogel with solid, finely divided CR2O3 and heating at 100-300 degrees C/0.01-250 Torr until the xerogel has taken up 0.1-10 wt. % Cr2O3 (calculated as Cr), and (3) treating the prod. for 10-1000 min. at 40-1100 degrees C in a moisture-free gas stream contg. >10 vol. % O2. The catalyst give high yields and have high activity, and the resulting polymers have relatively narrow particle size distribution, low fines content and a sufficiently high melt index when made in the absence of mol. wt. regulators.

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