Preparation of a supported catalyst for the polymerization of .alpha.-olefins

• US 5,455,216 A
• Filed: 09/21/1993
• Issued: 10/03/1995
• Est. Priority Date: 09/23/1992
• Status: Expired due to Term

• Current Assignee: Basell Polyolefine GmbH (Lyondellbasell Industries NV)
• Original Assignee: BASF AG (BASF SE)
• Inventors: Goertz, Hans-Helmut, Funk, Guido, Lux, Martin, Saive, Roland, Mueller, Hans-Joachim, Konrad, Rainer, Follmer, Godofredo
• Primary Examiner(s): PAL, ASOKKUMAR
• Application Number:
  US08/124,047
• Time in Patent Office: 742 Days
• Field of Search: 502/256, 526/10.6, 526/130
• US Class Current: 502/256
• CPC Class Codes: C08F 10/00 Homopolymers and copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
• CPC Class Codes: C08F 4/02 Carriers therefor
• CPC Class Codes: C08F 4/025 Metal oxides
• CPC Class Codes: C08F 4/24 Oxides

Abstract

A process for the preparation of a supported catalyst for the polymerization of α-olefins, in which

(1) a silicon dioxide-containing support gel is prepared by

(1.1) introducing a sodium water glass or potassium water glass solution into a swirling stream of an aqueous mineral acid longitudinally and tangentially to the stream, spraying the resultant silica hydrosol in drop form into a gaseous medium and allowing it to solidify to form a hydrogel, and freeing the resultant hydrogel from salts by washing without prior ageing,

(1.2) drying the hydrogel resulting from (1.1) to form the support gel,

(2) the support gel (1) is charged with chromium trioxide or a chromium compound which can be converted into chromium trioxide under the conditions of process step (3), giving a chromium-containing support gel, and

(3) the chromium-containing support gel (2) is heated at from 400° to 1100° C. for from 10 to 1000 minutes in an anhydrous gas stream containing oxygen in a concentration of greater than 10% by volume,

comprises drying the hydrogel resulting from step (1.1) in step (1.2) within a time of not more than 60 seconds in a shaping, high-speed dryer at an inlet temperature of from 80° to 400° C.

Claims

1. A process for the preparation of a supported catalyst for the polymerization of α

-olefins, in which

(1) a silicon dioxide-containing support gel is prepared by

(1.1) introducing a sodium water glass or potassium water glass solution into a swirling stream of an aqueous mineral acid longitudinally and tangentially to the stream, spraying the resultant silica hydrosol in drop form into a gaseous medium and allowing it to solidify to form a hydrogel, and freeing the resultant hydrogel from salts by washing without prior ageing,

(1.2) drying the hydrogel resulting from (1.1) to form the support gel,

(2) the support gel (1) is charged with chromium trioxide or a chromium compound which can be converted into chromium trioxide under the conditions of process step (3), giving a chromium-containing support gel, and

(3) the chromium-containing support gel (2) is heated at from 400°

to 1100°

C. for from 10 to 1000 minutes in an anhydrous gas stream containing oxygen in a concentration of greater than 10% by volume,

which comprises drying the hydrogel resulting from step (1.1) in step (1.2) within a time of not more than 60 seconds in a shaping, high-speed dryer at an inlet temperature of from 80°

to 400°

C.

2. The process of claim 1, wherein the aqueous mineral acid used in step (1.1) contains aluminum ions.

3. The process of claim 1, wherein the hydrogel resulting from step (1.1) is, before the drying in step (1.2), subjected to a further step (1.1.1) in which a maximum of 95% by weight of the water present in the hydrogel is extracted.

4. The process of claim 3, wherein the extraction of the water present in the hydrogel which is carried out in step (1.1.1) is carried out with the aid of at least one C₁ - to C₄ -alcohol and/or C₃ - to C₅ -ketone.

5. The process of claim 1, wherein the support gel is classified (1.2.1) after it has been formed in step (1.2) and before it has been charged in step (2) with chromium trioxide or a chromium compound which can be converted into chromium trioxide.

6. The process of claim 1, wherein the support gel obtained in step (1.2) or (1.2.1) has a spherical shape with a diameter of from 10 to 300μ

m, a surface area of from 100 to 1000 m² /g and a pore volume of from 0.5 to 2.5 cm³ /g.

7. A process of claim 1, wherein the support gel obtainable from step (1) is additionally charged, in step (2), with inorganic, fluoride-containing compounds.

8. A supported catalyst for the polymerization of α

-olefins, prepared by the process of claim 1.