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US4008176A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for the manufacture of a catalyst

Assignee: Hoechst AG
•
Filing: 1975-02-27
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Granted: 1977-02-15
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Expires: 1995-02-27
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Abstract

Abstract A catalyst of high activity and stereospecificity in α-olefin polymerization is obtained when titanium trichloride, prepared from titanium tetrachloride by reduction with an aluminum alkyl halide, is thermally treated, first with an ether in the presence of a cyclopolyene and the solid reaction product is then treated with an aluminum alkyl halide in the presence of a small amount of a cyclopolyene and/or an olefin. With the catalyst obtained high space-time yields of α-olefin polymers and copolymers can be produced.

Inventors

  • 👤 Kurt Rust
  • 👤 Erwin Schrott
  • 👤 Helmut Strametz
  • 👤 Hans-Jurgen Kablitz

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-31 18:52
CPC Classifications
C; C08; C08F; C08F10/00; Y; Y10; Y10S; Y10S526/00; Y10S526/903; Y10S526/907

Claims Analysis

Total Claims: 11
Claim 1
Independent Claim 206 words
In a process for the manufacture of a polymerization catalyst which comprises reacting titanium tetrachloride in an inert hydrocarbon solvent with an aluminum organic compound containing an aluminum dialkyl chloride at a temperature of from -20 to + 20° C in a molar proportion of aluminum dialkyl chloride to TiCl 4 of from 0.8 : 1 to 1.5:1, separating and washing the reaction product, subsequently thermally treating the TiCl 3 -containing reaction product suspended in the hydrocarbon solvent in the presence of an ether (said reaction product being component A), mixing with an aluminum dialkyl halide (component B), the improvement which comprises subjecting the suspension containing the solid washed reaction product, component A, to a thermal treatment at a temperature of from 40 to 150° C in the presence of a dialkyl ether in a molar ratio of TiCl 3 to ether of from 1:0.6 to 1:1.2 and also in the presence of a cyclopolyene in a molar ratio of TiCl 3 to cyclopolyene of from 1:0.001 to 1:0.15, and then effecting an after-treatment of component A with an aluminum alkyl halide at a temperature of from 0 to 60° C in a molar ratio of aluminum alkyl halide to TiCl 3 of from 0.8:1to 10:1.
Claim 2
Dependent Claim 206 words
In a process for the manufacture of a polymerization catalyst which comprises reacting titanium tetrachloride in an inert hydrocarbon solvent with an aluminum organic compound containing an aluminum dialkyl chloride at a temperature of from -20 to + 20° C in a molar proportion of aluminum dialkyl chloride to TiCl 4 of from 0.8 : 1 to 1.5:1, separating and washing the reaction product, subsequently thermally treating the TiCl 3 -containing reaction product suspended in the hydrocarbon solvent in the presence of an ether (said reaction product being component A), mixing with an aluminum dialkyl halide (component B), the improvement which comprises subjecting the suspension containing the solid washed reaction product, component A, to a thermal treatment at a temperature of from 40 to 150° C in the presence of a dialkyl ether in a molar ratio of TiCl 3 to ether of from 1:0.6 to 1:1.2 and also in the presence of a cyclopolyene in a molar ratio of TiCl 3 to cyclopolyene of from 1:0.001 to 1:0.15, and then effecting an after-treatment of component A with an aluminum alkyl halide at a temperature of from 0 to 60° C in a molar ratio of aluminum alkyl halide to TiCl 3 of from 0.8:1to 10:1.
Claim 3
Dependent Claim 25 words
A process according to claim 1, wherein said after-treatment is effected on component A without prior separation of the mother liquor from the thermal treatment.
Claim 4
Dependent Claim 60 words
A process according to claim 2, wherein said after-treatment is effected in the presence of a small amount of an unsaturated compound selected from the group consisting of cyclopolyene, an olefin, and mixtures thereof at a TiCl 3/ unsaturated compound molar ratio of from 1:0.001 to 1:1 for the cyclopolyenes present and from 1:1 to 1:100 for the olefins present.
Claim 5
Dependent Claim 21 words
A process according to claim 1 and wherein the after-treatment is carried out in the present of an aluminum dialkyl monohalide.
Claim 6
Dependent Claim 42 words
A process according to claim 1 wherein the after-treatment is carried out in the presence of an aluminum alkyl dihalide or sesquihalide and the catalyst component A is saparated and washed with an inert hydrocarbon solvent before being subjected to said after-treatment.
Claim 7
Dependent Claim 41 words
A process according to claim 3 and wherein the unsaturated compound is selected from the group consisting of cycloheptatriene-1,3,5; cyclooctatriene-1,3,5; cyclooctatetraene-1,3,5,7 and the alkyl and alkoxy substituted derivatives thereof in which the alkyl group contains from 1 to 4 carbon atoms.
Claim 8
Dependent Claim 25 words
A process according to claim 3 and wherein the unsaturated compound is a mono-olefin selected from the group consisting of ethylene, propylene, butene-1 and 4-methylpentene-1.
Claim 9
Dependent Claim 27 words
A process according to claim 1 further comprising as an additional catalyst component, C, a cyclopolyene as a stereoregulator, to be mixed with components A and B.
Claim 10
Dependent Claim 19 words
A process according to claim 3 further comprising as an additional catalyst component, C, a cyclopolyene as a stereoregulator.
Claim 11
Dependent Claim 9 words
A catalyst prepared by the process of claim 1.

References Cited (Backward Citations)

US3029231A Cited
US3058970A Cited
US2914515A Cited
US3394118A Cited
US3864278A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1980-02-15 1980-08-16 1981-02-15 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1984-02-15 1984-08-16 1985-02-15 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1988-02-15 1988-08-16 1989-02-15 $7700.00 Window Closed / Lapsed

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