US3926848A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Process for increasing activity of heavy transition metal halide stereospecific catalysts
Assignee: ExxonMobil Technology and Engineering Co
•
Filing: 1973-04-19
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Granted: 1975-12-16
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Expires: 1993-04-19
Abstract
Abstract Ziegler-Natta transition metal catalysts, especially physicalenergy-activated cocrystallized metal halide catalysts such as TiCl3. 1/3 AlCl3 catalysts obtained with commercial ball milling techniques can be treated to be unexpectedly more active and more stereospecific. The process comprises heating the Ziegler-Natta catalysts, e.g. the physical-energy-activated, e.g. ball-milled, catalyst in certain inert solvents above the boiling point of the solvents for certain time intervals and at certain specified temperatures.
Inventors
- 👤 Harry Jan Wristers
- 👤 Herschel Claude Williams
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 14:25
CPC Classifications
C; C08; C08F; C08F10/00; C08F110/00; Y; Y10; Y10S; Y10S526/00; Y10S526/906
Claims Analysis
Total Claims: 11
Claim 1
Independent Claim
145 words
A PROCESS FOR INCREASING THE ACTIVITY OF COCRYSTALLIZED TICL3 1/3 ALCL3, OBTAINED BY ALUMINUM REDUCTION OF TICL4, WHICH IS AN ALREADY EFFECTIVE CATALYST WHICH COMPRISES THE SEQUENTIAL STEPS OF DRY BALL MILLING AND A HEAT SOAK TREATMENT TO REMOVE TRACE QUANTITIES OF MATERIALS DETRIMENTAL TO POLYMERIZATION SELECTED FROM THE GROUP CONSISTING OF: TICL4, ALCL3 AND COMBINATIONS THEREOF FROM ACTIVE CATALYST SITES OF SAID CATALYST BY CONTACTING SAID CATALYST WITH AN INERT AND SELECTIVE SOLVENT SELECTED FROM THE GROUP CONSISTING OF BENZENE AND HEPTANE HAVING A SOLVATION AFFINITY FOR SAID DETRIMENTAL MATERIALS FOR 1/2 TO 60 MINUTES AND AT A TEMPERATURE OF 100* TO 160*C SUFFICIENT TO RESULT IN A TREATED CATALYST WITH INCREASED ACTIVITY, DECREASED WAXY POLYMER AND INCREASED C7-INSOLUBLES WIGH RESPECT TO PROPYLENE POLYMERIZED WITH SAID TREATED CATALYST, AS COMPARED TO PROPYLENE POLYMERIZED WITH AN IDENTICAL CATALYST THAT IS UNTREATED BY THE PROCESS HEREOF.
Claim 2
Dependent Claim
145 words
A PROCESS FOR INCREASING THE ACTIVITY OF COCRYSTALLIZED TICL3 1/3 ALCL3, OBTAINED BY ALUMINUM REDUCTION OF TICL4, WHICH IS AN ALREADY EFFECTIVE CATALYST WHICH COMPRISES THE SEQUENTIAL STEPS OF DRY BALL MILLING AND A HEAT SOAK TREATMENT TO REMOVE TRACE QUANTITIES OF MATERIALS DETRIMENTAL TO POLYMERIZATION SELECTED FROM THE GROUP CONSISTING OF: TICL4, ALCL3 AND COMBINATIONS THEREOF FROM ACTIVE CATALYST SITES OF SAID CATALYST BY CONTACTING SAID CATALYST WITH AN INERT AND SELECTIVE SOLVENT SELECTED FROM THE GROUP CONSISTING OF BENZENE AND HEPTANE HAVING A SOLVATION AFFINITY FOR SAID DETRIMENTAL MATERIALS FOR 1/2 TO 60 MINUTES AND AT A TEMPERATURE OF 100* TO 160*C SUFFICIENT TO RESULT IN A TREATED CATALYST WITH INCREASED ACTIVITY, DECREASED WAXY POLYMER AND INCREASED C7-INSOLUBLES WIGH RESPECT TO PROPYLENE POLYMERIZED WITH SAID TREATED CATALYST, AS COMPARED TO PROPYLENE POLYMERIZED WITH AN IDENTICAL CATALYST THAT IS UNTREATED BY THE PROCESS HEREOF.
Claim 3
Dependent Claim
13 words
The process of claim 1 wherein said time is 10 to 35 minutes.
Claim 4
Dependent Claim
28 words
The process of claim 1 wherein said catalyst has been subjected to ball-milling sufficient to cause at least a three-fold increase in the surface area of said catalyst.
Claim 5
Dependent Claim
31 words
A process according to claim 1 wherein said process is carried out in a sealed vessel in order to utilize the high vapor pressures generated from said solvent at increased temperatures.
Claim 6
Dependent Claim
11 words
The process according to claim 3 wherein said solvent is benzene.
Claim 7
Dependent Claim
11 words
A process according to claim 1 wherein said solvent is heptane.
Claim 8
Dependent Claim
19 words
A process according to claim 1 wherein said heat soak is carried out both before and after said ball-milling.
Claim 9
Dependent Claim
31 words
A process according to claim 7 wherein said heat soaks are carried out in a sealed vessel in order to utilize the high pressures generated from said solvent at increased temperatures.
Claim 10
Dependent Claim
73 words
A process for further increasing the activity of a cocrystallized TiCl3. 1/3 AlCl3 which has been dry ball-milled to initially increase its surface area from about 3 to 50 fold which comprises heat soaking from about 3 to 15 wt. % of said catalyst in a benzene solvent at a temperature of 100* to 160* C from 10 minutes to 35 minutes in a closed container and separating said solvent from said catalyst.
Claim 11
Dependent Claim
73 words
A process for further increasing the activity of a cocrystallized TiCl3. 1/3 AlCl3 which has been dry ball-milled to initially increase its surface area from about 3 to 50 fold which comprises heat soaking from about 3 to 15 wt. % of said catalyst in a benzene solvent at a temperature of 100* to 160* C from 10 minutes to 35 minutes in a closed container and separating said solvent from said catalyst.
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USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1978-12-15 | 1979-06-16 | 1979-12-16 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1982-12-15 | 1983-06-16 | 1983-12-16 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1986-12-15 | 1987-06-16 | 1987-12-16 | $7700.00 | Window Closed / Lapsed |