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US3977997A Expired / Lapsed US ⏱️ 0.0 years remaining

Manufacture of a modified titanium component for Ziegler-Natta catalysts

Assignee: BASF SE
•
Filing: 1974-12-16
•
Granted: 1976-08-31
•
Expires: 1994-12-16
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Abstract

Abstract A process for the manufacture of a modified titanium-containing component of a Ziegler-Natta catalyst for the polymerization of C 3-6 α-monoolefins, wherein a specific titanium-containing compound and a specific phosphorus-containing compound are dry-milled at a specific grinding acceleration in a vibratory ball mill. The characteristic feature of the process of the invention is that a mill is used which has a specific useful volume and the mill is initially charged with a specific amount of the titanium-containing compound, which is milled at a low temperature while the phosphorus-containing compound is gradually added, whereupon milling is continued while the temperature of the process material is gradually raised to a specific value and maintained at said value for a specific period of time, whereupon, if desired, milling is again continued at a lower temperature for a specific period of time. In this manner, modified titanium-containing components are obtained which in the polymerization process produce highly reproducible yields of polymer.

Inventors

  • 👤 Hans Schick
  • 👤 Heinz Mueller-Tamm
  • 👤 Peter Hennenberger

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-31 09:01
CPC Classifications
C; C08; C08F; C08F110/00; Y; Y10; Y10S; Y10S526/00; Y10S526/906

Claims Analysis

Total Claims: 5
Claim 1
Independent Claim 120 words
A process for the manufacture of a modified titanium-containing component of a Ziegler-Natta catalyst for the polymerization of C 3-6 α-monoolefins by dry-milling a. a titanium-containing compound of the general formula TiCl.sub.3 . nAlCl.sub.3 , wherein n denotes a number of from 0 to 0.7, and b. a phosphorus-containing compound of the general formula O.sub.m PX.sub.3, where m denotes 0 or 1, X denotes R, OR or NR 2 and R denotes alkyl, aryl, alkaryl or aralkyl, all of not more than 24 carbon atoms, in a vibratory ball mill at a grinding acceleration of from 30 to 80 m × sec - 2 and in a molar ratio of (a) : (b) of from 1:0.1 to 1:1, which comprises:
Claim 2
Dependent Claim 120 words
A process for the manufacture of a modified titanium-containing component of a Ziegler-Natta catalyst for the polymerization of C 3-6 α-monoolefins by dry-milling a. a titanium-containing compound of the general formula TiCl.sub.3 . nAlCl.sub.3 , wherein n denotes a number of from 0 to 0.7, and b. a phosphorus-containing compound of the general formula O.sub.m PX.sub.3, where m denotes 0 or 1, X denotes R, OR or NR 2 and R denotes alkyl, aryl, alkaryl or aralkyl, all of not more than 24 carbon atoms, in a vibratory ball mill at a grinding acceleration of from 30 to 80 m × sec - 2 and in a molar ratio of (a) : (b) of from 1:0.1 to 1:1, which comprises:
Claim 3
Dependent Claim 109 words
initially charging a mill which has a useful volume of from 2 to 200 liters, with from 0.1 to 120 kg of the titanium-containing compound (a), 2. milling the process material at a temperature of from -50° to -5°C while the amount of phosphorus-containing compound (b) corresponding to the desired molar ratio is added continuously or in small portions over a period of from 2 to 100 hours, 3. further milling the process material while the temperature thereof is raised to from 5° to 50°C over a period of from 0.1 to 5 hours and then held at this temperature over a period of from 1 to 100 hours.
Claim 4
Dependent Claim 109 words
initially charging a mill which has a useful volume of from 2 to 200 liters, with from 0.1 to 120 kg of the titanium-containing compound (a), 2. milling the process material at a temperature of from -50° to -5°C while the amount of phosphorus-containing compound (b) corresponding to the desired molar ratio is added continuously or in small portions over a period of from 2 to 100 hours, 3. further milling the process material while the temperature thereof is raised to from 5° to 50°C over a period of from 0.1 to 5 hours and then held at this temperature over a period of from 1 to 100 hours.
Claim 5
Dependent Claim 36 words
A process as set forth in claim 1 wherein the process material obtained from step (3) is further milled at a temperature of from -50° to -5°C over a period of from 1 to 30 minutes.

References Cited (Backward Citations)

US3032510A Cited
US3216987A Cited
US3389129A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1979-08-31 1980-03-01 1980-08-31 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1983-08-31 1984-03-01 1984-08-31 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1987-08-31 1988-03-01 1988-08-31 $7700.00 Window Closed / Lapsed

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