Patent US3857795A successfully refreshed from Google Patents.
US3857795A
Expired / Lapsed
US
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Preparation of ticl{11 {11 component of olefin polymerization catalyst
Assignee: Shell USA Inc
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Filing: 1972-12-18
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Granted: 1974-12-31
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Expires: 1992-12-18
Abstract
Abstract Titanium trichloride-containing compositions for use as catalyst component in stereoregular olefin polymerization are prepared by gradual addition of a solution of titanium tetrachloride to a solution of trialkyl aluminum in certain low-boiling inert diluents. The mixture is prepared and held at a temperature below about -90* C until addition is complete, is thereafter gradually warmed up at least to ambient temperature but not above 80* C and held until reduction of TiCl4 to TiCl5 is complete, and is then heated to an elevated temperature at which the TiCl3 is converted to the violet form. Refinements of this procedure include control of mixing and heating rates and post-treatment of the reaction product to produce catalyst components having various desired properties. According to one mode of the invention, titanium trichloridecontaining compositions can be obtained in particles which are larger and/or more clear and glassy and/or have a smoother surface than can be obtained when the mixing of titanium tetrachloride with aluminum trialkyl is carried out at conditions outside those specified. Used with dialkyl aluminum chloride in the polymerization of propylene, such compositions can produce excellent stereoregular polypropylene in the form of polymer particles of high bulk density which are substantially free of fines and hence non-dusting and exhibiting good powder flow. According to a second mode, titanium trichloride-containing compositions can be obtained in particles which, while still relatively dense, have a porous surface. Used with dialkyl aluminum chloride, these compositions are especially suitable for use in staged propylene polymerization followed by ethylenepropylene copolymerization to produce impact-improved polypropylene compositions.
Inventors
- 👤 Der Bend H Van
- 👤 W Sjardijn
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 05:47
CPC Classifications
C; C08; C08F; C08F10/00
Claims Analysis
Total Claims: 24
Claim 1
Independent Claim
61 words
THE METHOD OF PRODUCING A TITANIUM TRICHLORIDE COMPOSITION CONSISTING OF DENSE SMOOTH SURFACES PARTICLES ADAPTED FOR USE AS A CATALYST COMPONENT IN THE STEROROREGULAR POLYMERIZATION OF PROPYLENE TO A POLYMER POWDER CONTAINING NO MORE THAN 2% OF FINES OF LESS THAN 53 MICRON DIAMETER AND HAVING A FREELY SETTLED BULK DENSITY OF AT LEAST ABOUT 0.35 G/ML WHICH CONSISTS ESSENTIALLY OF:
Claim 2
Independent Claim
61 words
THE METHOD OF PRODUCING A TITANIUM TRICHLORIDE COMPOSITION CONSISTING OF DENSE SMOOTH SURFACES PARTICLES ADAPTED FOR USE AS A CATALYST COMPONENT IN THE STEROROREGULAR POLYMERIZATION OF PROPYLENE TO A POLYMER POWDER CONTAINING NO MORE THAN 2% OF FINES OF LESS THAN 53 MICRON DIAMETER AND HAVING A FREELY SETTLED BULK DENSITY OF AT LEAST ABOUT 0.35 G/ML WHICH CONSISTS ESSENTIALLY OF:
Claim 3
Dependent Claim
91 words
GRADUALLY OVER A PERIOD OF AT LEAST ONE HOUR, ADDING A SOLUTION OF TITANIUM TETRACHLORIDE IN ALKANE DILUENT TO AN AGITATED SOLUTION OF ALUMINUM TRIALKYLENE IN ALKANE DILUENT AT A MOLE RATIO OF TITANIUM TETRACHLORIDE TO ALUMINUM TRIALKYL IN THE RANGE FROM 3:0.9 TO 3-1.5, AT A MIXING TEMPERATURE T WITHIN THE RANGE FROM BELOW -90* TO -125*C WHEREIN THE FREEZING POINT OF SAID DILUENT IS BELOW (T15)*C THE FIRST 10 PERCENT OF SAID TITAIUM TETRACHLORIDE BEING ADDED GRADUALLY AT SUBSTANTIALLY UNIFORM RATE OVER A PERIOD OF AT LEAST 25 MINUTES;
Claim 4
Dependent Claim
91 words
GRADUALLY OVER A PERIOD OF AT LEAST ONE HOUR, ADDING A SOLUTION OF TITANIUM TETRACHLORIDE IN ALKANE DILUENT TO AN AGITATED SOLUTION OF ALUMINUM TRIALKYLENE IN ALKANE DILUENT AT A MOLE RATIO OF TITANIUM TETRACHLORIDE TO ALUMINUM TRIALKYL IN THE RANGE FROM 3:0.9 TO 3-1.5, AT A MIXING TEMPERATURE T WITHIN THE RANGE FROM BELOW -90* TO -125*C WHEREIN THE FREEZING POINT OF SAID DILUENT IS BELOW (T15)*C THE FIRST 10 PERCENT OF SAID TITAIUM TETRACHLORIDE BEING ADDED GRADUALLY AT SUBSTANTIALLY UNIFORM RATE OVER A PERIOD OF AT LEAST 25 MINUTES;
Claim 5
Dependent Claim
70 words
AFTER COMPLETION OF SAID ADDITION GRADUALLY RAISING THE TEMPERATURE OF THE MIXTURE TO AT LEAST ABOUT -30*C AT A RATE LESS THAN 1*C PER MINUTE AND MAINTAINING IT BELOW 80*C UNTIL THE REDUCTION OF TICL4 TO TICL3 IS SUBSTANTIALLY COMPLETE; CONVERTING SAID TICL3 TO THE VOILET FORM BY RAISING THE TEMPERATURE OF THE TICL3-CONTAINING COMPOMENT SLURRIED IN ALKANE DILUENT, TO A TEMPERATURE IN THE RANGE BETWEEN 100* AND 250*C; AND
Claim 6
Dependent Claim
70 words
AFTER COMPLETION OF SAID ADDITION GRADUALLY RAISING THE TEMPERATURE OF THE MIXTURE TO AT LEAST ABOUT -30*C AT A RATE LESS THAN 1*C PER MINUTE AND MAINTAINING IT BELOW 80*C UNTIL THE REDUCTION OF TICL4 TO TICL3 IS SUBSTANTIALLY COMPLETE; CONVERTING SAID TICL3 TO THE VOILET FORM BY RAISING THE TEMPERATURE OF THE TICL3-CONTAINING COMPOMENT SLURRIED IN ALKANE DILUENT, TO A TEMPERATURE IN THE RANGE BETWEEN 100* AND 250*C; AND
Claim 7
Dependent Claim
43 words
after completion of said addition gradually raising the temperature of the mixture to at least about -30* C at a rate less than 1* C per minute and maintaining it below 80* C until the reduction of TiCl4 to TiCl3 is substantially complete;
Claim 8
Dependent Claim
43 words
after completion of said addition gradually raising the temperature of the mixture to at least about -30* C at a rate less than 1* C per minute and maintaining it below 80* C until the reduction of TiCl4 to TiCl3 is substantially complete;
Claim 9
Dependent Claim
48 words
The method according to claim 1 wherein said aluminum trialkyl is aluminum triethyl, said diluent is n-butane, n-pentane or isopentane, or mixtures thereof, said ratio is in the range from 3:1.05 to 3:1.3 and said mixing temperature T is in the range from below -90* to -110* C.
Claim 10
Dependent Claim
48 words
after completion of said addition gradually raising the temperature of the mixture to at least about -30* C at a rate in the range from 2* to 5* C per minute and maintaining it below 80* C until the reduction of TiCl4 to TiCl3 therein is substantially complete;
Claim 11
Dependent Claim
48 words
after completion of said addition gradually raising the temperature of the mixture to at least about -30* C at a rate in the range from 2* to 5* C per minute and maintaining it below 80* C until the reduction of TiCl4 to TiCl3 therein is substantially complete;
Claim 12
Dependent Claim
32 words
converting said TiCl3 to the violet form by raising the temperature of the resulting TiCl3-containing component, slurried in alkane diluent, to a temperature in the range between 100* and 250* C and
Claim 13
Dependent Claim
32 words
converting said TiCl3 to the violet form by raising the temperature of the resulting TiCl3-containing component, slurried in alkane diluent, to a temperature in the range between 100* and 250* C and
Claim 14
Independent Claim
40 words
The method of producing a titanium trichloride composition consisting of dense particles having a porous surface, adapted for use as catalyst component in the staged, stereoregular polymerization of propylene and propylene-ethylene mixture to produce impact-improved copolymer which consists essentially of:
Claim 15
Independent Claim
40 words
The method of producing a titanium trichloride composition consisting of dense particles having a porous surface, adapted for use as catalyst component in the staged, stereoregular polymerization of propylene and propylene-ethylene mixture to produce impact-improved copolymer which consists essentially of:
Claim 16
Dependent Claim
31 words
converting said TiCl3 to the violet form by raising the temperature of the TiCl3-containing component slurried in alkane diluent, to a temperature in the range between 100* and 250* C; and
Claim 17
Dependent Claim
31 words
converting said TiCl3 to the violet form by raising the temperature of the TiCl3-containing component slurried in alkane diluent, to a temperature in the range between 100* and 250* C; and
Claim 18
Dependent Claim
10 words
cooling the resulting slurry to at least below 80* C.
Claim 19
Dependent Claim
10 words
cooling the resulting slurry to at least below 80* C.
Claim 20
Dependent Claim
9 words
COOLING THE RESULTING SLURRY TO AT LEAST BELOW 80*C.
Claim 21
Dependent Claim
9 words
COOLING THE RESULTING SLURRY TO AT LEAST BELOW 80*C.
Claim 22
Dependent Claim
10 words
cooling the resulting slurry to at least below 80* C.
Claim 23
Dependent Claim
10 words
cooling the resulting slurry to at least below 80* C.
Claim 24
Dependent Claim
48 words
The method according to claim 3 wherein said aluminum trialkyl is aluminum triethyl, said diluent is n-butane, n-pentane or isopentane, or mixtures thereof, said ratio is in the range from 3:1.05 to 3:1.3 and said mixing temperature T is in the range from below -90* to -110* C.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1977-12-30 | 1978-07-01 | 1978-12-31 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1981-12-30 | 1982-07-01 | 1982-12-31 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1985-12-30 | 1986-07-01 | 1986-12-31 | $7700.00 | Window Closed / Lapsed |