US4305841A
Expired / Lapsed
US
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Process for the manufacture of a catalyst
Assignee: Hoechst AG
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Filing: 1979-09-12
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Granted: 1981-12-15
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Expires: 1999-09-12
Abstract
Abstract A catalyst for the polymerization of 1-olefins is prepared by successively applying a chromate ester and a titanium ester to a carrier containing silicon dioxide, in the absence of an unsaturated polymerizable hydrocarbon, and activating with an aluminum-organic compound. In the manufacture of the catalyst no washing liquids are obtained from which metal compounds would have to be separated. In the presence of hydrogen the catalyst gives a high yield of polymers with broad molecular weight distribution and a small content of high molecular constituents. The films made therefrom are practically free from specks.
Inventors
- 👤 Klemens Gutweiler
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 15:12
CPC Classifications
C; C08; C08F; C08F10/00
Claims Analysis
Total Claims: 30
Claim 1
Independent Claim
241 words
A process for producing a catalyst, which comprises reacting, in the absence of water and in an inert diluent and under inert gas, a chromate ester of the formula (RO).sub.2 CrO.sub.2, wherein R is a tertiary alkyl or aralkyl of from 4 to 24 carbon atoms, with an anhydrous carrier selected from the group consisting of oxides of silicon, oxides of aluminum and mixtures thereof, the chromate ester being reacted with the carrier at a temperature of from 0° to 40° C. for a period of from 1 to 360 minutes in a proportion of from 1 to 40 millimols of chromate ester per 100 g of carrier; treating the reaction product thereof, which is suspended in said inert diluent, at a temperature of from 0° to 100° C. for a period of from 0.5 to 80 hours, in the absence of an unsaturated polymerizable hydrocarbon and under inert gas, with a titanium compound of the formula ##STR2## wherein R 4 , R 4' , R 4" and R 4'" are the same or not all the same and each is a linear or branched alkyl group of from 1 to 12 carbon atoms, the amount of said titanium compound being such that the proportion of Cr to Ti is of from 1:1 to 1:10; and mixing said treated reaction product, either while said product is still in suspension or after removal of the diluent and drying, with an aluminum-organic compound.
Claim 2
Dependent Claim
241 words
A process for producing a catalyst, which comprises reacting, in the absence of water and in an inert diluent and under inert gas, a chromate ester of the formula (RO).sub.2 CrO.sub.2, wherein R is a tertiary alkyl or aralkyl of from 4 to 24 carbon atoms, with an anhydrous carrier selected from the group consisting of oxides of silicon, oxides of aluminum and mixtures thereof, the chromate ester being reacted with the carrier at a temperature of from 0° to 40° C. for a period of from 1 to 360 minutes in a proportion of from 1 to 40 millimols of chromate ester per 100 g of carrier; treating the reaction product thereof, which is suspended in said inert diluent, at a temperature of from 0° to 100° C. for a period of from 0.5 to 80 hours, in the absence of an unsaturated polymerizable hydrocarbon and under inert gas, with a titanium compound of the formula ##STR2## wherein R 4 , R 4' , R 4" and R 4'" are the same or not all the same and each is a linear or branched alkyl group of from 1 to 12 carbon atoms, the amount of said titanium compound being such that the proportion of Cr to Ti is of from 1:1 to 1:10; and mixing said treated reaction product, either while said product is still in suspension or after removal of the diluent and drying, with an aluminum-organic compound.
Claim 3
Dependent Claim
257 words
A process for producing a catalyst, which comprises reacting, in the absence of water and in an inert diluent and under inert gas, a chromate ester of the formula (RO).sub.2 CrO.sub.2, wherein R is tertiary alkyl or aralkyl of from 4 to 24 carbon atoms, with a carrier previously dried at a temperature of from 120° to 800° C. to remove all water adsorbed thereon and selected from the group consisting of oxides of silicon, oxides of aluminum and mixtures thereof, the chromate ester being reacted with the carrier at a temperature of from 0° to 40° C. for a period of from 1 to 360 minutes in a proportion of from 1 to 40 millimols of chromate ester per 100 g of carrier; treating the reaction product thereof, which is suspended in said inert diluent, at a temperature of from 0° to 100° C. for a period of from 0.5 to 80 hours, in the absence of an unsaturated polymerizable hydrocarbon and under inert gas, with a titanium compound of the formula ##STR3## wherein R 4 , R 4' , R 4" and R 4'" are the same or not all the same and each is a linear or branched alkyl grop of from 1 to 12 carbon atoms, the amount of said titanium compound being such that the proportion of Cr to Ti is of from 1:1 to 1:10; and mixing said treated reaction product, either while said product is still in suspension or after removal of the diluent and drying, with an aluminum-organic compound.
Claim 4
Dependent Claim
257 words
A process for producing a catalyst, which comprises reacting, in the absence of water and in an inert diluent and under inert gas, a chromate ester of the formula (RO).sub.2 CrO.sub.2, wherein R is tertiary alkyl or aralkyl of from 4 to 24 carbon atoms, with a carrier previously dried at a temperature of from 120° to 800° C. to remove all water adsorbed thereon and selected from the group consisting of oxides of silicon, oxides of aluminum and mixtures thereof, the chromate ester being reacted with the carrier at a temperature of from 0° to 40° C. for a period of from 1 to 360 minutes in a proportion of from 1 to 40 millimols of chromate ester per 100 g of carrier; treating the reaction product thereof, which is suspended in said inert diluent, at a temperature of from 0° to 100° C. for a period of from 0.5 to 80 hours, in the absence of an unsaturated polymerizable hydrocarbon and under inert gas, with a titanium compound of the formula ##STR3## wherein R 4 , R 4' , R 4" and R 4'" are the same or not all the same and each is a linear or branched alkyl grop of from 1 to 12 carbon atoms, the amount of said titanium compound being such that the proportion of Cr to Ti is of from 1:1 to 1:10; and mixing said treated reaction product, either while said product is still in suspension or after removal of the diluent and drying, with an aluminum-organic compound.
Claim 5
Dependent Claim
11 words
A catalyst produced by a process as defined in claim 1.
Claim 6
Dependent Claim
11 words
A catalyst produced by a process as defined in claim 2.
Claim 7
Dependent Claim
21 words
A process as defined in claim 1, wherein R is tertiary alkyl or aralkyl of from 4 to 10 carbon atoms.
Claim 8
Dependent Claim
11 words
A catalyst produced by a process as defined in claim 5.
Claim 9
Dependent Claim
64 words
A process as defined in claim 1, wherein said carrier has a specific surface of from 50 to 1000 m 2 /g, a pore volume in the range of from 0.2 to 3 ml/g, a particle size in the range of from 1 to 500 μm, and a hydroxyl group content in the range of from 0.5 to 50 millimols per gram of carrier.
Claim 10
Dependent Claim
11 words
A catalyst produced by a process as defined in claim 7.
Claim 11
Dependent Claim
65 words
A process as defined in claim 7, wherein said specific surface is of from 100 to 800 m 2 /g, said pore volume is in the range of from 0.4 to 3 ml/g, said particle size is in the range of from 10 to 200 μm and the hydroxyl group content is in the range of from 1 to 20 millimols per gram of carrier.
Claim 12
Dependent Claim
11 words
A catalyst produced by a process as defined in claim 9.
Claim 13
Dependent Claim
64 words
A process as defined in claim 9, wherein the carrier has a specific surface of from 150 to 650 m 2 /g, a pore volume in the range of from 0.6 to 2.7 ml/g, a particle size in the range of from 20 to 100 μm and a hydroxyl group content in the range of from 1.5 to 10 millimols per gram of carrier.
Claim 14
Dependent Claim
11 words
A catalyst produced by a process as defined in claim 11.
Claim 15
Dependent Claim
35 words
A process as defined in claim 1, wherein the temperature is of from 15° to 25° C. and the proportion is of from 2 to 25 millimols of chromate ester per 100 g of carrier.
Claim 16
Dependent Claim
11 words
A catalyst produced by a process as defined in claim 13.
Claim 17
Dependent Claim
41 words
A process as defined in claim 1, wherein R 4 ,R 4' , R " and R '" are the same or not all the same and each is a linear or branched alkyl of from 3 to 8 carbon atoms.
Claim 18
Dependent Claim
11 words
A catalyst produced by a process as defined in claim 15.
Claim 19
Dependent Claim
29 words
A process as defined in claim 1, wherein the titanium compound is ethyl titanate, i-propyl titanate, n-butyl titanate, i-butyl titanate, tert.-butyl titanate, amyl titanate, octyl titanate or dodecyl titanate.
Claim 20
Dependent Claim
11 words
A catalyst produced by a process as defined in claim 17.
Claim 21
Dependent Claim
41 words
A process as defined in claim 1, wherein the reaction temperature is of from 20° to 70° C., the reaction time is of from 0.5 to 24 hours and the proportion of chromium to titanium is of from 1:1 to 1:6.
Claim 22
Dependent Claim
11 words
A catalyst produced by a process as defined in claim 19.
Claim 23
Dependent Claim
125 words
A process as defined in claim 1, wherein the aluminum organic compound is a compound of the formula AlR 5 3 or AlR 5 2 H, R 5 being hydrocarbon of from 1 to 16 carbon atoms; a polymeric aluminum organic compound consisting of monomers of the formula ##STR4## wherein R 6 is alkyl of from 2 to 12 carbon atoms; or a compound of the formula R 7 2 AlCl or R 7 3 Al 2 Cl 3 wherein R 7 is alkyl of from 1 to 16 carbon atoms or a reaction product of an aluminum trialkyl or aluminum dialkyl hydride, each alkyl of which is of from 1 to 16 carbon atoms, with a diene of from 4 to 20 carbon atoms.
Claim 24
Dependent Claim
11 words
A catalyst produced by a process as defined in claim 21.
Claim 25
Dependent Claim
42 words
A process as defined in claim 21, wherein R 5 is alkyl of from 1 to 16 carbon atoms, R 6 is alkyl of from 2 to 6 carbon atoms and R 7 is alkyl of from 2 to 4 carbon atoms.
Claim 26
Dependent Claim
11 words
A catalyst produced by a process as defined in claim 23.
Claim 27
Dependent Claim
38 words
A process as defined in claim 1, wherein the aluminum organic compound is mixed with said titanium compound-treated reaction product in a proportion such that the ratio of chromium to the aluminum organic compound is 0.2:1 to 0.1:1.
Claim 28
Dependent Claim
11 words
A catalyst produced by a process as defined in claim 25.
Claim 29
Dependent Claim
16 words
A process as defined in claim 25, wherein the ratio is of from 0.05:1 to 0.01:1.
Claim 30
Dependent Claim
11 words
A catalyst produced by a process as defined in claim 27.
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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) | 1984-12-14 | 1985-06-15 | 1985-12-15 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-12-14 | 1989-06-15 | 1989-12-15 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-12-14 | 1993-06-15 | 1993-12-15 | $7700.00 | Window Closed / Lapsed |