US3976632A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Reactivation of organochromium olefin polymerization catalyst in presence of oxygen
Assignee: Phillips Petroleum Co
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Filing: 1974-12-04
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Granted: 1976-08-24
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Expires: 1994-12-04
Abstract
Abstract A particulate catalyst support containing titanium is heated to calcination temperature and thereafter impregnated with a π bonded organochromium compound. Thereafter the chromium-containing support is reactivated, at least a portion of the reactivation occurring in the presence of oxygen. In one embodiment at least 2 percent solvent is present as the catalyst is reactivated at approximately room temperature. In an alternate embodiment the support is calcined at a temperature within the range of 1450° to 1650°F. Such catalysts are particularly suitable for the production of high melt index polymer from at least one mono-1-olefin containing 2 to 8 carbon atoms per molecule.
Inventors
- 👤 Joseph A. Delap
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 07:59
CPC Classifications
C; C08; C08F; C08F10/00; Y; Y02; Y02P; Y02P20/00; Y02P20/50; Y02P20/584; Y10; Y10S; Y10S526/00; Y10S526/909
Claims Analysis
Total Claims: 33
Claim 1
Independent Claim
110 words
A process for producing a catalyst comprising: calcining a silica-containing particulate support containing titanium in air at a temperature within the range of 700° to 2000°F; thereafter impregnating the thus calcined titanium-containing support with a nonaqueous solution of a diarene organochromium compound having the following structure ##SPC2## wherein R is selected from the group consisting of hydrogen and alkyl radicals having from 1 to 6 carbon atoms; and thereafter treating the thus organochromium-impregnated support in the form of a free flowing powder containing at least 2 weight percent solvent, based on the weight of said impregnated support, with molecular oxygen at a temperature within the range of 40° to 150°F.
Claim 2
Dependent Claim
110 words
A process for producing a catalyst comprising: calcining a silica-containing particulate support containing titanium in air at a temperature within the range of 700° to 2000°F; thereafter impregnating the thus calcined titanium-containing support with a nonaqueous solution of a diarene organochromium compound having the following structure ##SPC2## wherein R is selected from the group consisting of hydrogen and alkyl radicals having from 1 to 6 carbon atoms; and thereafter treating the thus organochromium-impregnated support in the form of a free flowing powder containing at least 2 weight percent solvent, based on the weight of said impregnated support, with molecular oxygen at a temperature within the range of 40° to 150°F.
Claim 3
Dependent Claim
85 words
A method according to claim 1 wherein said organochromium compound is one of dibenzene chromium and dicumene chromium or mixtures thereof and is present in an amount within the range of 0.1 to 10 parts by weight per 100 parts by weight of said activated titanium-containing support, said titanium is present in an amount within the range of 1-8 weight percent based on the weight of said support and said solvent is present in an amount within the range of 15 to 50 weight percent.
Claim 4
Dependent Claim
16 words
A method according to claim 1 wherein said support is silica coprecipitated with a titanium compound.
Claim 5
Dependent Claim
21 words
A method according to claim 3 wherein said titanium compound coprecipitated with said silica is titanyl sulfate or titanium potassium oxalate.
Claim 6
Dependent Claim
21 words
A method according to claim 1 wherein said support is calcined at a temperature within the range of 1450° to 1650°F.
Claim 7
Dependent Claim
27 words
A method according to claim 1 wherein said oxygen is supplied in an amount sufficient to give 0.25 to 0.75 moles of oxygen per mole of chromium.
Claim 8
Dependent Claim
85 words
A method according to claim 6 wherein said calcination is carried out at a temperature within the range of 1450° to 1650°F, said organochromium compound is one of dibenzene chromium and dicumene chromium or mixtures thereof and is present in an amount within the range of 0.1 to 10 parts by weight per 100 parts by weight of said titanium-containing support, and said titanium is present in an amount within the range of 1 to 8 weight percent based on the weight of said support.
Claim 9
Dependent Claim
10 words
A catalyst produced according to the method of claim 7.
Claim 10
Dependent Claim
10 words
A catalyst produced according to the method of claim 1.
Claim 11
Dependent Claim
30 words
A polymerization process which comprises contacting at least one polymerizable mono-1-olefin having 2-8 carbon atoms per molecule under polymerization conditions with a catalyst produced by the method of claim 1.
Claim 12
Dependent Claim
11 words
A process according to claim 10 wherein said olefin is ethylene.
Claim 13
Dependent Claim
34 words
A method according to claim 10 wherein said contacting is carried out in a liquid diluent at a temperature such that at least a substantial part of polymer produced is insoluble in said diluent.
Claim 14
Dependent Claim
31 words
A method according to claim 10 wherein said contacting is carried out at a temperature within the range of 150° to 230°F and substantially all polymer produced is in particle form.
Claim 15
Dependent Claim
32 words
A method according to claim 10 wherein said contacting is carried out in a liquid diluent selected from paraffins or cycloparaffins or mixtures thereof having 3 to 12 carbon atoms per molecule.
Claim 16
Dependent Claim
22 words
A method according to claim 14 wherein said diluent is selected from the group consisting of propane, isobutane, cyclohexane, n-dodecane, and methylcyclohexane.
Claim 17
Dependent Claim
11 words
A method according to claim 15 wherein said diluent is isobutane.
Claim 18
Dependent Claim
61 words
A process for producing a catalyst comprising: calcining in air a silica-containing particulate support containing titanium at a temperature within the range of 1450 to 1650°F; thereafter impregnating the thus calcined titanium-containing support with a nonaqueous solution of a π bonded organochromium compound; and thereafter treating the thus organochromium-impregnated support with molecular oxygen at a temperature within the range of 40°-150°F.
Claim 19
Dependent Claim
61 words
A process for producing a catalyst comprising: calcining in air a silica-containing particulate support containing titanium at a temperature within the range of 1450 to 1650°F; thereafter impregnating the thus calcined titanium-containing support with a nonaqueous solution of a π bonded organochromium compound; and thereafter treating the thus organochromium-impregnated support with molecular oxygen at a temperature within the range of 40°-150°F.
Claim 20
Dependent Claim
39 words
A method according to claim 17 wherein said organochromium compound is a diarene chromium having the following structure ##SPC3## wherein R is selected from the group consisting of hydrogen and alkyl radicals having from 1 to 6 carbon atoms.
Claim 21
Dependent Claim
69 words
A method according to claim 17 wherein said organochromium compound is one of dibenzene chromium and dicumene chromium or mixtures thereof and is present in an amount within the range of 0.1 to 10 parts by weight per 100 parts by weight of said activated titanium-containing support, and said titanium is present in an amount within the range of 1-8 weight percent based on the weight of said support.
Claim 22
Dependent Claim
16 words
A method according to claim 17 wherein said support is silica coprecipitated with a titanium compound.
Claim 23
Dependent Claim
18 words
A method according to claim 17 wherein said treatment with oxygen is carried out at about room temperature.
Claim 24
Dependent Claim
27 words
A method according to claim 17 wherein said oxygen is supplied in an amount within the range of 0.25 to 0.75 moles per mole of said chromium.
Claim 25
Dependent Claim
6 words
A catalyst according to claim 22.
Claim 26
Dependent Claim
23 words
A method according to claim 17 wherein said oxygen is present in an amount greater than 1 mole per mole of said chromium.
Claim 27
Dependent Claim
9 words
A catalyst produced by the method of claim 24.
Claim 28
Dependent Claim
30 words
A polymerization process which comprises contacting at least one polymerizable mono-1-olefin having 2-8 carbon atoms per molecule under polymerization conditions with a catalyst produced by the method of claim 17.
Claim 29
Dependent Claim
11 words
A process according to claim 26 wherein said olefin is ethylene.
Claim 30
Dependent Claim
34 words
A method according to claim 26 wherein said contacting is carried out in a liquid diluent at a temperature such that at least a substantial part of polymer produced is insoluble in said diluent.
Claim 31
Dependent Claim
31 words
A method according to claim 26 wherein said contacting is carried out at a temperature within the range of 150° to 230°F and substantially all polymer produced is in particle form.
Claim 32
Dependent Claim
32 words
A method according to claim 26 wherein said contacting is carried out in a liquid diluent selected from paraffins or cycloparaffins or mixtures thereof having 3 to 12 carbon atoms per molecule.
Claim 33
Dependent Claim
22 words
A method according to claim 30 wherein said diluent is selected from the group consisting of propane, isobutane, cyclohexane, n-dodecane, and methylcyclohexane.
References Cited (Backward Citations)
US2825721A
Cited
US3014020A
Cited
US2912421A
Cited
US3013002A
Cited
US3349067A
Cited
US3326871A
Cited
US3709853A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1979-08-24 | 1980-02-23 | 1980-08-24 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1983-08-24 | 1984-02-23 | 1984-08-24 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1987-08-24 | 1988-02-23 | 1988-08-24 | $7700.00 | Window Closed / Lapsed |