Patent US4424320A successfully refreshed from Google Patents.
US4424320A
Expired / Lapsed
US
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Polymerization with a silica base catalyst having titanium incorporated through use of peroxide
Assignee: Phillips Petroleum Co
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Filing: 1982-09-27
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Granted: 1984-01-03
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Expires: 2002-09-27
Abstract
Abstract A silica composition having a high concentration of titanium is produced by solubilizing a titanium compound by combining same with a peroxide such as hydrogen peroxide. In a preferred embodiment, the peroxide is combined with the acid typically used in producing a gel from the combination of a silicate solution and an acid although the solubilizing component can also be used to simply impregnate particulate silica. The resulting composition has a high titanium content and an unusual pore structure makes it ideally suited as a catalyst base. When contemplated as a catalyst base, chromium can simply be coprecipitated with the silica and titanium. The resulting catalyst is ideally suited for the polymerization of olefins under slurry conditions.
Inventors
- 👤 Max P. McDaniel
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 20:01
CPC Classifications
B; B01; B01J; B01J37/00; B01J37/02; B01J37/03; B01J37/036; B01J21/00; B01J21/06; B01J21/08; B01J23/00; B01J23/16; B01J23/24; B01J23/26; C; C01; C01G; C01G23/00; C08; C08F; C08F110/00; C08F110/02
Claims Analysis
Total Claims: 20
Claim 1
Independent Claim
113 words
A polymerization process comprising: contacting at least one mono-1-olefin having 2 to 8 carbon atoms per molecule in a reaction zone under polymerization conditions with a catalyst produced by a process comprising: combining a titanium compound, a peroxide, and a mineral acid to form a first solution; thereafter combining said first solution with a second solution comprising an alkali metal silicate; allowing gellation to occur; aging for a time of at least one hour; washing to remove alkali metal ions; removing water to produce a xerogel; wherein said xerogel contains in addition a chromium compound; activating said xerogel containing said chromium in an oxygen-containing atmosphere at an elevated temperature; and recovering a polymer.
Claim 2
Dependent Claim
113 words
A polymerization process comprising: contacting at least one mono-1-olefin having 2 to 8 carbon atoms per molecule in a reaction zone under polymerization conditions with a catalyst produced by a process comprising: combining a titanium compound, a peroxide, and a mineral acid to form a first solution; thereafter combining said first solution with a second solution comprising an alkali metal silicate; allowing gellation to occur; aging for a time of at least one hour; washing to remove alkali metal ions; removing water to produce a xerogel; wherein said xerogel contains in addition a chromium compound; activating said xerogel containing said chromium in an oxygen-containing atmosphere at an elevated temperature; and recovering a polymer.
Claim 3
Dependent Claim
13 words
A polymerization process according to claim 1 wherein said olefin is predominantly ethylene.
Claim 4
Dependent Claim
16 words
A polymerization process according to claim 1 wherein said polymerization is carried out under slurry conditions.
Claim 5
Dependent Claim
24 words
A polymerization process according to claim 3 wherein said polymerization is carried out at a temperature within the range of 60° to 110° C.
Claim 6
Dependent Claim
38 words
A method according to claim 1 wherein a base is added after combination of said first and second solutions to effect said gellation, and wherein said water is removed by contact with a normally liquid volatile organic compound.
Claim 7
Dependent Claim
32 words
A method according to claim 5 wherein said base is ammonium hydroxide and said normally liquid volatile organic compound is one of ethyl acetate or a C 5 or C 6 alcohol.
Claim 8
Dependent Claim
31 words
A method according to claim 6 wherein said peroxide is hydrogen peroxide, said silicate is sodium silicate, and said mineral acid is sulfuric acid and said titanium compound is titanyl sulfate.
Claim 9
Dependent Claim
34 words
A method according to claim 7 wherein the resulting xerogel has a pore volume of 2 to 3 cc/g and an average pore diameter as measured by nitrogen absorption of greater than 600 angstroms.
Claim 10
Dependent Claim
30 words
A method according to claim 8 wherein the resulting xerogel has a weight percent titanium content within the range of 6 to 15 based on the weight of said xerogel.
Claim 11
Dependent Claim
30 words
A method according to claim 1 wherein said peroxide is hydrogen peroxide, said silicate is sodium silicate, said acid is sulfuric acid and wherein said titanium compound is titanyl sulfate.
Claim 12
Dependent Claim
23 words
A method according to claim 1 wherein said water is removed by contacting the washed gel with a normally liquid volatile organic compound.
Claim 13
Dependent Claim
23 words
A method according to claim 1 wherein said chromium compound is present in said first solution so as to produce a silica-titanium-chromium tergel.
Claim 14
Dependent Claim
83 words
A polymerization process comprising: contacting at least one mono-1-olefin having 2 to 8 carbon atoms per molecule in a reaction zone under polymerization conditions with a catalyst produced by a process comprising: combining a mineral acid, a titanium compound, and a peroxide to form a solution; combining said solution with silica to form a treated silica composition, said composition containing in addition a chromium compound; activating said thus treated silica composition in an oxygen-containing atmosphere at an elevated temperature; and recovering a polymer.
Claim 15
Dependent Claim
83 words
A polymerization process comprising: contacting at least one mono-1-olefin having 2 to 8 carbon atoms per molecule in a reaction zone under polymerization conditions with a catalyst produced by a process comprising: combining a mineral acid, a titanium compound, and a peroxide to form a solution; combining said solution with silica to form a treated silica composition, said composition containing in addition a chromium compound; activating said thus treated silica composition in an oxygen-containing atmosphere at an elevated temperature; and recovering a polymer.
Claim 16
Dependent Claim
12 words
A method according to claim 13 wherein said olefin is predominantly ethylene.
Claim 17
Dependent Claim
15 words
A method according to claim 13 wherein said polymerization is carried out under slurry conditions.
Claim 18
Dependent Claim
23 words
A method according to claim 15 wherein said polymerization is carried out at a temperature within the range of 60° to 110° C.
Claim 19
Dependent Claim
12 words
A method according to claim 13 wherein said silica is particulate silica.
Claim 20
Dependent Claim
80 words
A method according to claim 17 wherein said peroxide is hydrogen peroxide, said mineral acid is sulfuric acid, said titanium compound is titanyl sulfate and wherein titanium is present in an amount within the range of 6 to 15 weight percent based on the weight of said silica and said chromium compound is present in an amount sufficient to give chromium in an amount within the range of 0.5 to 5 weight percent based on the weight of said silica.
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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) | 1987-01-02 | 1987-07-04 | 1988-01-03 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1991-01-02 | 1991-07-04 | 1992-01-03 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1995-01-02 | 1995-07-04 | 1996-01-03 | $7700.00 | Window Closed / Lapsed |