US4246137A
Expired / Lapsed
US
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Method of preparing zirconia-silica xerogels, the xerogels, and xerogel catalysts
Assignee: Enron Chemical Co
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Filing: 1979-05-31
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Granted: 1981-01-20
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Expires: 1999-05-31
Abstract
Abstract A method of preparing large pore volume zirconia-silica catalyst supports, the resulting supports and a method of polymerizing olefins comprising contacting an olefin or mixture of olefins with a catalyst prepared with these supports. The supports are prepared by reacting a zirconium compound of the formula M 4 Zr(C 2 O 4 ) 4 .nH 2 O, where M is an alkali metal or ammonium ion and n equals 0 to 10, with a silicon compound of the type A 2 SiO 3 , where A is an alkali metal, in an aqueous solution at a pH equal to at least 11, then adding an acidic solution to a pH of about 5-9 to produce a hydrocogel. The hydrocogel is then aged and washed free of soluble by-products first with water, then with aqueous ammonium nitrate and again with water. The water is removed from the washed hydrocogel by azeotropic distillation or by washing with a water miscible solvent and then calcining the resulting xerocogel.
Inventors
- 👤 Robert A. Dombro
- 👤 William Kirch
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-03 11:47
CPC Classifications
B; B01; B01J; B01J21/00; B01J21/06; B01J21/066; B01J37/00; B01J37/02; B01J37/03; B01J37/036; C; C08; C08F; C08F10/00; C08F110/00; C08F110/02
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
210 words
The method of preparing large pore volume zirconia-silica useful as a catalyst support for a catalyst for polymerizing and copolymerizing olefins, comprising: a. reacting a zirconium compound of the formula M 4 Zr(C 2 O 4 ) 4 .nH 2 O, where M is an alkali metal or ammonium ion and n equals 0 to 10, with a silicon compound of the type A 2 SiO 3 , where A is an alkali metal, in an aqueous solution at a pH of at least 11 and then adding an acidic material to a pH of about 5-9, to produce a hydrocogel; b. aging said hydrocogel at a temperature between about ambient to 90° C. for at least one hour; c. washing said hydrocogel of b first with water, then with aqueous ammonium nitrate and again with water; d. removing water from the resulting washed hydrocogel of c to produce a xerocogel by azeotropic distillation by mixing with a compound capable of forming an azeotrope with water or by washing the hydrocogel with a water miscible solvent to produce a substantially water-free, large pore volume zirconia-silica catalyst support; and e. calcining the resulting xerocogel at a temperature of about 1000°-1800° F. preparatory to its use as an olefin polymerization catalyst support.
Claim 2
Independent Claim
210 words
The method of preparing large pore volume zirconia-silica useful as a catalyst support for a catalyst for polymerizing and copolymerizing olefins, comprising: a. reacting a zirconium compound of the formula M 4 Zr(C 2 O 4 ) 4 .nH 2 O, where M is an alkali metal or ammonium ion and n equals 0 to 10, with a silicon compound of the type A 2 SiO 3 , where A is an alkali metal, in an aqueous solution at a pH of at least 11 and then adding an acidic material to a pH of about 5-9, to produce a hydrocogel; b. aging said hydrocogel at a temperature between about ambient to 90° C. for at least one hour; c. washing said hydrocogel of b first with water, then with aqueous ammonium nitrate and again with water; d. removing water from the resulting washed hydrocogel of c to produce a xerocogel by azeotropic distillation by mixing with a compound capable of forming an azeotrope with water or by washing the hydrocogel with a water miscible solvent to produce a substantially water-free, large pore volume zirconia-silica catalyst support; and e. calcining the resulting xerocogel at a temperature of about 1000°-1800° F. preparatory to its use as an olefin polymerization catalyst support.
Claim 3
Dependent Claim
11 words
the method of claim 1 wherein M is an alkali metal.
Claim 4
Dependent Claim
11 words
The method of claim 1 wherein M is an ammonium ion.
Claim 5
Dependent Claim
21 words
The method of claim 1 wherein said acidic compound in said aqueous solution is sulfuric acid, hydrochloric acid or ammonium sulfate.
Claim 6
Dependent Claim
26 words
The method of claim 1 wherein water is removed from the washed hydrocogel by azeotropic distillation with a compound capable of forming an azeotrope with water.
Claim 7
Dependent Claim
18 words
The method of claim 1 wherein water is removed by washing the hydrocogel with a water miscible solvent.
Claim 8
Dependent Claim
10 words
A catalyst support prepared by the method of claim 1.
Claim 9
Dependent Claim
10 words
A catalyst support prepared by the method of claim 2.
Claim 10
Dependent Claim
10 words
A catalyst support prepared by the method of claim 3.
Claim 11
Dependent Claim
10 words
A catalyst support prepared by the method of claim 4
Claim 12
Dependent Claim
10 words
A catalyst support prepared by the method of claim 5.
Claim 13
Dependent Claim
10 words
A catalyst support prepared by the method of claim 6.
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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) | 1984-01-20 | 1984-07-21 | 1985-01-20 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1988-01-20 | 1988-07-21 | 1989-01-20 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1992-01-20 | 1992-07-21 | 1993-01-20 | $7700.00 | Window Closed / Lapsed |