Patent US4547557A successfully refreshed from Google Patents.
US4547557A
Expired / Lapsed
US
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Silica-titania cogel from two-step hydrolysis
Assignee: Phillips Petroleum Co
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Filing: 1984-07-09
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Granted: 1985-10-15
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Expires: 2004-07-09
Abstract
Abstract A silica-titania cogel is produced in a two-step process wherein in the first step an alkyl polysilicate and/or a tetraalkyl silicate is partially hydrolyzed in an alkaline organic solvent using insufficient water to complete hydrolysis and thereafter a tetraalkyl titanate and an excess of water are added to complete the hydrolysis. The resulting product is as good or better than silica-titania cogels made by expensive prior art techniques and offers the advantage of not requiring washing step to remove alkali metal ions and thus also does not require an azeotrope drying step to remove water.
Inventors
- 👤 Max P. McDaniel
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-31 18:59
CPC Classifications
C; C08; C08F; C08F10/00
Claims Analysis
Total Claims: 28
Claim 1
Independent Claim
79 words
A method comprising: (a) partially hydrolyzing a silicate ester comprising at least one of an organopolysilicate and a tetraorganoxysilicate in an organic solvent under alkaline conditions using less than the stoichiometric amount of water required for complete hydrolysis; (b) thereafter combining the partially hydrolyzed product of (a) with a titanium tetraalkoxide; thereafter (c) adding sufficient water to complete the hydrolysis and produce a silica sol; and (d) combining said silica sol with sufficient base to form a silica-titania gel.
Claim 2
Independent Claim
79 words
A method comprising: (a) partially hydrolyzing a silicate ester comprising at least one of an organopolysilicate and a tetraorganoxysilicate in an organic solvent under alkaline conditions using less than the stoichiometric amount of water required for complete hydrolysis; (b) thereafter combining the partially hydrolyzed product of (a) with a titanium tetraalkoxide; thereafter (c) adding sufficient water to complete the hydrolysis and produce a silica sol; and (d) combining said silica sol with sufficient base to form a silica-titania gel.
Claim 3
Dependent Claim
13 words
A method according to claim 1 wherein said silicate ester is said organopolysilicate.
Claim 4
Dependent Claim
12 words
A method according to claim 2 wherein said organopolysilicate is ethyl polysilicate.
Claim 5
Dependent Claim
13 words
A method according to claim 1 wherein said silicate ester is said tetraorganoxysilicate.
Claim 6
Dependent Claim
11 words
A method according to claim 4 wherein said tetraorganoxysilicate is tetra-n-propoxysilane.
Claim 7
Dependent Claim
22 words
A method according to claim 1 wherein said organic solvent of (a) is rendered alkaline through the use of concentrated ammonium hydroxide.
Claim 8
Dependent Claim
13 words
A method according to claim 1 wherein said organic solvent is an alcohol.
Claim 9
Dependent Claim
17 words
A method according to claim 7 wherein said alcohol is a 3 to 4 carbon atom alcohol.
Claim 10
Dependent Claim
11 words
A method according to claim 8 wherein said alcohol is n-propanol.
Claim 11
Dependent Claim
26 words
A method according to claim 1 said titanium tetraalkoxide is of the formula Ti(OR') 4 where R' is a 1 to 6 carbon atom alkyl group.
Claim 12
Dependent Claim
12 words
A method according to claim 10 wherein said tetraalkoxide is tetraisopropyl titanate.
Claim 13
Dependent Claim
29 words
A method according to claim 10 wherein the total amount of water used is within the range of 1.5 to 5 times the stoichiometric amount needed for complete hydrolysis.
Claim 14
Dependent Claim
29 words
A method according to claim 1 wherein the total amount of water used is within the range of 1.5 to 5 times the stoichiometric amount needed for complete hydrolysis.
Claim 15
Dependent Claim
14 words
A method according to claim 1 wherein said base of (d) is ammonium hydroxide.
Claim 16
Dependent Claim
90 words
A method according to claim 14 wherein said organic solvent is n-propanol and is rendered alkaline in step (a) through the use of concentrated ammonium hydroxide, water is present in step (a) in an amount sufficient to give 15-60 mole percent of complete hydrolysis of the stoichiometric amount for complete hydrolysis wherein said titanium tetraalkoxide is tetraisopropyl titanate and wherein in step (c) said water is added in an amount wherein the total water is within the range of 1.5 to 5 times the stoichiometric amount needed for complete hydrolysis.
Claim 17
Dependent Claim
15 words
A method according to claim 15 wherein a chromium compound is present in said silica.
Claim 18
Dependent Claim
24 words
A method according to claim 16 wherein the chromium compound is introduced prior to forming said gel so as to form a silica-titania-chromium tergel.
Claim 19
Independent Claim
36 words
A method according to said 17 wherein said chromium compound is present in an amount sufficient to give 0.5 to 2 weight percent chromium based on the weight of said silica plus chromium compound after drying.
Claim 20
Independent Claim
36 words
A method according to said 17 wherein said chromium compound is present in an amount sufficient to give 0.5 to 2 weight percent chromium based on the weight of said silica plus chromium compound after drying.
Claim 21
Dependent Claim
13 words
A method according to claim 1 comprising in addition introducing a chromium compound.
Claim 22
Dependent Claim
9 words
A catalyst produced by the method of claim 19.
Claim 23
Dependent Claim
9 words
A catalyst produced by the method of claim 18.
Claim 24
Independent Claim
124 words
A method comprising: (a) partially hydrolyzing a silicate ester comprising at least one of an organopolysilicate and a tetraorganoxysilicate in an organic solvent under alkaline conditions using less than the stoichiometric amount of water required for complete hydrolysis; (b) thereafter combining the partially hydrolyzed product of (a) with a titanium tetraalkoxide; thereafter (c) adding sufficient water to complete the hydrolysis and produce a silica sol; thereafter (d) combining said silica sol with sufficient base to form a silica-titania gel; thereafter (e) drying said gel to form a xerogel, said xerogel also containing a chromium compound; (f) contacting at least one mono-1-olefin having 2 to 8 carbon atoms per molecule in a reaction zone under polymerization conditions with said xerogel; and (g) recovering a polymer.
Claim 25
Independent Claim
124 words
A method comprising: (a) partially hydrolyzing a silicate ester comprising at least one of an organopolysilicate and a tetraorganoxysilicate in an organic solvent under alkaline conditions using less than the stoichiometric amount of water required for complete hydrolysis; (b) thereafter combining the partially hydrolyzed product of (a) with a titanium tetraalkoxide; thereafter (c) adding sufficient water to complete the hydrolysis and produce a silica sol; thereafter (d) combining said silica sol with sufficient base to form a silica-titania gel; thereafter (e) drying said gel to form a xerogel, said xerogel also containing a chromium compound; (f) contacting at least one mono-1-olefin having 2 to 8 carbon atoms per molecule in a reaction zone under polymerization conditions with said xerogel; and (g) recovering a polymer.
Claim 26
Dependent Claim
19 words
A method according to claim 22 wherein said olefin is selected from ethylene, propylene, 1-butene, 1-pentene, 1-hexene and 1-octene.
Claim 27
Dependent Claim
11 words
A method according to claim 22 wherein said olefin comprises ethylene.
Claim 28
Dependent Claim
15 words
A method according to claim 22 wherein said polymerization is carried out under slurry conditions.
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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) | 1988-10-14 | 1989-04-15 | 1989-10-15 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1992-10-14 | 1993-04-15 | 1993-10-15 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1996-10-14 | 1997-04-15 | 1997-10-15 | $7700.00 | Window Closed / Lapsed |