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US4176089A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for the preparation of silica-titania and catalysts comprising the same

Assignee: ExxonMobil Technology and Engineering Co
•
Filing: 1978-08-03
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Granted: 1979-11-27
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Expires: 1998-08-03
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Abstract

Abstract High surface area, low bulk density silica-titania materials which are particularly effective as catalysts or catalyst supports are prepared by mixing a silicon alkoxide, a titanium alkoxide and an organic diluent, adding the resulting premixed alkoxides to a hydrolysis medium comprising water and a solvent to form a silica-titania precipitate, separating the silica-titania precipitate from the hydrolysis medium, drying and calcining the precipitate and recovering the resulting high surface area silica-titania product.

Inventors

  • 👤 Neville L. Cull

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-30 02:11
CPC Classifications
B; B01; B01J; B01J21/00; B01J21/06; B01J21/063; B01J29/00; B01J29/89; B01J37/00; B01J37/02; B01J37/03; B01J37/031; B01J37/033

Claims Analysis

Total Claims: 39
Claim 1
Independent Claim 53 words
A process for the preparation of a silica-titania composition which comprises the steps of: (a) mixing a silicon alkoxide, titanium alkoxide and an organic diluent, and (b) adding the resulting mixed alkoxides mixture to a hydrolysis mixture comprising water and an organic solvent to hydrolyze said mixed alkoxides and form a silica-titania precipitate.
Claim 2
Dependent Claim 53 words
A process for the preparation of a silica-titania composition which comprises the steps of: (a) mixing a silicon alkoxide, titanium alkoxide and an organic diluent, and (b) adding the resulting mixed alkoxides mixture to a hydrolysis mixture comprising water and an organic solvent to hydrolyze said mixed alkoxides and form a silica-titania precipitate.
Claim 3
Dependent Claim 35 words
The process of claim 1 wherein said silica-titania composition has a surface area ranging from about 100 to about 400 m 2 /g and a bulk density ranging from about 0.2 to about 0.60 g/cc.
Claim 4
Dependent Claim 35 words
The process of claim 1 wherein said silica-titania composition has a surface area ranging from about 200 to about 400 m 2 /g and a bulk density ranging from about 0.3 to about 0.6 g/cc.
Claim 5
Dependent Claim 19 words
The process of claim 1 wherein said silica-titania composition comprises from about 53 to about 91 weight percent titania.
Claim 6
Dependent Claim 12 words
The process of claim 1 wherein said organic diluent comprises an alcohol.
Claim 7
Dependent Claim 16 words
The process of claim 1 wherein said organic solvent in said hydrolysis mixture is an alcohol.
Claim 8
Dependent Claim 24 words
The process of claim 1 wherein the molar ratio of silicon alkoxide to titanium alkoxide in step (a) ranges from about 0.05:1 to 10:1.
Claim 9
Dependent Claim 21 words
The process of claim 1 wherein the molar ratio of silicon alkoxide to titanium alkoxide in step (a) is about 1:1.
Claim 10
Dependent Claim 24 words
The process of claim 1 wherein the hydrolysis of step (b) is conducted at a temperature ranging from about 25 to about 100° C.
Claim 11
Dependent Claim 26 words
The process of claim 1 wherein said mixed alkoxides mixture is added to said hydrolysis mixture at a rate of about 2 to about 6 cc/minute.
Claim 12
Dependent Claim 31 words
The process of claim 1 wherein said alkoxide constituent of said silicon alkoxide and of said titanium alkoxide is selected from the group consisting of C 1 to C 20 alkoxides.
Claim 13
Dependent Claim 26 words
The process of claim 1 wherein said alcohol diluent used in step (a) is selected from the groups consisting of C 1 to C 4 alcohols.
Claim 14
Dependent Claim 27 words
The process of claim 3 wherein said alcohol solvent used in said hydrolysis mixture is selected from the group consisting of C 1 to C 4 alcohols.
Claim 15
Dependent Claim 24 words
The process of claim 1 wherein said water is present in said hydrolysis mixture in an amount sufficient to hydrolyze theoretically completely said alkoxides.
Claim 16
Dependent Claim 33 words
The process of claim 1 wherein said organic solvent is present in said hydrolysis mixture in an amount ranging from about 50 to about 95 volume percent based on the total hydrolysis mixture.
Claim 17
Dependent Claim 22 words
The process of claim 1 wherein said silica-titania precipitate is separated from said hydrolysis mixture and wherein the separated precipitate is calcined.
Claim 18
Dependent Claim 21 words
The process of claim 16 wherein said calcination is conducted at a temperature ranging from about 400 to about 800° C.
Claim 19
Dependent Claim 16 words
The process of claim 16 wherein prior to said calcination step, said precipitate is air dried.
Claim 20
Dependent Claim 88 words
A process for the preparation of a catalyst which comprises compositing a metal or a compound of a metal selected from the group consisting of Groups IB, IIA, IIB, IVA, IVB, VIB, VIIB and VIII and mixtures thereof and a silica-titania composition prepared by steps which comprise: (a) mixing a silicon alkoxide, a titanium alkoxide and an organic diluent, and (b) adding the resulting mixed alkoxides mixture to a hydrolysis mixture comprising water and an organic solvent to hydrolyze said mixed alkoxides and to form a silica-titania precipitate.
Claim 21
Dependent Claim 88 words
A process for the preparation of a catalyst which comprises compositing a metal or a compound of a metal selected from the group consisting of Groups IB, IIA, IIB, IVA, IVB, VIB, VIIB and VIII and mixtures thereof and a silica-titania composition prepared by steps which comprise: (a) mixing a silicon alkoxide, a titanium alkoxide and an organic diluent, and (b) adding the resulting mixed alkoxides mixture to a hydrolysis mixture comprising water and an organic solvent to hydrolyze said mixed alkoxides and to form a silica-titania precipitate.
Claim 22
Dependent Claim 35 words
The process of claim 19 wherein said silica-titania composition has a surface area ranging from about 100 to about 400 m 2 /g and a bulk density ranging from about 0.2 to about 0.6 g/cc.
Claim 23
Dependent Claim 35 words
The process of claim 19 wherein said silica-titania composition has a surface area ranging from about 200 to about 400 m 2 /g and a bulk density ranging from about 0.3 to about 0.6 g/cc.
Claim 24
Dependent Claim 19 words
The process of claim 19 wherein said silica-titania composition comprises from about 53 to about 91 weight percent titania.
Claim 25
Dependent Claim 12 words
The process of claim 19 wherein said organic diluent comprises an alcohol.
Claim 26
Dependent Claim 16 words
The process of claim 19 wherein said organic solvent in said hydrolysis mixture is an alcohol.
Claim 27
Dependent Claim 24 words
The process of claim 19 wherein the molar ratio of silicon alkoxide to titanium alkoxide in step (a) ranges from about 0.05:1 to 10:1.
Claim 28
Dependent Claim 20 words
The process of claim 19 wherein the molar ratio of siliconalkoxide to titanium alkoxide in step (a) is about 1:1.
Claim 29
Dependent Claim 24 words
The process of claim 19 wherein the hydrolysis of step (b) is conducted at a temperature ranging from about 25° to about 100° C.
Claim 30
Dependent Claim 26 words
The process of claim 19 wherein said mixed alkoxides mixture is added to said hydrolysis mixture at a rate of about 2 to about 6 cc/minute.
Claim 31
Dependent Claim 31 words
The process of claim 19 wherein said alkoxide constituent of said silicon alkoxide and of said titanium alkoxide is selected from the group consisting of C 1 to C 20 alkoxides.
Claim 32
Dependent Claim 26 words
The process of claim 19 wherein said alcohol diluent used in step (a) is selected from the group consisting of C 1 to C 4 alcohols.
Claim 33
Dependent Claim 27 words
The process of claim 19 wherein said alcohol solvent used in said hydrolysis mixture is selected from the group consisting of C 1 to C 4 alcohols.
Claim 34
Dependent Claim 24 words
The process of claim 19 wherein said water is present in said hydrolysis mixture in an amount sufficient to hydrolyze theoretically completely said alkoxides.
Claim 35
Dependent Claim 33 words
The process of claim 19 wherein said organic solvent is present in said hydrolysis mixture in an amount ranging from about 50 to about 95 volume percent based on the total hydrolysis mixture.
Claim 36
Dependent Claim 22 words
The process of claim 19 wherein said silica-titania precipitate is separated from said hydrolysis mixture and wherein said separated precipitate is calcined.
Claim 37
Dependent Claim 21 words
The process of claim 34 wherein said calcination is conducted at a temperature ranging from about 400° to about 800° C.
Claim 38
Dependent Claim 16 words
The process of claim 34 wherein prior to said calcination step, said precipitate is air dried.
Claim 39
Dependent Claim 38 words
The process of claim 19 wherein said metal or compound of said metal composited with said silica-titania is selected from the group consisting of metals or compounds of copper, iron, chromium, vanadium, and the group VIII noble metals.

References Cited (Backward Citations)

US2378290A Cited
US2873246A Cited
US3639461A Cited
US3709833A Cited
US3983055A Cited
US3954670A Cited
US3993557A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1982-11-26 1983-05-28 1983-11-27 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1986-11-26 1987-05-28 1987-11-27 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1990-11-26 1991-05-28 1991-11-27 $7700.00 Window Closed / Lapsed

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