US4018816A
Expired / Lapsed
US
⏱️ 0.0 years remaining
Preparation of methacrylates
Assignee: Mitsubishi Chemical Corp
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Filing: 1975-12-17
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Granted: 1977-04-19
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Expires: 1995-12-17
Abstract
Abstract A methacrylate is prepared by reacting methacrylic acid and an alcohol in vapor phase in the presence of a catalyst. The catalyst is a solid acid catalyst of silica-titania obtained by coprecipitating the same from an aqueous solution of a silicon and a titanium compound.
Inventors
- 👤 Takeru Onoda
- 👤 Masayuki Otake
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-30 02:17
CPC Classifications
B; B01; B01J; B01J21/00; B01J21/06; B01J21/063; B01J37/00; B01J37/02; B01J37/03; C; C07; C07C; C07C67/00; C07C67/08
Claims Analysis
Total Claims: 18
Claim 1
Independent Claim
134 words
In a process for the preparation of a methacrylate by the vapor phase reaction of methacrylic acid with an aliphatic alcohol having 1 to 4 carbon atoms and 1 to 2 hydroxyl groups in the proportion of 0.5 - 100 moles of the aliphatic alcohol per mole of methacrylic acid, at a temperature of 160° - 360° C in the presence of a catalyst, the improvement wherein the catalyst is a solid acid silica-titania catalyst which is prepared by dissolving a silicon compound and a titanium compound in an aqueous medium in such proportions that the ratio of silicon to titanium is 0.1 - 100, adjusting the pH of the resultant aqueous solution so as to coprecipitate the silicon and the titanium components and then drying and calcining the coprecipitate to form the catalyst.
Claim 2
Dependent Claim
134 words
In a process for the preparation of a methacrylate by the vapor phase reaction of methacrylic acid with an aliphatic alcohol having 1 to 4 carbon atoms and 1 to 2 hydroxyl groups in the proportion of 0.5 - 100 moles of the aliphatic alcohol per mole of methacrylic acid, at a temperature of 160° - 360° C in the presence of a catalyst, the improvement wherein the catalyst is a solid acid silica-titania catalyst which is prepared by dissolving a silicon compound and a titanium compound in an aqueous medium in such proportions that the ratio of silicon to titanium is 0.1 - 100, adjusting the pH of the resultant aqueous solution so as to coprecipitate the silicon and the titanium components and then drying and calcining the coprecipitate to form the catalyst.
Claim 3
Dependent Claim
16 words
The process as claimed in claim 1 wherein said aliphatic alcohol is methanol or ethylene glycol.
Claim 4
Dependent Claim
21 words
The process as claimed in claim 1 wherein said silicon compound is silicon tetrachloride, a silicate salt or a silicate ester.
Claim 5
Dependent Claim
14 words
The process as claimed in claim 3 wherein said silicate salt is sodium silicate.
Claim 6
Dependent Claim
14 words
The process as claimed in claim 3 wherein said silicate ester is ethyl orthosilicate.
Claim 7
Dependent Claim
20 words
The process as claimed in claim 1 wherein said titanium compound is titanium tetrachloride, titanium sulfate or a titanate ester.
Claim 8
Dependent Claim
36 words
The process as claimed in claim 1 wherein said aqueous medium is water, a solution of a mineral acid in water, a solution of an alkali in water or a solution of an alcohol in water.
Claim 9
Dependent Claim
31 words
The process as claimed in claim 1 wherein the pH of the aqueous solution is acidic and wherein a basic substance is added to said solution to effect said pH adjustment.
Claim 10
Dependent Claim
31 words
The process as claimed in claim 1 wherein the pH of the aqueous solution is basic and wherein an acidic substance is added to said solution to effect said pH adjustment.
Claim 11
Dependent Claim
20 words
The process as claimed in claim 1 wherein said coprecipitate is calcined at a temperature of 250 - 1200° C.
Claim 12
Dependent Claim
26 words
The process as claimed in claim 1 wherein a hydroxyl-bearing organic compound having a molecular weight of more than 300 is dispersed in said aqueous solution.
Claim 13
Dependent Claim
30 words
The process as claimed in claim 11 wherein said hydroxyl-bearing organic compound is added in an amount of 1 - 100 wt% on the basis of the resultant solid silica-titania.
Claim 14
Dependent Claim
31 words
The process as claimed in claim 11 wherein said hydroxyl-bearing organic compound is a polysaccharide or a derivative thereof, a polymer of an unsaturated alcohol, a polyacetal or a polyalkylene glycol.
Claim 15
Dependent Claim
15 words
The process as claimed in claim 13 wherein said polysaccharide is starch or crystalline cellulose.
Claim 16
Dependent Claim
14 words
The process as claimed in claim 13 wherein said polysaccharide derivative is methyl cellulose.
Claim 17
Dependent Claim
22 words
The process as claimed in claim 13 wherein said polyalkylene glycol is polyethylene glycol having a molecular weight of more than 400.
Claim 18
Dependent Claim
25 words
The process as claimed in claim 13 wherein said polymer of the unsaturated alcohol is polyvinyl alcohol having a molecular weight of more than 500.
References Cited (Backward Citations)
US3639461A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1980-04-18 | 1980-10-18 | 1981-04-19 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1984-04-18 | 1984-10-18 | 1985-04-19 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1988-04-18 | 1988-10-18 | 1989-04-19 | $7700.00 | Window Closed / Lapsed |