GB431398A - Improvements in the manufacture and production of unsaturated esters - Google Patents
Improvements in the manufacture and production of unsaturated estersInfo
- Publication number
- GB431398A GB431398A GB50734A GB50734A GB431398A GB 431398 A GB431398 A GB 431398A GB 50734 A GB50734 A GB 50734A GB 50734 A GB50734 A GB 50734A GB 431398 A GB431398 A GB 431398A
- Authority
- GB
- United Kingdom
- Prior art keywords
- column
- ester
- esters
- methyl
- kept
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/18—Preparation of carboxylic acid esters by conversion of a group containing nitrogen into an ester group
- C07C67/22—Preparation of carboxylic acid esters by conversion of a group containing nitrogen into an ester group from nitriles
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Esters of aliphatic unsaturated acids having a low boiling point are separated from the materials used in their preparation by distilling the respective mixtures, washing the vapours evolved with water, condensing the vaporous binary azeotropic mixture of ester and water so formed, and separating the ester therefrom. Suitable esters comprise methyl, ethyl, propyl, butyl, allyl, ethylene glycol and monoethyl glycol esters of acrylic acid; methyl, ethyl, allyl and butyl esters of angelic, tiglic and methylacrylic acids; and methyl and ethyl esters of crotonic acid. In an example, a vaporous mixture of acrylic acid methyl ester, excess methanol, acrylic acid and water flows from the top of an esterification column II, <PICT:0431398/IV/1> kept at a temperature of 125--150 DEG C., to the lower part of a washing column IV where it encounters a downward flow of hot water admitted through a pipe 7. The still is kept at a temperature of 96 DEG C., and the binary azeotropic mixture of boiling point 71 DEG C. leaves the column through a pipe 8, passes through a dephlegmator V kept at 60 DEG C., is condensed and flows through a cooler VI to a separating vessel VII. The upper layer of ester is removed and the lower layer returned continuously to the washing column. Impure methanol from the latter is re-distilled in a column XI for re-use in the process. The ester may be prepared continuously in the column II by reacting ethylene cyanhydrin with methanol in the presence of sulphuric acid. The columns may be constructed of iron, aluminium, copper or materials lined with zinc, tin, lead or copper.ALSO:<PICT:0431398/III/1> Esters of aliphatic unsaturated acids having a low boiling point are separated from the materials used in their preparation by distilling the respective mixtures, washing the vapours evolved with water, condensing the vaporous binary azeotropic mixture of ester and water so formed, and separating the ester therefrom. Suitable esters comprise methyl, ethyl, propyl, butyl, allyl, ethylene glycol and monoethyl glycol esters of acrylic acid; methyl, ethyl, allyl and butyl esters of angelic, tiglic, and methyl acrylic acids; and methyl and ethyl esters of crotonic acid. In an example, a vaporous mixture of acrylic acid methyl ester, excess methanol, acrylic acid and water flows from the top of an esterification column II, kept at a temperature of 125 DEG --150 DEG C., to the lower part of a washing column IV where it encounters a downward flow of hot water admitted through a pipe 7. The still is kept at a temperature of 96 DEG C., and the binary azeotropic mixture of boiling point 71 DEG C., leaves the column through a pipe 8, passes through a dephlegmator V kept at 60 DEG C., is condensed and flows through a cooler VI to a separating vessel VII. The upper layer of ester is removed and the lower layer returned continuously to the washing column. Impure methanol from the latter is re-distilled in a column XI for re-use in the process. The ester may be prepared continuously in the column II by reacting ethylene cyanhydrin with methanol in the presence of sulphuric acid. The columns may be constructed of iron, aluminium, copper or materials lined with zinc, tin, lead or copper.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB50734A GB431398A (en) | 1934-01-05 | 1934-01-05 | Improvements in the manufacture and production of unsaturated esters |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
GB50734A GB431398A (en) | 1934-01-05 | 1934-01-05 | Improvements in the manufacture and production of unsaturated esters |
Publications (1)
Publication Number | Publication Date |
---|---|
GB431398A true GB431398A (en) | 1935-07-05 |
Family
ID=9705558
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
GB50734A Expired GB431398A (en) | 1934-01-05 | 1934-01-05 | Improvements in the manufacture and production of unsaturated esters |
Country Status (1)
Country | Link |
---|---|
GB (1) | GB431398A (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1141987B (en) * | 1959-04-24 | 1963-01-03 | Knapsack Ag | Process for the continuous production of pure acrylic acid n-butyl ester from acrylic acid amide sulfate |
DE1156790B (en) * | 1959-05-09 | 1963-11-07 | Knapsack Ag | Process for the continuous production of pure acrylic acid methyl ester from acrylic acid amide sulfate |
DE1254622B (en) * | 1961-09-21 | 1967-11-23 | Knapsack Ag | Process for the separation of acrylic acid n-butyl ester from its mixtures |
DE1254623B (en) * | 1961-12-16 | 1967-11-23 | Knapsack Ag | Process for the separation of acrylic acid n-butyl ester from its mixture with n-butanol |
CN108484395A (en) * | 2018-05-02 | 2018-09-04 | 宜兴市恒兴精细化工有限公司 | A kind of device of continuity method synthesis isobutyl isobutyrate |
-
1934
- 1934-01-05 GB GB50734A patent/GB431398A/en not_active Expired
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1141987B (en) * | 1959-04-24 | 1963-01-03 | Knapsack Ag | Process for the continuous production of pure acrylic acid n-butyl ester from acrylic acid amide sulfate |
DE1156790B (en) * | 1959-05-09 | 1963-11-07 | Knapsack Ag | Process for the continuous production of pure acrylic acid methyl ester from acrylic acid amide sulfate |
DE1254622B (en) * | 1961-09-21 | 1967-11-23 | Knapsack Ag | Process for the separation of acrylic acid n-butyl ester from its mixtures |
DE1254623B (en) * | 1961-12-16 | 1967-11-23 | Knapsack Ag | Process for the separation of acrylic acid n-butyl ester from its mixture with n-butanol |
CN108484395A (en) * | 2018-05-02 | 2018-09-04 | 宜兴市恒兴精细化工有限公司 | A kind of device of continuity method synthesis isobutyl isobutyrate |
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