GB872188A - A process for the manufacture of the dimethyl esters of terephthalic and isophthalic acid - Google Patents
A process for the manufacture of the dimethyl esters of terephthalic and isophthalic acidInfo
- Publication number
- GB872188A GB872188A GB3529259A GB3529259A GB872188A GB 872188 A GB872188 A GB 872188A GB 3529259 A GB3529259 A GB 3529259A GB 3529259 A GB3529259 A GB 3529259A GB 872188 A GB872188 A GB 872188A
- Authority
- GB
- United Kingdom
- Prior art keywords
- column
- pressure
- methanol
- water
- temperature
- 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
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
- C07C67/54—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
In a process for the manufacture of dimethyl terephthalate and/or isophthalate by esterification of the appropriate acid(s) with excess methanol, the reaction-product is passed to a distillation column where it is fractionated under such conditions of temperature and pressure that methanol is withdrawn from the head of the column, and liquid ester and liquid water are withdrawn, separately or together, from the lower section of the column. The temperature in the lower part of the column should be higher than 140 DEG C., and the pressure should exceed 3.6 atm. If the ester and water are drawn off together, they are separated in a phase-separator maintained at a temperature higher than the melting-point of the ester and at a pressure higher than the vapour-pressure of water, corresponding to the temperature. The methanol obtained at the head of the column may contain less than 1% by weight of water, and is returned to the esterification reactor. In an example, a solution of terephthalic acid in an excess of methanol is passed at 250 DEG C. and a pressure of 85 atm. gauge through a tubular reactor divided by partitions into 10 compartments connected in series. The mixture leaves the tenth compartment after a residence time of two hours, and is introduced into a distillation column in which the pressure is 4 atm. absolute. Liquid ester is withdrawn from the bottom of the column at a temperature of 155 DEG C. Water is removed some distance above the bottom, and methanol is withdrawn from the top of the column. Dimethyl terephthalate is distilled off in vacuo from the liquid ester, until approximately equimolar quantities of dimethyl terephthalate and monomethyl terephthalate remain behind as residue. This residue is returned to the tubular reactor. The dimethyl terephthalate, obtained as distillate, may be purified by crystallization from methanol; and the mother-liquor may be passed to the reactor.ALSO:In a process for the manufacture of dimethyl terephthalate and/or isophthalate by esterification of the appropriate acid(s) with excess methanol, the reaction product is passed to a distillation column where it is fractionated under such conditions of temperature and pressure that methanol is withdrawn from the head of the column and liquid ester and liquid water are withdrawn, separately or together, from the lower section of the column. The temperature in the lower part of the column should be higher than 140 DEG C. and the pressure should exceed 3.6 atm. If the ester and water are drawn off together, they are separated in a decanter maintained at a temperature higher than the melting point of the ester and at a pressure higher than the vapour-pressure of water, corresponding to the temperature. The methanol obtained at the head of the column may contain less than 1% by weight of water, and is returned to the esterification reactor.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| NL232411A NL97771C (en) | 1958-10-20 | 1958-10-20 | process for the preparation of dialkyl esters of tender and isophthalic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| GB872188A true GB872188A (en) | 1961-07-05 |
Family
ID=38652915
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB3529259A Expired GB872188A (en) | 1958-10-20 | 1959-10-19 | A process for the manufacture of the dimethyl esters of terephthalic and isophthalic acid |
Country Status (5)
| Country | Link |
|---|---|
| BE (1) | BE583763A (en) |
| DE (1) | DE1117101B (en) |
| FR (1) | FR1240774A (en) |
| GB (1) | GB872188A (en) |
| NL (1) | NL97771C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5578173A (en) * | 1995-04-03 | 1996-11-26 | Eastman Kodak Company | Removal of dimethylterephthalate from a methanolysis vapor stream |
-
1958
- 1958-10-20 NL NL232411A patent/NL97771C/en active
-
1959
- 1959-10-19 BE BE583763A patent/BE583763A/en unknown
- 1959-10-19 GB GB3529259A patent/GB872188A/en not_active Expired
- 1959-10-19 FR FR807856A patent/FR1240774A/en not_active Expired
- 1959-10-19 DE DES65481A patent/DE1117101B/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5578173A (en) * | 1995-04-03 | 1996-11-26 | Eastman Kodak Company | Removal of dimethylterephthalate from a methanolysis vapor stream |
Also Published As
| Publication number | Publication date |
|---|---|
| BE583763A (en) | 1960-04-19 |
| DE1117101B (en) | 1961-11-16 |
| FR1240774A (en) | 1960-09-09 |
| NL97771C (en) | 1961-04-17 |
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