GB757742A - Purifying isopropyl chloroformate by distillation - Google Patents
Purifying isopropyl chloroformate by distillationInfo
- Publication number
- GB757742A GB757742A GB3305/54A GB330554A GB757742A GB 757742 A GB757742 A GB 757742A GB 3305/54 A GB3305/54 A GB 3305/54A GB 330554 A GB330554 A GB 330554A GB 757742 A GB757742 A GB 757742A
- Authority
- GB
- United Kingdom
- Prior art keywords
- column
- isopropyl chloroformate
- phosgene
- cooled
- pool
- 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
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/08—Purification; Separation; Stabilisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C69/00—Esters of carboxylic acids; Esters of carbonic or haloformic acids
- C07C69/96—Esters of carbonic or haloformic acids
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
<PICT:0757742/III/1> Phosgene is separated from isopropyl chloroformate prepared by the action of phosgene on isopropyl alcohol by feeding the reaction product into the upper section of a fractionating column up which is flowing a vapour stream from a boiling pool of isopropyl chloroformate contained in the base of the column or in a reboiler connected to the base thereof: some of the liquid is continuously withdrawn from this pool and is cooled to below 40 DEG C., the operations being so conducted that the withdrawn isopropyl chloroformate is cooled within 15 minutes of its introduction into the column. Vapours comprising phosgene and isopropyl chloroformate are withdrawn from the head of the column, and are cooled to a temperature between 10 DEG and 30 DEG C. whereupn isopropyl chloroformate condenses leaving purified phosgene in the gaseous phase. The condensate is returned to the column as reflux. A mixture of phosgene and isopropyl chloroformate is fed through line 4 into the top of column 1 which is about 10 feet high and has a diameter of 12 inches. The column, which is packed with 1/2 -inch ceramic Berl saddles, is heated at the base by steamcoil 3 which maintains the pool of isopropyl chloroformate in still-pot 2 boiling at a temperature between 95 DEG and 99 DEG C. The vapours reaching the head of the column are passed via line 6 to watercooled condenser 5 which is maintained at about 25 DEG C.; and the resulting liquid and gas phases are separated in separator 7. Gaseous phosgene is removed from the system through pipe 8. The condensate is added to the feed at 9 and returned to the column. Isopropyl chloroformate of 98 per cent purity is removed from still-pot 2 by a constant level take-off pipe 10, and is cooled in heat-exchanger 11, and withdrawn to storage. The rate of feed, of boiling, and of reflux return are adjusted so that isopropyl chloroformate remains in the system for about 5 1/2 minutes prior to being cooled in heat-exchanger 11. Of this time, the delay is 4 minutes in the pool in still-pot 2.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US757742XA | 1953-02-25 | 1953-02-25 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| GB757742A true GB757742A (en) | 1956-09-26 |
Family
ID=22127892
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB3305/54A Expired GB757742A (en) | 1953-02-25 | 1954-02-04 | Purifying isopropyl chloroformate by distillation |
Country Status (1)
| Country | Link |
|---|---|
| GB (1) | GB757742A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115894244A (en) * | 2022-09-26 | 2023-04-04 | 湖南化工研究院有限公司 | Continuous synthesis method of isopropyl chloride |
-
1954
- 1954-02-04 GB GB3305/54A patent/GB757742A/en not_active Expired
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115894244A (en) * | 2022-09-26 | 2023-04-04 | 湖南化工研究院有限公司 | Continuous synthesis method of isopropyl chloride |
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