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Method for preparing epsilon-caprolactone

A technology of caprolactone and cyclohexanone, which is applied in the field of producing ε-caprolactone, can solve problems such as the need to determine process conditions, achieve stable reaction temperature control, reduce the possibility of safety problems, and improve heat exchange capacity. Effect

Inactive Publication Date: 2012-07-18
CHINA PETROCHEMICAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And ZL91109988.3 is in the small test (that is, the laboratory stage), and there are still many problems to be determined in order to reach the industrial production stage.

Method used

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  • Method for preparing epsilon-caprolactone

Examples

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Embodiment 1

[0043] Preparation of peracetic acid solution

[0044] First put 100kg of perfluorosulfonic acid resin into a volume of 2m 3 In the reactor R1, 600kg acetic acid, 440kg ethyl acetate and 1kg tributyl phosphate are charged into R1 from the input pipe 2.

[0045] The reactor has a packed distillation column and a reflux condenser with a settling tank. Stir this solution at about 20kPa (absolute pressure), heat it to about 40°C with steam, and add a total amount of 220kg of 50% (by weight) hydrogen peroxide solution through pipeline 1 into R1. Control the temperature of R1 to about 40-45°C, return the organic phase in the heterogeneous azeotrope condensed by the low-temperature system in the reflux condenser to R1, and the water phase is continuously discharged from the pipe 3 and recovered by the organic solvent The unit recovers the organic solvent therein and refluxes to R1. Acetic acid and hydrogen peroxide have been reacted until the water phase is basically not separated...

Embodiment 2

[0054] Preparation of peroxypropionic acid solution

[0055] 100kg of strongly acidic cationic resin (D001 type, produced by Changsha Dayu Chemical Co., Ltd.) is loaded in advance with a volume of 2m 3 In the reactor R1, 600kg propionic acid, 400kg ethyl propionate and 1kg tributyl phosphate are charged into R1 from the input pipe 2. Stir this solution at about 10kPa (absolute pressure), heat it to about 50°C with steam, and add a total amount of 220kg of 50% (by weight) hydrogen peroxide solution through pipeline 1 into R1. Control the temperature of R1 at about 50-55°C, return the organic phase in the heterogeneous azeotrope condensed by the low-temperature system in the reflux condenser to R1, and the water phase is continuously discharged from the pipe 3 and recovered by the organic solvent The unit recovers the organic solvent therein and refluxes to R1. Propionic acid and hydrogen peroxide have been reacted until the water phase is basically not separated in the sedime...

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Abstract

The invention discloses a method for preparing epsilon-caprolactone, under the condition that solid acid catalyst exists, peroxide carboxylic acid solution is obtained by using hydrogen peroxide to oxidate organic carboxylic acid in a stirring reactor which has a fractionating column, the obtained peroxide carboxylic acid solution is reacted with cyclohexanone to obtain epsilon-caprolactone solution, then the high-purity epsilon-caprolactone is obtained after distillation and purification.

Description

technical field [0001] The present invention relates to a kind of method of producing ε-caprolactone, and this method is in the presence of solid acid catalyst, the peroxycarboxylic acid solution that the organic carboxylic acid in organic solvent is oxidized by hydrogen peroxide is added to cyclohexanone The reaction system is carried out to obtain ε-caprolactone solution, which is then separated in a rectification tower to realize the production of high-purity ε-caprolactone. Background technique [0002] In the existing technology, ε-caprolactone is prepared by oxidizing cyclohexanone with peroxycarboxylic acid, and the peroxycarboxylic acid used includes peroxyacetic acid and peroxypropionic acid. However, in the usual production method, various by-products such as adipic acid and 5-hexenoic acid are produced, and it is difficult to separate and obtain high-purity ε-caprolactone from the reaction product. [0003] A method is mentioned in Japanese Patent 150681 / 1982, Ja...

Claims

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Application Information

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IPC IPC(8): C07D313/04B01J31/06B01J31/08
Inventor 彭志斌罗际安黎树根刘洪武周小文邓琼李华明
Owner CHINA PETROCHEMICAL CORP
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