Process for continuous preparation of high purity epsilon-caprolactone

A technology of caprolactone and process, which is applied in the field of ε-caprolactone preparation, can solve the problems of inability to realize continuous industrial production, difficulty in separation and purification, and many side reactions, so as to achieve small fluctuations in process parameters and stable and controllable process flow , The effect of stable product quality

Inactive Publication Date: 2016-06-08
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In view of the defects in the preparation of ε-caprolactone in the prior art, such as many side reactions, low yield, difficulty in separation and purification, and inability to realize continuous industrial production, the purpose of the present invention is to provide a high-yield, continuous preparation of high-purity The process of ε-caprolactone has simple operation, mild reaction conditions, stable product quality, and meets industrial production requirements.

Method used

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  • Process for continuous preparation of high purity epsilon-caprolactone

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Experimental program
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Embodiment 1

[0030] Build the experimental device according to the accompanying drawings, wherein A1 and A2 are equipped with catalysts, B1, B2, C1, and C2 are packed towers, and the bottom of each tower is a 500mL three-necked flask, A1, A2, B1, and B2 are heated in a water bath, and C1 and C2 are used Electric heating mantle heating. Except that tap water is used for condensation at the top of the C2 tower, all other towers use low-temperature water for condensation.

[0031] First, wrap the perfluorosulfonic acid resin into a sandbag shape with glass fiber cloth, with an equivalent diameter of about 6-8 mm, and put it into the middle section of catalytic distillation reactors A1 and A2 with a diameter of 45 mm. The catalyst bed is about 600 mm high. The upper and lower sides of the distillation tower are equipped with 400mm long glass spring packing, the top of the tower is equipped with a condenser and a water separation and reflux device, and the bottom of the tower is heated by a wat...

Embodiment 2

[0038] The experimental device of embodiment 2 is exactly the same as embodiment 1, but raw material and proportioning are different, and the solvent that is added in each kettle in advance is changed into ethyl propionate, and the operating conditions of each tower are different.

[0039] Weigh 3000g propionic acid, 3000g ethyl propionate, 50% H 2 o 2 Add 1000g to a 10L bottle, shake well, and then use a pump to introduce from pipe 1 or 2 at a speed of about 280g / h. The pressure of A1 and A2 is controlled at about 15kPa, and the temperature of the kettle is about 60°C. Cyclohexanone is introduced into B1 at a rate of about 56g / h, the pressure of B1 and B2 is controlled at about 12kPa, the kettle temperature is about 55°C, the pressure of C1 and C2 is controlled at about 0.5kPa, and the kettle temperature is about 100-110°C.

[0040] Calculated from the product composition, H 2 o 2 The conversion rate is 99.7%, the conversion rate of cyclohexanone is 99.9%, the selectivity ...

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Abstract

The present invention discloses a process for continuous preparation of high purity epsilon-caprolactone, according to the process, a reaction and separation integrated apparatus is used for continuous preparation and separation of an organic peroxy acid and epsilon-caprolactone, wherein the reaction and separation integrated apparatus comprises a catalytic reaction rectifying column, a reaction rectifying column, a stirring reactor and a rectifying column which are in turn connected, and the process is as follows: an organic acid and hydrogen peroxide are introduced into the catalytic reaction rectifying column for oxidation reaction to separate water under catalysis of strong acid cation exchange resin, the organic peroxy acid produced by the reaction enters the reaction rectifying column, and a crude epsilon-caprolactone solution is obtained by oxidizing reaction of the organic peroxy acid and cyclohexanone entering form the middle part of the reaction rectifying column; and a high yield of the high purity epsilon-caprolactone can be continuously obtained by rectification separation of the crude epsilon-caprolactone solution. The process is simple in operation and mild in reaction conditions, and the product is stable in quality and can meet the industrial production.

Description

technical field [0001] The invention relates to a process for continuously preparing high-purity ε-caprolactone, which belongs to the field of ε-caprolactone preparation. 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 formed, and it is difficult to separate and obtain high-purity ε-caprolactone from the reaction product. [0003] In Japanese Patent 150681 / 1982, Japanese Patent 124781 / 1983 and Chinese Patent ZL91109988.3, ​​a method is mentioned, wherein a stable ε- Caprolactone, the corresponding carboxylic acid and hydrogen peroxide are used in the form of a "peroxycarboxylic acid crude solution" obtained by their reaction in the presence of a boric acid catalyst, and water is also continuous...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D313/04
Inventor 周小文刘洪武黎树根邓琼汤照龙
Owner CHINA PETROLEUM & CHEM CORP
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