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Synthesis device for 6-carbonyl-8-chloroethylcaprylate and method for synthesizing 6-carbonyl-8-chloroethylcaprylate by using device

A technology for ethyl chlorooctanoate and a synthesis device, which is applied in chemical instruments and methods, preparation of carboxylic acid esters, preparation of organic compounds, etc., can solve problems such as non-conformance, unstable product quality, low production efficiency, etc. rate effect

Active Publication Date: 2020-05-22
SUZHOU FUSHILAI PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, the main method of producing 6-carbonyl-8-chlorooctanoic acid ethyl ester is: using 6-chloro-6-oxohexanoic acid ethyl ester as The raw material is aluminum trichloride as a catalyst, and ethylene gas is introduced to carry out the alkylation reaction. Since the reaction is carried out in the gas-liquid two-phase, and the reaction process requires 2 times the excess of ethylene, resulting in low production efficiency and unstable product quality And excessive ethylene has many problems of great potential safety hazards, which does not meet the needs of modern industrial production

Method used

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  • Synthesis device for 6-carbonyl-8-chloroethylcaprylate and method for synthesizing 6-carbonyl-8-chloroethylcaprylate by using device
  • Synthesis device for 6-carbonyl-8-chloroethylcaprylate and method for synthesizing 6-carbonyl-8-chloroethylcaprylate by using device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] use figure 1 The steps of the method for the synthetic 6-carbonyl-8-chlorooctanoic acid ethyl ester synthetic device of shown 6-carbonyl-8-chlorooctanoic acid ethyl ester are as follows:

[0028] A) To prepare the complexing solution, first pass ethyl 6-chloro-6-oxohexanoate and ethylene dichloride as the reaction raw materials through their respective pipelines, that is, pass through the 6-chloro-6-oxo with valve The ethyl hexanoate delivery pipeline and the dichloroethane delivery pipeline that is also equipped with a valve are fed from the complexing solution preparation tank 11 in the upper part of the complexing solution preparation tank 11 of the structural system of the complexing solution supply mechanism 1. Introduce in the complexing liquid preparation still 11, by figure 1 As shown, the aforementioned complexing solution preparation kettle 11 has two sets of identical structures, so as to fully ensure the uninterrupted delivery of 6-chloro-6-oxoethyl hexanoa...

Embodiment 2

[0032] Only change the mol ratio of 6-chloro-6-oxohexanoic acid ethyl ester, anhydrous aluminum chloride and ethylene dichloride described in step A) into 1: 1.6: 10, the flow rate of complexing liquid Change 11000L / min into 11000L / min, change the pressure of damping buffer 14 into 0.7MPa; Only change the pressure of the ethylene gas in step B) into 0.8MPa, change the pressure of damping buffer 14 into 0.6MPa, the pressure ratio of ethylene gas The pressure of the damping buffer 14 is 0.2MPa larger, and the flow rate of the ethylene gas is changed to 14L / min; only the temperature of the jacket water bath of the static mixer 32 in the step C) is changed to 65°C, and the material in the static mixer 32 Change the residence time to 60s, change the temperature of the reaction material to be synthesized after the heat exchange in the heat exchanger 33 to 25°C, change the hydrolysis temperature of the hydrolysis kettle 34 to 10°C, and change the 6-carbonyl-8-chlorooctanoic acid ethyl...

Embodiment 3

[0034] Only change the mol ratio of 6-chloro-6-oxohexanoic acid ethyl ester, anhydrous aluminum chloride and ethylene dichloride described in step A) into 1: 2.5: 8, the flow rate of complexing liquid Change 10000L / min into 10000L / min, change the pressure of damping buffer 14 into 0.3MPa; Only change the pressure of the ethylene gas in step B) into 0.9MPa, change the pressure of damping buffer 14 into 0.65MPa, the pressure ratio of ethylene gas The pressure of the damping buffer 14 is 0.25MPa larger, and the flow rate of the ethylene gas is changed to 18L / min; only the jacket water bath temperature of the static mixer 32 in the step C) is changed to 78°C, and the material in the static mixer 32 Change the residence time to 15s, change the temperature of the reaction material to be synthesized after the heat exchange in the heat exchanger 33 to 10°C, change the hydrolysis temperature of the hydrolysis kettle 34 to 25°C, and the gas phase of 6-carbonyl-8-chlorooctanoic acid ethyl...

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Abstract

The invention relates to a synthesis device for 6-carbonyl-8-chloroethylcaprylate and a method for synthesizing 6-carbonyl-8-chloroethylcaprylate by using the device. The method comprises the following steps: introducing reaction raw materials including 6-chloro-6-oxoethylhexanoate, dichloroethane and anhydrous aluminum trichloride into a complexing solution preparation kettle to prepare a complexing solution; conveying ethylene to an inlet of an ethylene compressor, conveying the ethylene to an ethylene buffer tank from an opening of the ethylene buffer tank through an outlet pipeline of theethylene compressor, and conveying the ethylene to a premixer of a reaction mechanism through an outlet pipeline of the ethylene buffer tank to obtain a reaction material to be synthesized; and introducing the reaction material to be synthesized in the premixer into a static mixer from an inlet end of the static mixer, introducing the reaction material to be synthesized to a heat exchanger from aninlet end of the heat exchanger through an outlet end pipeline of the static mixer, introducing the reaction material to be synthesized to a hydrolysis kettle through an outlet end pipeline of the heat exchanger, and carrying out layering and distilling to obtain a finished product. According to the invention, preparation efficiency is improved, the consistency and stability of product quality under the condition of a continuous flow reaction are guaranteed, yield is improved, and the method is energy-saving, environment-friendly and safe.

Description

technical field [0001] The invention belongs to the technical field of a lipoic acid intermediate synthesis device, in particular to a 6-carbonyl-8-chlorooctanoic acid ethyl ester synthesis device, and also relates to a method for synthesizing 6-carbonyl-8-chlorooctanoic acid ethyl ester by the device. Background technique [0002] The aforementioned 6-carbonyl-8-chlorooctanoic acid ethyl ester synthetic device is substantially a 6-carbonyl-8-chlorooctanoic acid ethyl ester continuous flow synthetic device (hereinafter the same), correspondingly, the aforementioned synthetic 6-carbonyl-8-chlorooctanoic acid The method for ethyl ester is substantially the method for continuous flow synthesis of 6-carbonyl-8-chlorooctanoic acid ethyl ester (the same below). [0003] The English name of 6-carbonyl-8-chlorooctanoic acid ethyl ester is: ethyl 8-chloro-6-oxooctanoate, and the molecular formula is: C 10 h 17 o 3 Cl; molecular weight: 220.69, is a chemical reaction intermediate f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/347C07C69/716
CPCC07C67/347C07C69/716Y02P20/10
Inventor 丁建飞唐欢陆建刚钱庆石晓青邵敏张鑫彦
Owner SUZHOU FUSHILAI PHARMA CO LTD