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Preparation process of 2-propoxy chloroethane

A technology for the preparation of propoxyl ethyl chloride and its preparation technology, which is applied in the field of preparation technology of 2-propoxyl ethyl chloride, can solve the problems of low yield, cumbersome process steps, high energy consumption, etc., and achieve high product yield, Simple process and high catalytic efficiency

Inactive Publication Date: 2017-08-18
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a kind of preparation technology of 2-propoxyl ethyl chloride, solve the problems of low yield, complicated processing steps and high energy consumption in the existing technology, and have mild reaction conditions, simple technology, The operation process is safe and reliable, and the purity and yield of the product are significantly improved

Method used

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  • Preparation process of 2-propoxy chloroethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] The preparation technology of 2-propoxyl ethyl chloride is as follows:

[0018] (1) Weigh 100g of ethylene glycol mono-n-propyl ether, 0.1g of N,N-dimethylaniline, and 1.125g of triethylamine respectively, and add them to a reaction vessel with a reflux condenser, and 116.54g of chlorinated Add sulfoxide (99.2% content, 0.1% sulfuryl chloride content) into the constant pressure dropping funnel, heat up to 45°C, start stirring, slowly add thionyl chloride dropwise to the reaction vessel, and release sulfur dioxide during the reaction and hydrogen chloride gas, control the rate of addition of thionyl chloride to keep the temperature of the reaction solution at 55±5°C;

[0019] (2) After the addition of thionyl chloride is completed, the temperature is gradually raised to 90°C according to the reaction gas release rate until no gas is released, and the crude product is obtained after the heat preservation is continued for 1 hour. After the crude product is cooled to 60°C, ...

Embodiment 2

[0021] The preparation technology of 2-propoxyl ethyl chloride is as follows:

[0022] (1) Weigh 100g of ethylene glycol mono-n-propyl ether, 0.2g of N,N-dimethylaniline, and 0.334g of triethylamine, and add them to a reaction vessel with a reflux condenser, and 117.69g of chlorinated Add sulfoxide (99.0% content, 0.3% sulfuryl chloride content) into the constant pressure dropping funnel, heat up to 45°C, start stirring, slowly add thionyl chloride dropwise to the reaction vessel, and release sulfur dioxide during the reaction and hydrogen chloride gas, control the rate of addition of thionyl chloride to keep the temperature of the reaction solution at 60±5°C;

[0023] (2) After the dropwise addition of thionyl chloride is completed, the temperature is gradually raised to 95°C according to the reaction gas release rate until no gas is released, and the crude product is obtained after the heat preservation is continued for 1 hour. After the crude product is cooled to 40°C, a ce...

Embodiment 3

[0025] The preparation technology of 2-propoxyl ethyl chloride is as follows:

[0026] (1) Weigh 100g of ethylene glycol mono-n-propyl ether, 0.3g of N,N-dimethylaniline, and 0.5g of triethylamine, and add them to a reaction vessel with a reflux condenser, and 116.54g of chlorinated Add sulfoxide (99.3% content, 0.5% sulfuryl chloride content) into the constant pressure dropping funnel, heat up to 50°C, start stirring, slowly add thionyl chloride dropwise to the reaction vessel, and release sulfur dioxide during the reaction and hydrogen chloride gas, control the rate of addition of thionyl chloride to keep the temperature of the reaction solution at 60±5°C;

[0027] (2) After the dropwise addition of thionyl chloride is completed, the temperature is gradually raised to 95°C according to the reaction gas release rate until no gas is released, and the crude product is obtained after the heat preservation is continued for 1 hour. After the crude product is cooled to 40°C, a cert...

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Abstract

The invention relates to a preparation process of 2-propoxy chloroethane and belongs to the technical field of organic synthesis of fine chemical intermediates. The synthetic process comprises the following steps: by taking ethylene glycol monopropyl ether and excess thionyl chloride as raw materials and adopting a high efficiency composite catalyst, controlling the reaction rate through dropwise adding the thionyl chloride, raising the temperature and preserving the temperature to obtain a crude product, neutralizing, hydrolyzing, standing and layering to obtain the 2-propoxy chloroethane. Compared with the prior art, the preparation process disclosed by the invention has the advantages that the catalyst is higher in catalytic efficiency, low in price and easy to get; the process is simple, safe and reliable; the product is high in yield and stable in quality; the product content is up to above 99.0%; the yield is greater than 98.5%; catalysts used in the prior art easily react with little hydrochloric acid contained in the product to form complex salt which is a precipitate in the 2-propoxy chloroethane and then the product quality is influenced; and the preparation process is particularly suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation process of 2-propoxyethyl chloride, which belongs to the technical field of organic synthesis of fine chemical intermediates. Background technique [0002] At present, the preparation method of 2-propoxyl chloroethane mainly takes ethylene glycol mono-n-propyl ether as starting raw material, adopts different chlorinating agents to chlorinate its hydroxy groups, as in "Zhejiang Chemical Industry" in 1999, 30(4 ) published "the synthetic method of 2-n-propoxyl ethyl chloride", it is with ethylene glycol monopropyl ether as starting raw material, and thionyl chloride is as chlorinating agent, adopts composite catalyst, and final product content is 98.1%, yield 97%; CN200810061878.0 discloses taking bis(trichloromethyl)carbonate as chlorinating agent, replacing chlorinating agents such as thionyl chloride, phosphorus oxychloride, hydrogen chloride, under organic solvent condition , using organic amines as catalysts t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/22C07C43/12
CPCC07C41/22C07C43/12
Inventor 石余飞韩楠楠薛居强王荣海张泰铭王军李光辉黄桂青
Owner SHANDONG KAISHENG NEW MATERIALS
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