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The preparation method of 2-chloroethyl propyl ether

A technology of chloroethyl propyl ether and n-propyl ether, which is applied in the field of preparation of 2-chloroethyl propyl ether, can solve the problems of many process steps, low product yield and high price, and achieves safe and reliable technological process. The effect of high product yield and low production cost

Active Publication Date: 2018-01-30
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Tong Guotong discloses a preparation method of the herbicide pretilachlor intermediate 2-chloroethyl propyl ether in the patent CN200810061878.0. The method uses bis(trichloromethyl)carbonate as the chlorinating agent instead of chlorinated chlorinated Chlorinating agents such as sulfone, phosphorus oxychloride, and hydrogen chloride, under organic solvent conditions, use organic amines as catalysts to synthesize 2-chloroethyl propyl ether intermediates. Due to the addition of organic solvents, the product must be distilled and purified, resulting in The product yield is low, the energy consumption is high, the product quality is unstable, and there are many process steps. At the same time, the price of bis(trichloromethyl)carbonate (triphosgene for short) is relatively high, which is not conducive to industrialization
[0004] In summary, the traditional 2-chloroethyl propyl ether preparation method has problems such as low product yield, unstable quality, serious environmental pollution, cumbersome process, and prominent safety hazards. Therefore, it is urgent to develop an efficient, safe, and environmentally friendly method. The preparation method of 2-chloroethyl propyl ether

Method used

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  • The preparation method of 2-chloroethyl propyl ether
  • The preparation method of 2-chloroethyl propyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Take 100g of ethylene glycol mono-n-propyl ether and 0.1g of 4-dimethylaminopyridine respectively into the reaction vessel with a reflux condenser, add 120g of thionyl chloride (content 99.2%, sulfuryl chloride content 0.1%) into the constant pressure drop Liquid funnel, start stirring, slowly add thionyl chloride dropwise to the reaction vessel, the reaction process releases sulfur dioxide and hydrogen chloride gas, control the rate of thionyl chloride addition to keep the temperature of the reaction solution at 25°C.

[0029] After the addition of thionyl chloride is completed, turn on the heating, and gradually raise the temperature to 90°C according to the reaction gas release rate, until no gas is released, and continue to keep warm for 2 hours to obtain the crude product; after the crude product is cooled to 50°C, add water to it for hydrolysis, and let it stand for stratification The water layer was removed, the organic layer was neutralized with sodium hydroxide ...

Embodiment 2

[0031] Take 100g ethylene glycol mono-n-propyl ether and 0.3g 4-dimethylaminopyridine respectively and add them to the reaction vessel with a reflux condenser, add 123.4g of thionyl chloride (content 99.0%, sulfuryl chloride content 0.3%) to constant pressure Start the stirring in the dropping funnel, and slowly add thionyl chloride dropwise to the reaction vessel. During the reaction, sulfur dioxide and hydrogen chloride gas are released, and the dropping rate of thionyl chloride is controlled to keep the temperature of the reaction solution at 30°C.

[0032] After the dropwise addition of thionyl chloride is completed, turn on the heating, and gradually raise the temperature to 95°C according to the rate of reaction gas release, until no gas is released, and continue to keep warm for 3 hours to obtain the crude product; after the crude product is cooled to 40°C, add water to it for hydrolysis, and let it stand for stratification The water layer was removed, the organic layer ...

Embodiment 3

[0034] Take 100g ethylene glycol mono-n-propyl ether and 0.5g 4-dimethylaminopyridine respectively and add them to the reaction vessel with a reflux condenser, add 125.6g of thionyl chloride (content 98.2%, sulfuryl chloride content 0.5%) to constant pressure Start the stirring in the dropping funnel, and slowly add thionyl chloride dropwise to the reaction vessel. During the reaction process, sulfur dioxide and hydrogen chloride gas are released, and the dropping rate of thionyl chloride is controlled to keep the temperature of the reaction solution at 50°C.

[0035] After the addition of thionyl chloride is completed, turn on the heating, and gradually raise the temperature to 100°C according to the reaction gas release rate until no gas is released, and continue to keep warm for 4 hours to obtain the crude product; after the crude product is cooled to 30°C, add water to it for hydrolysis, and let it stand for stratification The water layer was removed, the organic layer was ...

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Abstract

The invention belongs to the technical field of organic synthesis and specifically relates to a preparation method of 1-(2-chloroethoxy)propane. By an efficient nucleophilic catalyst, 2-propoxyethanol and thionyl chloride are used as main raw materials, and reaction temperature is strictly controlled by dropwise adding thionyl chloride; after heating and thermal insulation, a crude product is obtained; and after hydrolysis, neutralization and standing for liquid separation, 1-(2-chloroethoxy)propane is obtained. In comparison with traditional technologies, the invention has the following advantages: efficiency of the catalyst is higher; the technological process is safe and reliable; operation is simple; product yield is high; quality is stable; product content reaches 99.0% and above; yield is greater than 98.5%; and production cost is lower. The preparation method of the invention is especially suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a preparation method of 2-chloroethyl propyl ether. Background technique [0002] The 2-chloroethyl propyl ether in the present invention is 2-propoxyl chloroethane, which is one of the important raw materials for the preparation of the herbicide pretilachlor. Herbicides are widely used in the field of rice planting, have a broad market, and are in great demand at home and abroad. [0003] At present, 2-chloroethyl propyl ether mainly uses ethylene glycol mono-n-propyl ether as the starting material, and uses different chlorinating agents to chlorinate its hydroxy groups. Yang Jianping etc. (the synthetic method of 2-n-propoxyl ethyl chloride, Zhejiang chemical industry, 1999, the 30th volume, the 4th phase) are chlorination agent with ethylene glycol monopropyl ether and thionyl chloride, adopt composite catalyst, The content of the final product can reac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C41/22C07C43/12
CPCC07C41/22C07C43/12
Inventor 贾远超张泰铭马团芝张善民孙丰春王鑫海王炼张良肖志宇
Owner SHANDONG KAISHENG NEW MATERIALS