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The Synthetic Technology of 2-Propoxy Ethyl Chloride

A technology of propoxy ethyl chloride and synthesis process, which is applied in the field of synthesis technology of 2-propoxy ethyl chloride, can solve the problems of cumbersome process, many process steps and high price, and achieves simple process and high catalytic efficiency. , the effect of low production cost

Active Publication Date: 2018-06-19
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-propoxychloroethane in the patent CN200810061878.0. The method uses bis(trichloromethyl)carbonate as the chlorinating agent instead of chlorinated ethylene chloride. Chlorinating agents such as sulfone, phosphorus oxychloride, and hydrogen chloride, under organic solvent conditions, use organic amines as catalysts to synthesize 2-propoxychloroethane. Due to the addition of organic solvents, the product must be distilled and purified, resulting in product yields The production rate 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] The traditional synthesis process of 2-propoxychloroethane has problems such as low product yield, unstable quality, serious environmental pollution, cumbersome process and prominent safety hazards. Therefore, the development of efficient, safe and environmentally friendly 2-propoxychloroethane Ethane Production Process Gets Wide Attention

Method used

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  • The Synthetic Technology of 2-Propoxy Ethyl Chloride
  • The Synthetic Technology of 2-Propoxy Ethyl Chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take 100g of ethylene glycol mono-n-propyl ether, 0.1g of pyridine and 0.14g of N,N-dimethylformamide respectively and add them to a reaction vessel with a reflux condenser, and 125.65g of thionyl chloride (content 99.2%, sulfuryl chloride Content 0.1%) was added to the constant pressure dropping funnel, heated to 35°C, started stirring, and slowly added thionyl chloride dropwise to the reaction vessel, sulfur dioxide and hydrogen chloride gas were released during the reaction process, and the rate of addition of thionyl chloride was controlled to make the temperature of the reaction solution Keep at 55±5°C.

[0031] After the dropwise addition of thionyl chloride, gradually raise the temperature to 90°C according to the rate of reaction gas release, until no gas is released, and continue to keep warm for 2h to obtain the crude product; cool the crude product to 30°C, directly add solid sodium hydroxide and stir, and thoroughly dissolve the thionyl chloride Decompose to...

Embodiment 2

[0033] Take 100g of ethylene glycol mono-n-propyl ether, 0.3g of pyridine and 0.55g of N,N-dimethylformamide into the reaction vessel with a reflux condenser, and 131.4g of thionyl chloride (content 99.0%, sulfuryl chloride Content 0.3%) was added into the constant pressure dropping funnel, heated to 40°C, started stirring, slowly added thionyl chloride dropwise to the reaction vessel, sulfur dioxide and hydrogen chloride gas were released during the reaction, and the rate of addition of thionyl chloride was controlled to make the temperature of the reaction solution Keep at 60±5°C.

[0034] After the dropwise addition of thionyl chloride is completed, gradually raise the temperature to 95°C according to the reaction gas release rate until no gas is released, and continue to keep warm for 3h to obtain the crude product; cool the crude product to 40°C, directly add solid sodium hydroxide and stir, and thoroughly dissolve the thionyl chloride Decompose to obtain 116.4 g of 2-pro...

Embodiment 3

[0036] Take 100g of ethylene glycol mono-n-propyl ether, 0.5g of pyridine and 1.15g of N,N-dimethylformamide into the reaction vessel with reflux condenser respectively, and 137.1g of thionyl chloride (content 98.3%, sulfuryl chloride Content 0.5%) was added into the constant pressure dropping funnel, heated to 45°C, started stirring, slowly added thionyl chloride dropwise to the reaction vessel, sulfur dioxide and hydrogen chloride gas were released during the reaction, and the rate of addition of thionyl chloride was controlled to make the temperature of the reaction solution Keep at 60±5°C.

[0037] After the dropwise addition of thionyl chloride, 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 4h to obtain the crude product; cool the crude product to 40°C, directly add solid sodium hydroxide and stir, and thoroughly dissolve the thionyl chloride Decompose to obtain 116.1 g of 2-prop...

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Abstract

The invention belongs to the technical field of organic synthesis, and in particular relates to a synthesis process of 2-propoxy-chloroethane. The synthesis process comprises the steps that ethylene glycol mono-n-propyl ether and thionyl chloride are used as main materials under the synergistic effect of multiple catalysts; the reaction temperature is controlled by dropwise adding the thionyl chloride; a crude product is obtained through temperature rise and heat preservation; solid alkali is directly added after cooling to resolve excessive thionyl chloride and neutralization is performed; the 2-propoxy-chloroethane is finally obtained through filtration. Compared with the existing process, the synthesis process of the 2-propoxy-chloroethane has the advantages that the catalysts are low in price, easy to obtain, the catalytic efficiency is higher, the technological process is simple and convenient, safe and reliable, the product yield is high and the quality is stable, and the product content reaches 99.2 percent or more, the yield is greater than 98.6 percent, the product cost is lower, and the synthesis process of 2-propoxy-chloroethane is particularly suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a synthesis process of 2-propoxyethyl chloride. Background technique [0002] 2-Propoxyethyl chloride is one of the important raw materials for the preparation of the herbicide pretilachlor. As a low-toxicity, broad-spectrum and high-efficiency professional selective herbicide, it is widely used in the field of rice planting and has a broad market. The external demand is large. [0003] At present, the preparation of 2-propoxychloroethane mainly uses ethylene glycol mono-n-propyl ether as the starting material, and uses different chlorinating agents to chlorinate its hydroxyl group. 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 produ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/12C07C41/22
CPCC07C41/22C07C43/12
Inventor 张泰铭王业英冷亮张善民毕义霞李文娟贾远超
Owner SHANDONG KAISHENG NEW MATERIALS