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Continuous preparation method of high-content 2-chloroethanol

A technology with high content of chloroethanol, which is applied in the preparation of organic compounds, the preparation of halogens, and the preparation of hydroxyl compounds. It can solve the problems of obvious heat release, flammability, explosion, and toxicity, so as to improve the utilization rate and reduce the cost of raw materials. , the effect of high reaction efficiency

Pending Publication Date: 2020-03-27
WUXI YINXING PLASTIC IND TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the transportation, storage and use of chlorine and ethylene are extremely dangerous
[0003] At present, ethylene oxide and hydrogen chloride (or hydrochloric acid) are generally used as raw materials to produce high-concentration 2-chloroethanol at home and abroad. This process is to synthesize ethylene oxide and hydrogen chloride in liquid phase under certain conditions, and obtain it through dehydration and rectification. High-concentration 2-chloroethanol, although the product purity can reach more than 98%, but the whole reaction process exothermic is obvious, non-continuous production, raw material ethylene oxide is a toxic, flammable and explosive liquefied petroleum gas, not easy to travel long distances Transport, storage and use

Method used

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  • Continuous preparation method of high-content 2-chloroethanol
  • Continuous preparation method of high-content 2-chloroethanol

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Put 330g of ethylene glycol, 200g of hydrochloric acid (36%), 51g of water and 39g of adipic acid into the reaction kettle, stir and raise the temperature, until the temperature in the kettle reaches 110°C and reflux occurs, drop into the kettle at a rate of 150g / h Mixed solution (ethylene glycol: 36% hydrochloric acid: the weight ratio of water is 2.2: 3.6: 1). When the condensate just appears in the top condenser, turn on the reflux ratio control immediately, keep the reflux ratio 2:3 and the temperature in the kettle at 113±3°C to obtain the crude product of 2-chloroethanol, the content is 42%, and the acid value (calculated as HCl ) was 0.07%, and the yield of 2-chloroethanol (calculated as HCl) in the reaction stage reached 99.3%.

[0030] Put 800g of the above-mentioned crude product and 240g of water-carrying benzene into the rectification kettle, heat and keep the top temperature at 67-72°C, distill at atmospheric pressure, and remove the lower layer of water by...

Embodiment 2

[0033] Put 500g of ethylene glycol, 303g of hydrochloric acid (36%), 77g of water and 59g of adipic acid into the reaction kettle, stir and raise the temperature, until the temperature in the kettle reaches 110°C and reflux occurs, drop into the kettle at a rate of 180g / h Mixed solution (ethylene glycol: 36% hydrochloric acid: the weight ratio of water is 2.2: 3.6: 1). When the condensate just appeared in the top condenser, turn on the reflux ratio control immediately, keep the reflux ratio 2:3 and the temperature in the kettle at 115±3°C, and obtain the crude product of 2-chloroethanol, the content is 41.8%, the acid value (calculated by HCl ) was 0.07%, and the yield of 2-chloroethanol (calculated as HCl) in the reaction stage reached 99%.

[0034] Put 800g of the above-mentioned crude product and 240g of water-carrying agent benzene into the rectification kettle, and dehydrate at the top temperature of 67-72°C. Remove benzene at a kettle temperature of 110-130°C.

[0035]...

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Abstract

The invention provides a continuous preparation method of high-content 2-chloroethanol, which comprises the following specific steps: quantitative ethylene glycol, 36% hydrochloric acid, water and a catalyst adipic acid are used as base materials and react at 110-120 DEG C until reflux occurs, and a mixed solution of ethylene glycol, 36% hydrochloric acid and water is continuously and dropwisely added; the generated 2-chloroethanol and water are evaporated out along with azeotropy at the temperature, the reflux ratio is controlled to be 2: 3, one part of condensate flows back to a packed tower, and the other part of condensate enters a receiving tank to obtain a 2-chloroethanol crude product with the concentration being about 42%; and finally, the crude product is subjected to benzene dehydration with water, debenzolization and vacuum distillation to obtain 2-chloroethanol with the content of 99% or above. The method is high in reaction efficiency and low in raw material cost, and theobtained 2-chloroethanol is suitable for production of intermediates in the industries of medicines, dyes and pesticides. The method adopts relatively safe ethylene glycol as a raw material instead ofethylene oxide, and the transportation, storage and use risks are low.

Description

technical field [0001] The invention belongs to the field of organic chemical industry, and in particular relates to a continuous preparation method of high-content 2-chloroethanol. Background technique [0002] 2-Chloroethanol is an important organic solvent and raw material for organic synthesis. It is not only an important raw material for the synthesis of polysulfide rubber, but also widely used in the pharmaceutical, dye and pesticide industries. There are two main methods for the industrial preparation of 2-chloroethanol, namely the chloric acid method and the ethylene oxide method. The chloric acid method is to pass ethylene and chlorine gas into water at the same time, chlorine gas and water react to form hypochlorous acid, and hypochlorous acid is added to ethylene to produce 2-chloroethanol. The content of the 2-chloroethanol aqueous solution obtained by this method is relatively low, and it takes a long time of azeotropic dehydration and vacuum distillation to ob...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/62C07C29/80C07C29/82C07C31/36
CPCC07C29/62C07C29/80C07C29/82C07C31/36
Inventor 蒋奇伟
Owner WUXI YINXING PLASTIC IND TECH
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