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Method for preparing chlorphenesin by using micro-channel continuous flow reactor

A technology of chlorphenesin and reactor, which is applied in the field of microchannel continuous flow reactor to prepare chlorphenesin, can solve the problems of low conversion rate of raw materials, potential safety hazards, small heat exchange area, etc., and achieve simple and efficient reaction process , the effect of improving production efficiency

Inactive Publication Date: 2019-02-01
HUBEI ARTEC CARBOHYDRATE CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The object of the present invention is to provide a kind of method that adopts microchannel continuous flow reactor to prepare chlorphenesin, to solve the problem that present domestic and foreign all adopt p-chlorophenol and 3-chloro-1,2-propanediol in the above-mentioned background technology as Starting raw materials, the condensation products are obtained through the action of alkali, such as p-chlorophenol, 3-chloro-1,2-propanediol, and sodium hydroxide is refluxed in ethanol solution for 3-6 hours to react. First, the reaction is exothermic in large quantities. Traditional The tank reaction has a small heat transfer area and has potential safety hazards. Secondly, the reaction produces water, which will not only prevent the reaction from proceeding, but also cause the hydrolysis of 3-chloro-1,2-propanediol to glycerol, so the conversion rate of raw materials is lower than 90%, and the problem of generating more waste liquid

Method used

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  • Method for preparing chlorphenesin by using micro-channel continuous flow reactor

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] a) Put 1 mol of chlorophenol and 1.02 mol of 3-chloro-1,2-propanediol into volumetric flask A with a volume of 1L, add 500ml of methanol and stir to dissolve, after completely dissolved, add methanol again to make the volume to 1L, Add 1.02mol30% liquid sodium methoxide to 500ml volumetric flask B, and use methanol to set the volume to 500ml, then connect volumetric flask A to the microchannel continuous flow reactor produced by Shandong Haomai Machinery Technology Co., Ltd. with a constant flow pump, Adjust the flow rate to 1ml / s, connect the volumetric flask B to the microchannel continuous flow reactor produced by Shandong Haomai Machinery Technology Co., Ltd. with a constant flow pump, adjust the flow rate to 0.6ml / s, and set the temperature at 60°C , carry out the etherification reaction, receive the reaction liquid with the flask to obtain the semi-finished product A;

[0018] b) Leave the semi-finished product A obtained in step a) to cool naturally to 30°C, plac...

Embodiment 2

[0021] a) Put 1 mol of chlorophenol and 1.02 mol of 3-chloro-1,2-propanediol into volumetric flask A with a volume of 1L, add 505ml of methanol and stir to dissolve, after completely dissolved, add methanol again to make the volume to 1L, Add 1mol30% liquid sodium methoxide into 500ml volumetric flask B, and adjust the volume to 500ml with methanol, and connect volumetric flask A to the microchannel continuous flow reactor produced by Shandong Haomai Machinery Technology Co., Ltd. using a constant flow pump. Adjust the flow rate to 1.2ml / s, connect the volumetric flask B to the microchannel continuous flow reactor produced by Shandong Haomai Machinery Technology Co., Ltd. with a constant flow pump, adjust the flow rate to 0.6ml / s, and set the temperature at 500°C , carry out the etherification reaction, receive the reaction liquid with the flask to obtain the semi-finished product A;

[0022] b) Leave the semi-finished product A obtained in step a) to cool naturally to 30°C, p...

Embodiment 3

[0025] a) Put 1 mol of chlorophenol and 1.2 mol of 3-chloro-1,2-propanediol into volumetric flask A with a volume of 1L, add 520ml of methanol and stir to dissolve, after completely dissolved, add methanol again to make the volume to 1L, Add 1 mol of 30% liquid sodium methoxide into 500ml volumetric flask B, and make the volume to 500ml with methanol, connect volumetric flask A to the continuous flow reactor produced by Corning Company of the United States with a constant flow pump, and adjust the flow rate to 1.2ml / second, the volumetric flask B is connected to the microchannel continuous flow reactor produced by Corning Corporation of the United States using a constant flow pump, the flow rate is adjusted to 0.4ml / s, the temperature is set at 700 ° C, and the etherification reaction is carried out. Receive the reaction solution to obtain the semi-finished product A;

[0026] b) Leave the semi-finished product A obtained in step a) to cool naturally to 25°C, put the cooled ...

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Abstract

The invention belongs to the technical field of organic chemistry, and particularly relates to a method for preparing chlorphenesin by using a micro-channel continuous flow reactor. The method for preparing the chlorphenesin by using the micro-channel continuous flow reactor comprises the following specific operation steps: a) injecting a methanol mixed solution of chlorophenol and 3-chloro-1,2-propanediol and a liquid sodium methoxide solution in the micro-channel continuous flow reactor, staying for 30-120 seconds at the temperature of 40-100 DEG C, and carrying out etherification reaction;and b) cooling, centrifuging, concentrating and recrystallizing a reaction solution to obtain the product. Compared with a traditional method, the method has the advantages that the whole reaction process is simple and efficient, and is safe and reliable, the total yield can reach 90%, the product purity reaches 99.5% or above, and the production efficiency is improved effectively.

Description

technical field [0001] The invention relates to the technical field of organic chemistry, in particular to a method for preparing chlorphenesin by using a microchannel continuous flow reactor. Background technique [0002] Chlorphenesin is a fine chemical product. In medicine and cosmetics, chlorphenesin is used as an antibacterial preservative. At present, p-chlorophenol and 3-chloro-1,2-propanediol are used as starting materials at home and abroad. , to obtain condensation products through the action of alkali, such as p-chlorophenol, 3-chloro-1,2-propanediol, and sodium hydroxide in ethanol solution to reflux for 3-6 hours to react. First, the reaction is exothermic in large quantities, and the traditional kettle method The heat exchange area of ​​the reaction is small, which has potential safety hazards. Secondly, the reaction produces water, which will not only prevent the reaction from proceeding, but also cause the hydrolysis of 3-chloro-1,2-propanediol to glycerol, s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/16C07C43/23B01J19/00
CPCB01J19/0093C07C41/16C07C43/23
Inventor 李林飞
Owner HUBEI ARTEC CARBOHYDRATE CHEM
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