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Industrial preparation method of acryloyloxyethyl trimethyl ammonium chloride

A technology of acryloyloxyethyltrimethylammonium chloride and dimethylaminoethyl acrylate, which is applied in the preparation of aminohydroxy compounds, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problem of unpleasant smell, product Low purity, waste of activated carbon and other problems, to achieve the effect of optimizing feeding time and rate, optimizing internal structure, and improving product yield

Pending Publication Date: 2022-07-22
山东蓝湾新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But this method needs to add polymerization inhibitor in the initial process, easily causes the prepared product purity to be lower; Basic anion exchange resin has the process of regeneration simultaneously, and easily deactivates, and is difficult in actual industrial operation; In addition, because Trimethylamine can corrode aluminum, magnesium, zinc, tin, copper, and copper alloys, etc., and has an unpleasant smell. Storage and application requirements are high, resulting in high overall actual operating costs
[0004] The method for preparing acryloyloxyethyltrimethylammonium chloride under pressurized conditions with dimethylaminoethyl acrylate and monochloromethane can effectively solve the above problems at present, but there is still a difference between the injection rate of monochloromethane and the dichloromethane in this method. The stirring rate of the reactor is uncoordinated, the liquid flow in the reactor is unscientific, and the reactants cannot be fully contacted, resulting in a low conversion rate of dimethylaminoethyl acrylate
At the same time, in the later stage of the reaction, the viscosity of the reaction system increases, and the reactor cannot effectively extract the heat of the reaction and locally overheats and self-polymerizes, resulting in difficulties in post-processing of the product
For the recovery of excess monochloromethane added, the adsorption rate of traditional activated carbon is up to 75%, and it cannot be reused after adsorption, resulting in waste of activated carbon

Method used

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preparation example Construction

[0046] The embodiment of the present invention provides an industrial preparation method of acryloyloxyethyl trimethyl ammonium chloride, and the industrial preparation method comprises:

[0047] (1) dimethylaminoethyl acrylate, deionized water and monochloromethane are added to the first-stage reactor for feeding;

[0048] (2) After the first-stage reactor completes feeding, transfer the material in the first-stage reactor to the second-stage reactor for 0.5-1.0 h; then the second-stage reactor The material in the reactor is transferred to the third-stage reactor to react for 0.5-1.0 h to obtain the primary product;

[0049] (3) the primary product is placed in a stripping tower for stripping treatment;

[0050] (4) The stripping tower bottom liquid obtained by the stripping treatment is placed in the fourth-stage reactor and stirred, and then the material in the fourth-stage reactor is transferred to the fifth-stage reactor and stirred. Stirring was performed to obtain the...

Embodiment 1

[0107] 1. 2500kg of dimethylaminoethyl acrylate and 746.67kg of deionized water are pumped into the first-stage reactor through a pipeline, and controlled to inject 1000kg of monochloromethane into the reactor at a constant speed within 1.0h, and the reaction is achieved at the feed rate. Start stirring when the minimum stirring liquid level of the device is started, and the stirring speed is 40rpm;

[0108] Ⅱ. The reaction starts after the first-stage reactor is put into monochloromethane, and then the temperature rises to about 35°C, and the ethylene glycol aqueous solution is adjusted to control the reaction temperature to rise to 41°C, and the pressure of the first-stage reactor is increased by the compressed air regulating valve. pressure to 0.7MPa;

[0109] Ⅲ. After the feeding is completed, transfer the material of the first-stage reactor to the second-stage reactor with a pump, and open the gas phase balance pipe between the first-stage reactor and the second-stage rea...

Embodiment 2

[0117] Embodiment 2 is basically the same as embodiment 1, and the difference lies in that: monochloromethane is 885kg.

[0118] In this example, the conversion rate of dimethylaminoethyl acrylate was 88%, and 2980.1kg of acryloyloxyethyltrimethylammonium chloride product was obtained. The product was a colorless and slightly turbid liquid with a purity of 79.2%. Degree is 1%, moisture is 19.9%.

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Abstract

The invention provides an industrial preparation method of acryloyloxyethyl trimethyl ammonium chloride. The method comprises the following steps: adding dimethylamino ethyl acrylate, deionized water and methane chloride into a first-stage reactor for feeding; after the first-stage reactor finishes feeding, transferring the materials in the first-stage reactor into a second-stage reactor to react for 0.5-1.0 h; transferring the material in the second-stage reactor into a third-stage reactor, and reacting for 0.5-1.0 h to obtain a primary product; carrying out steam stripping treatment on the primary product in a steam stripping tower; and placing a stripping tower bottom solution obtained through stripping treatment into a fourth-stage reactor, stirring, transferring a material in the fourth-stage reactor into a fifth-stage reactor, and stirring to obtain the acryloyloxyethyl trimethyl ammonium chloride. According to the industrial preparation method, multiple reaction kettles are adopted for intermittent reaction, industrial continuous production is achieved, high efficiency is achieved, the product yield is high, and the methane chloride separation effect is good.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to an industrial preparation method of acryloyloxyethyltrimethylammonium chloride. Background technique [0002] Acryloyloxyethyltrimethylammonium chloride is one of the quaternary ammonium salt raw materials required for the production of cationic acrylamide polymers. Cationic acrylamide polymers are used in petrochemical, papermaking, textile printing and dyeing, daily chemicals, especially as flocculation It has important application value in water treatment, sludge dewatering and other fields, so the market demand of acryloyloxyethyltrimethylammonium chloride has grown steadily. [0003] The Chinese patent with the application number of CN201110142015.8 discloses a method for producing (meth)acryloyloxyethyltrimethylammonium chloride by transesterification, in the combination of polymerization inhibitor and basic anion exchange resin as catalyst. Under the action, (m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C219/08C07C213/02C07C213/10C07C17/38C07C19/03
CPCC07C213/02C07C213/10C07C17/38C07C219/08C07C19/03
Inventor 李金江王兵杰荣洪杰
Owner 山东蓝湾新材料有限公司
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