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Method for preparing dimethyl diallyl ammonium chloride

A technology of dimethyl diallyl ammonium chloride and dimethylamine aqueous solution, which is applied in chemical instruments and methods, preparation of amino compounds, preparation of organic compounds, etc., can solve the problems of inability to accurately control the reaction temperature, continuous production, Dropping process is slow and other problems, to achieve the effect of short reaction residence time, stable product quality and high safety

Active Publication Date: 2015-02-25
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to propose a method for preparing dimethyl diallyl ammonium chloride in view of the fact that dimethyl diallyl ammonium chloride cannot accurately control the reaction temperature, the reaction time is too long, the dropping process is slow, and continuous production cannot be performed. ammonium chloride method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1 equivalent of dimethylamine and 1 equivalent of sodium hydroxide were formulated into 40wt% dimethylamine aqueous solution and 32wt% sodium hydroxide aqueous solution through two pumps and first pumped into the mixing module for mixing, then the above mixed solution and allyl chloride According to the molar ratio of 1:2.0 pumped into the microchannel, the flow rates of allyl chloride, dimethylamine aqueous solution, and sodium hydroxide aqueous solution were controlled at 1.8ml / min, 1.5ml / min, and 1.0ml / min respectively, and passed through the microchannel modular reaction device. The reaction was carried out in a microstructure reactor at 40°C, and the reaction residence time was kept at 6.25min. The reaction product is introduced into the separator, static layered, the oil phase is removed to take the water layer, the pH value of the water layer is adjusted to 5-7 with dilute hydrochloric acid, and then decolorized by activated carbon under reduced pressure distillat...

Embodiment 2

[0028] 1 equivalent of dimethylamine and 1 equivalent of sodium hydroxide were formulated into 40wt% dimethylamine aqueous solution and 32wt% sodium hydroxide aqueous solution through two pumps and first pumped into the mixing module for mixing, then the above mixed solution and allyl chloride According to the molar ratio of 1:2.0 pumped into the microchannel, the flow rates of allyl chloride, dimethylamine aqueous solution, and sodium hydroxide aqueous solution were controlled at 1.8ml / min, 1.5ml / min, and 1.0ml / min respectively, and passed through the microchannel modular reaction device. The reaction was carried out in a microstructure reactor at 45°C, and the reaction residence time was kept at 6.25min. The reaction product is introduced into the separator, static layered, the oil phase is removed to take the water layer, the pH value of the water layer is adjusted to 5-7 with dilute hydrochloric acid, and then decolorized by activated carbon under reduced pressure distillat...

Embodiment 3

[0030] 1 equivalent of dimethylamine and 1 equivalent of sodium hydroxide were formulated into 40wt% dimethylamine aqueous solution and 32wt% sodium hydroxide aqueous solution through two pumps and first pumped into the mixing module for mixing, then the above mixed solution and allyl chloride According to the molar ratio of 1:2.0 pumped into the microchannel, the flow rates of allyl chloride, dimethylamine aqueous solution, and sodium hydroxide aqueous solution were controlled at 1.8ml / min, 1.5ml / min, and 1.0ml / min respectively, and passed through the microchannel modular reaction device. The reaction was carried out in a microstructure reactor at 55°C, and the reaction residence time was kept at 6.25min. The reaction product is introduced into the separator, static layered, the oil phase is removed to take the water layer, the pH value of the water layer is adjusted to 5-7 with dilute hydrochloric acid, and then decolorized by activated carbon under reduced pressure distillat...

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Abstract

The invention discloses a method for preparing dimethyl diallyl ammonium chloride, which comprises the following steps: mixing a 20-50 wt% dimethylamine aqueous solution and a 25-40 wt% sodium hydroxide water solution; respectively and simultaneously pumping chloropropene and the mixed solution into a microchannel modular reactor, and keeping at the temperature of 25-65 DEG C for 5-20 minutes; and introducing the discharged material of the microchannel modular reactor into a separator, standing to stratify, removing the supernatant turbid oil, taking the understratum water layer, regulating the pH value to 5-7, and carrying out vacuum distillation and activated carbon adsorption decolorization to obtain the high-grade dimethyl diallyl ammonium chloride water solution. The preparation method disclosed by the invention is a continuous process, and has the characteristics of controllable preparation technique, high safety, mild reaction conditions, short reaction retention time and stable product quality; and the production device is simple, and is easy for disassembly and assembly and convenient to carry and move. The device can be conveniently adjusted by simply increasing or decreasing the quantity of the microchannels.

Description

technical field [0001] The invention relates to a method for preparing dimethyl diallyl ammonium chloride, which belongs to the technical field of chemical synthesis. Background technique [0002] Dimethyldiallylammonium chloride (DMDAAC) is a widely used cationic monomer. Because of its high positive charge density, good water solubility and easy control of relative molecular weight, it is widely used in daily chemical industry, sewage treatment, papermaking, petroleum treatment and other industries. [0003] There are two conventional synthesis techniques for dimethyl diallyl ammonium chloride, namely one-step method and two-step method. [0004] The one-step method is to directly prepare the cationic monomer by combining dimethylamine, allyl chloride and sodium hydroxide in the same reaction system. CN1800146 adopts a one-step method to alternately drop sodium hydroxide solution and allyl chloride solution into the allyl chloride solution. CN1362401A is also an improve...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C211/63C07C209/12
Inventor 郭凯方正沈卫东孙芹欧阳平凯
Owner NANJING UNIV OF TECH
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