Preparation method of quaternary ammonium cationic monomer aqueous solution

A cationic monomer, aqueous solution technology, applied in the preparation of organic compounds, chemical instruments and methods, preparation of aminohydroxy compounds, etc., can solve the problems of high price, reduce the hydrolysis of raw materials, stable production conditions, etc., and achieve maintenance and operation safety. Convenience, increased reaction rate and effect of mild reaction conditions

Inactive Publication Date: 2015-07-01

浙江友联化学工业有限公司

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Problems solved by technology

Moreover, it takes a long time to stabilize the reaction conditions, and the production efficiency is low

This method is also difficult to make production conditions such as reaction temperature, the proportioning ratio of reaction raw materials stable, and product quality also becomes unstable easily.

[0006] Japanese Patent Laid-Open No. 7-206790 discloses a synthesis method of quaternary ammonium salt-type cationic monomers. The synthesis reaction is carried out in a thin-film steamer reactor, which greatly shortens the reaction time and...

Abstract

The invention discloses a preparation method of a quaternary ammonium cationic monomer aqueous solution. The preparation method comprises the following steps: after fully mixing a mixture of unsaturated tertiary amine and a polymerization inhibitor with water, continuously feeding the mixture to a tower reactor from the upper part of the tower reactor; and continuously introducing gas halohydrocarbon from the lower part of the tower reactor to the tower reactor, wherein the unsaturated tertiary amine and the gas halohydrocarbon in the tower reactor are in countercurrent contact to react, the reaction temperature is 35-60 DEG C and the reaction time is 3-15 minutes. The preparation method disclosed by the invention realizes continuous production and is short in reaction time, and the conversion ratio of the unsaturated tertiary amine reaches over 99.8%, the content of a byproduct acrylic acid is less than 1000ppm, the content of the byproduct is low, the product yield is high and the product quality is stable.

Application Domain

Organic compound preparationAmino-hyroxy compound preparation

Technology Topic

ChemistryAqueous solution +7

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Examples

Experimental program(6)
Comparison scheme(2)

Example Embodiment

[0035] Example 1

[0036] The tower reactor is an ordinary rectification tower with an electric heating belt attached to the tower body. The specification is 30×2.5mm and the height is 1.5m. It is equipped with Φ2×2mm stainless steel θ ring packing, and the packing height is 1.3m. Heated by an electric heating belt, the temperature of the tower section is raised to 45°C, dimethylaminoethyl acrylate with a p-hydroxyanisole content of 0.06% and water are fed into the static state at the feed rate of 6g/min and 2.1g/min respectively. The mixer enters the reaction tower from the feed port at the top of the tower reactor after thorough mixing, and the methyl chloride gas enters the reaction tower from the bottom of the tower reactor at a feed rate of 2.3 g/min. The product formed after the reaction mass reacted in the reaction tower for 5 minutes was collected in a glass round bottom flask.

[0037] Analyze the content of dimethylaminoethyl acrylate in the crude product to calculate the conversion rate of raw materials. The conversion rate of dimethylaminoethyl acrylate was 99.8%. The crude product was analyzed by high performance liquid chromatography and the concentration of by-product acrylic acid was determined as 613ppm. Remove the reaction liquid in the flask, blow the air for 30 minutes to purge the excess methyl chloride gas, and then wash it with toluene to remove the residual small amount of dimethylaminoethyl acrylate, and then obtain acryloxyethyl trimethyl chloride An aqueous solution product with an ammonium content of 80.2%.

Example Embodiment

[0038] Example 2

[0039] The tower reactor is an ordinary rectification tower with an electric heating belt attached to the tower body. The specification is 30×2.5mm and the height is 1.5m. It is equipped with Φ2×2mm stainless steel θ ring packing, and the packing height is 1.3m. The temperature of the tower section is raised to 35℃ by heating with an electric heating belt. Dimethylaminoethyl acrylate with a hydroquinone content of 0.15% and water are added into the static mixing at the feed rate of 9g/min and 3.2g/min respectively. After being fully mixed, it enters the reaction tower from the top feed port of the tower reactor, and the methyl chloride gas enters the reaction tower from the bottom of the tower reactor at a feed rate of 3.5 g/min. The product formed after the reaction mass reacted in the reaction tower for 4 minutes was collected in a glass round bottom flask.

[0040] Analyze the content of dimethylaminoethyl acrylate in the crude product to calculate the conversion rate of raw materials. The conversion rate of dimethylaminoethyl acrylate is 97.5%. The crude product is analyzed by high performance liquid chromatography and the concentration of by-product acrylic acid is determined as 925ppm. Remove the reaction liquid in the flask, blow the air for 30 minutes to purge the excess methyl chloride gas, and then wash it with toluene to remove the residual small amount of dimethylaminoethyl acrylate, and then obtain acryloxyethyl trimethyl chloride An aqueous solution product with an ammonium content of 78.3%.

Example Embodiment

[0041] Example 3

[0042] The tower reactor is an ordinary rectification tower with an electric heating belt attached to the tower body. The specification is 30×2.5mm and the height is 1.5m. It is equipped with Φ2×2mm stainless steel θ ring packing, and the packing height is 1.3m. Heated by an electric heating belt, the temperature of the tower section is raised to 55°C, and dimethylaminoethyl methacrylate with a hydroquinone content of 0.1% and water are added simultaneously at a feed rate of 6g/min and 2.0g/min. The static mixer enters the reaction tower from the feed port at the top of the tower reactor after thorough mixing, and the methyl chloride gas enters the reaction tower from the bottom of the tower reactor at a feed rate of 2.1 g/min. The product formed after the reaction mass reacted in the reaction tower for 8 minutes was collected in a glass round bottom flask.

[0043] Analyze the content of dimethylaminoethyl methacrylate in the crude product to calculate the conversion rate of the raw material. The conversion rate of the raw material dimethylaminoethyl methacrylate is 99.8%. The crude product is analyzed by high performance liquid chromatography to determine the side effects. The concentration of the product methacrylic acid was 525 ppm. The reaction liquid in the flask was removed, and the excess methyl chloride gas was purged with air for 30 minutes, and then washed with toluene. After removing the residual small amount of dimethylaminoethyl methacrylate, the methacryloxyethyl trimethacrylate was obtained. An aqueous solution product with a methyl ammonium chloride content of 80.1%.

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Classification and recommendation of technical efficacy words

short stay
Reduce hydrolysis rate

Preparation method of quaternary ammonium cationic monomer aqueous solution

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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