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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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 can reduce the hydrolysis of raw materials, but the conversion rate of raw materials is low. , the product yield is low
Moreover, the structure of this thin film evaporator reactor is complex, the production efficiency is low, the price is expensive, and it needs stirring to assist mass transfer, which limits the large-scale application of this process in industry
U.S. Patent No. 6,686,203 uses a rotating disk stirring tower to carry out the reaction continuously, but there is a problem that the residence time of the material is too long

Method used

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  • Preparation method of quaternary ammonium cationic monomer aqueous solution
  • Preparation method of quaternary ammonium cationic monomer aqueous solution
  • Preparation method of quaternary ammonium cationic monomer aqueous solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 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 to raise the temperature of the tower section to 45°C, and dimethylaminoethyl acrylate and water with a p-hydroxyanisole content of 0.06% were added to the static The mixer enters the reaction tower from the top feed port of the tower reactor after being fully mixed, and the methyl chloride gas enters the reaction tower from the bottom of the tower reactor at a feed rate of 2.3g / min. The product formed after the reaction mass was 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 dimethylaminoet...

Embodiment 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. Heated by an electric heating belt to raise the temperature of the tower section to 35°C, dimethylaminoethyl acrylate and water with a hydroquinone content of 0.15% were added to 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 3.5g / min. The product formed after the reaction mass was 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 ma...

Embodiment 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 to raise the temperature of the tower section to 55°C, and dimethylaminoethyl methacrylate with a hydroquinone content of 0.1% and water were added at the same time at a feed rate of 6g / min and 2.0g / min respectively The static mixer enters the reaction tower from the top feed port of the tower reactor after being fully mixed, 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 was 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 in the flask to calcula...

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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.

Description

technical field [0001] The invention belongs to the field of chemical products, and in particular relates to a preparation method of an aqueous solution of a quaternary ammonium salt type cationic monomer. Background technique [0002] Quaternary ammonium salt-type cationic monomers (such as acryloyloxyethyltrimethylammonium chloride, methacryloyloxyethyltrimethylammonium chloride) are one of the key raw materials for the synthesis of cationic polyacrylamide, and are widely used in Synthetic water treatment flocculants have important uses in environmental protection, papermaking, oil recovery, soil improvement, etc. [0003] The synthesis reaction of the quaternary ammonium cationic monomer can be carried out in a reactor, using water as a solvent, adding the unsaturated tertiary amine as the reaction raw material to the reactor at one time, and then continuously adding halogenated hydrocarbons to remove the heat of reaction while reacting , so as to obtain the aqueous solu...

Claims

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Application Information

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IPC IPC(8): C07C219/08C07C213/02C07C213/10
Inventor 杨青波马国林金丰富
Owner 浙江友联化学工业有限公司
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