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Quaternarization method of (dialkyl) aminoethyl methacrylate

A technology of dialkylaminoethyl methacrylate and dialkylaminoethyl acrylate, which is applied in the field of chemical products, can solve problems such as high operating costs, inflammability and explosion, and large investment, and achieve easy industrial production and safe High performance and easy control

Inactive Publication Date: 2011-08-17
烟台浩昇投资有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Organic solvents such as acetonitrile, acetone, and ether are extremely volatile, flammable and explosive. For the industrial scale preparation of quaternary ammonium salts of dialkylaminoethyl (meth)acrylates, a large amount of investment is required for safety protection, and the operating cost is high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a 1000-liter pressure-resistant reactor, add 500Kg (9.90 kilomoles) of methyl chloride, and slowly raise the temperature to 36-38°C under stirring. Then in reactor, measure and add the dimethylaminoethyl methacrylate that contains polymerization inhibitor hydroquinone 1000ppm, add up to 157.21Kg (1.0 kilomoles), add in 1 hour, carry out heating and cooling by reactor jacket, Maintain the temperature in the kettle at 36-38°C and stir for 2 hours.

[0021] After cooling, the material is filtered through a closed filter. The solid crystal is the quaternary ammonium salt of dimethylaminoethyl methacrylate. After collection, it is dried under reduced pressure and low temperature to obtain the finished product. Excessive methyl chloride exists in the filtrate, a part of the methyl chloride is vaporized, and after recovery by freezing, it can be recycled for quaternization reaction.

Embodiment 2

[0023] In a 1000-liter pressure-resistant reactor, add 500Kg (7.75 kilomoles) of monochloroethane, and slowly raise the temperature to 35-38°C under stirring. Then metered into the reactor containing the dimethylaminoethyl acrylate of polymerization inhibitor hydroquinone 2000ppm, a total of 143.18Kg (1.0 kilomoles), added in 1 hour, heated and cooled by the reactor jacket, maintained the reactor The inner temperature was 35-38°C, and stirred for 2 hours.

[0024] After cooling, the material is filtered through a closed filter. The solid crystal is the quaternary ammonium salt of dimethylaminoethyl acrylate. After collection, it is dried at low temperature to obtain the finished product. Excess monochloroethane exists in the filtrate, and a part of monochloroethane vaporizes, and after freezing and recovery, it can be recycled for quaternization reaction.

Embodiment 3

[0026] In a 1000-liter pressure-resistant reactor, add 420Kg of recovered monochloroethane in Example 2, supplement 100Kg of fresh monochloroethane, and slowly heat up to 36-39° C. under stirring. Then in reactor, measure and add the dimethylaminoethyl acrylate that contains polymerization inhibitor tert-butylhydroquinone 1000ppm, add up to 143.18Kg, add in 1 hour, carry out heating and cooling by reactor jacket, maintain the temperature in the still 36-39°C, stirring for 2 hours.

[0027] After the reaction is completed, the material is filtered through a closed filter, and the solid crystal is the quaternary ammonium salt of dimethylaminoethyl acrylate, which is collected and dried at low temperature to obtain the finished product. Excess monochloroethane exists in the filtrate, and a part of monochloroethane vaporizes, and after freezing and recovery, it can be recycled for quaternization reaction.

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PUM

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Abstract

The invention relates to a quaternarization method of (dialkyl) aminoethyl methacrylate, belonging to the field of chemical products. The quaternarization method of (dialkyl) aminoethyl methacrylate comprises the following steps of: (1) adding halogenated hydrocarbon in a pressure reaction kettle; (2) adding (dialkyl) aminoethyl methacrylate of a polymerization inhibitor in the pressure reaction kettle at 20-40 DEG C and stirring for reacting, wherein (dialkyl) dimethylaminoethyl methacrylate contains 300-3000ppm of polymerization inhibitor, and the mole ratio of halogenated hydrocarbon to (dialkyl) aminoethyl methacrylate in the reaction is (2-20):1; (3) after the reaction is finished, cooling, filtering and separating, drying at low temperature to obtain the quaternary ammonium salt of dialkyl aminoethyl methacrylate; and (4) freezing the filtrate for recycling, wherein the main component of the filtrate is halogenated hydrocarbon which can be reused in the reaction process of the method. The quaternarization method of (dialkyl) aminoethyl methacrylate has the advantages of simple reaction process, easiness for control and high safety, can be used for producing solid products and is easy for industrial production.

Description

1. Technical field [0001] The invention relates to a method for quaternizing dialkylaminoethyl (meth)acrylate, which belongs to the field of chemical products. 2. Background technology [0002] Dialkylaminoethyl acrylate and quaternary ammonium salt of dialkylaminoethyl methacrylate are unsaturated cationic monomers and one of the key raw materials for cationic polyacrylamide. They are widely used in environmental protection, papermaking, oil recovery, and soil improvement. etc. have important uses. [0003] The manufacture method of the unsaturated quaternary ammonium salt described in Chinese patent CN1174188, CN1337936, CN1296942, CN1337935, CN1384095 etc., is to carry out in aqueous solution. Due to the quaternization reagent chlorinated hydrocarbons such as methyl chloride, the solubility in water is very small, the reaction equipment needs intensive stirring, and the reaction speed is slow. The final product of the reaction is in the form of an aqueous solution. Bec...

Claims

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Application Information

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IPC IPC(8): C07C219/08C07C213/08
Inventor 鲁钟钧刘福胜
Owner 烟台浩昇投资有限公司
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