Preparation method of dimethylaminoethyl acrylate and catalyst thereof

A technology of dimethylaminoethyl acrylate and methyl acrylate, applied in the field of preparation method of dimethylaminoethyl acrylate and its catalyst, to achieve high activity, convenient continuous operation and high selectivity

Inactive Publication Date: 2016-02-17
ZHEJIANG SATELLITE PETRO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] In U.S. Patent No. 8,067,633, an improved titanate catalyst is generated by the reaction of titanate and polyhydric alcohol in cyclohexane, which is used to prepare dimethylaminoethyl acrylate. Although no solid precipitation occurs during the reaction, there will still be Introduce impurities such as ethanol, isopropanol or butanol and by-products of the reaction of these alcoholic impurities with acrylates

Method used

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  • Preparation method of dimethylaminoethyl acrylate and catalyst thereof
  • Preparation method of dimethylaminoethyl acrylate and catalyst thereof

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Experimental program
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Effect test

Embodiment 1

[0040] In a reactor with a packing rectification column and agitator, add a mixture of 260g dimethylaminoethanol, 80g tetraisopropyl titanate and 8.3g ethylene glycol and heat it to reflux, and the formed isopropanol is refined The distillation tower was discharged continuously, and 65g of isopropanol distillate was obtained in 5 hours, and finally 279g of orange liquid product was obtained, which was directly used as a transesterification catalyst, and it consisted of 81.4g of catalyst and 197.6g of dimethylaminoethanol.

Embodiment 2

[0042] Add the catalyst solution of 145g dimethylaminoethanol, 516g methyl acrylate, 48g embodiment 1 (wherein containing catalyzer 14g, the quality of catalyzer is 2% of reaction raw material gross mass) , 1.4g phenothiazine and 0.17g tris-(2,2,6,6-tetramethylpiperidinyl nitroxide free radical) phosphite, stirred, heated to 83~110°C, the temperature at the top of the rectifying column was 62 At ~64°C, methanol is generated during the reaction, which forms an azeotrope with methyl acrylate and is removed. Add dropwise 50g of methyl acrylate solution containing 1% p-hydroxyanisole in the condenser at the top of the rectification column to stabilize the material in the cold rectification column. The conversion rate was monitored by gas chromatographic analysis of the reaction solution in the reaction bottle, and the conversion rate of dimethylaminoethanol reached 94.5% after the transesterification reaction time was 6 hours. After the reaction is completed, lower the temperatur...

Embodiment 3

[0047] Add the catalyst solution of 162g dimethylaminoethanol, 516g methyl acrylate, 24g embodiment 1 (wherein containing catalyst 7g, the quality of catalyst is 1% of reaction raw material gross mass) , 1.4g phenothiazine and 0.17g tris-(2,2,6,6-tetramethylpiperidinyl nitroxide free radical) phosphite, stirred, heated to 83~110°C, the temperature at the top of the rectifying column was 62 At ~64°C, methanol is generated during the reaction, which forms an azeotrope with methyl acrylate and is removed. Add dropwise 50g of methyl acrylate solution containing 1% p-hydroxyanisole in the condenser at the top of the rectification column to stabilize the material in the cold rectification column. The conversion rate was monitored by gas chromatographic analysis of the reaction liquid in the reaction bottle, and the conversion rate of dimethylaminoethanol was 89.0% after the transesterification reaction time was 6 hours. After the reaction is completed, lower the temperature, adjust...

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Abstract

The invention discloses a preparation method of dimethylaminoethyl acrylate and a catalyst thereof. Methyl acrylate and dimethylamino ethyl alcohol are used as raw materials, in a condition that a prepared modified catalyst and a polymerization inhibitor exist, a interesterification process is carried out, methanol generated from the reaction is timely removed by azeotropic distillation, obtained reaction products containing dimethylaminoethyl acrylate are distilled in a pressure reduction condition, and the dimethylaminoethyl acrylate product is obtained. The catalyst for the interesterification process is a titanate modified catalyst, and has high catalytic activity and good dissolvability; deposition does not generate in the reaction process, new impurities are not introduced, scale does not generate on the reactor wall, and the catalyst can be reused.

Description

technical field [0001] The invention belongs to the technical field of acrylate synthesis, and in particular relates to a preparation method of dimethylaminoethyl acrylate and a catalyst thereof. Background technique [0002] Dimethylaminoethyl acrylate is a multi-functional active monomer. Because it has reactive amino groups and polymerizable vinyl groups, it has the characteristics of olefins, amines, and esters. It can undergo quaternization and polymerization under certain conditions. , addition and hydrolysis and other chemical reactions, dimethylaminoethyl acrylate is an important raw material for the manufacture of quaternary ammonium cationic polymer flocculants, so it is widely used in water treatment, papermaking and other fields, and is also used in light-cured coatings, rubber, Preparation of plastics, surfactants, fibers, pharmaceuticals, cosmetic additives, and drug coating films for contact lenses. [0003] At present, the synthetic methods of dimethylaminoe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C219/06C07C213/06C07C213/10B01J21/06
Inventor 杨青波马国林金丰富
Owner ZHEJIANG SATELLITE PETRO CHEM CO LTD
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