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Method for preparing (methyl) crylic acid hydroxyalkyl ester

A technology of hydroxyalkyl acrylate and manufacturing method, which is applied in the direction of reaction preparation of ester group and hydroxyl group, preparation of carboxylate, chemical instruments and methods, etc., can solve problems such as easy gelation, and achieve high-purity effect

Active Publication Date: 2012-03-14
RESONAC CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it has recently been clarified that this method tends to tend to gel in the reaction system

Method used

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  • Method for preparing (methyl) crylic acid hydroxyalkyl ester
  • Method for preparing (methyl) crylic acid hydroxyalkyl ester

Examples

Experimental program
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Effect test

manufacture example 1

[0058] (Synthesis of Vinyloxybutyl Methacrylate)

[0059] Add 1000 g of 4-hydroxybutyl vinyl ether (manufactured by Maruzen Petrochemical Co., Ltd. HBVE), 3000 g of methyl methacrylate, and 0.65 g of p-methoxyphenol into a 4 L four-necked round-bottom detachable flask, and install a rectification column ( 15 segments), mixer, air inlet tube, thermometer. Under stirring, start heating while introducing dry air at a rate of 100ml / min, adjust the pressure to about 40kPa so that the liquid temperature in the flask is 75°C during reflux, and remove the moisture in the system. After confirming that the water content in the system was 300 ppm or less, 8.6 g of titanium tetraisopropoxide was added as a catalyst, and the pressure in the flask was controlled to about 60 kPa so that the reaction temperature was 95±5°C. When heating to reflux, monitor the temperature of the upper part of the rectification column (column top temperature). Since it is close to the azeotropic temperature of...

Embodiment 1

[0061] (Synthesis of 4-hydroxybutyl methacrylate using ethylene glycol)

[0062] 2.5 g of p-toluenesulfonic acid and 101 g of ethylene glycol were charged into a 1 L four-necked separable flask, and a stirrer, a thermometer, an air introduction tube, and a vacuum pump with a cold trap were installed. While stirring, 250 g of vinyloxybutyl methacrylate synthesized in Production Example 1 was gradually added, and the liquid temperature was adjusted to maintain at 40°C. After the addition, the pressure was reduced to 30 kPa, and the stirring was continued for 1 hour while introducing dry air at a rate of 100 ml / min. Then, the reaction liquid was analyzed by gas chromatography, and no vinyloxybutyl methacrylate peak was found. However, in the analysis by liquid chromatography, it was confirmed that 14.4% of acetal dimers were produced, so 25.2 g of ethylene glycol was added and the pressure was set at 5 kPa to perform deacetalization reaction. Analysis was carried out after 2 hou...

Embodiment 2

[0064] (Synthesis of 4-hydroxybutyl methacrylate using propylene glycol)

[0065] 2.5 g of p-toluenesulfonic acid and 124 g of propylene glycol were charged into a 1 L four-necked detachable flask, and a stirrer, a thermometer, an air inlet tube, and a vacuum pump with a cooling trap were installed. While stirring, 250 g of vinyloxybutyl methacrylate synthesized in Production Example 1 was gradually added, and the liquid temperature was adjusted to maintain at 40°C. After the addition, the pressure was reduced to 30 kPa, and the stirring was continued for 1 hour while introducing dry air at a rate of 100 ml / min. Then, the reaction liquid was analyzed by gas chromatography, and no vinyloxybutyl methacrylate peak was found. However, in the analysis by liquid chromatography, it was confirmed that 16.2% of acetal dimers were produced, so 31 g of propylene glycol was added and the deacetalization reaction was carried out at a pressure of 5 kPa. Analysis was carried out after 2 hou...

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Abstract

The present invention relates to a method for effectively preparing (methyl) crylic acid hydroxyalkyl ester of high purity without complicated refining processes. The method for preparing (methyl) crylic acid hydroxyalkyl ester is characterized in that through an ester exchange method, alcohol (methyl) propylene containing vinyl ether is acidated to obtain (methyl) crylic acid hydroxyalkyl ester containing vinyl ether, and the vinylation removing reaction is carried out under the presence of acid catalyst and diol, then diol is further added to carry out acetalation removing reaction.

Description

technical field [0001] The present invention relates to a method for producing hydroxyalkyl (meth)acrylates using vinyl ether-containing alcohols. Background technique [0002] As a method for producing hydroxyalkyl (meth)acrylate, the usual mainstream method is to extract and separate only the monoester after obtaining a mixture of diol, monoester and diester from alkanediol by esterification. Specifically, a method of reacting (meth)acrylic acid and alkanediol in the presence of a strong acid is disclosed (for example, see Patent Document 1). However, this method has disadvantages such as generation of by-products due to strong acid and lower yield. As a means to solve this problem, various reports have been made about the transesterification reaction between alkane diol and (meth)acrylate (for example, refer to Patent Documents 2 to 4). In addition, methods for efficiently extracting and purifying 4-hydroxybutyl (meth)acrylate have also been reported (for example, refer ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C67/297
CPCC07C67/03C07C69/54
Inventor 龟井淳一
Owner RESONAC CORP
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