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Process for producing(methyl) propenoic acid hydroxyalkyl ester

A technology of hydroxyalkyl acrylate and acrylic acid, which is applied in the field of preparation of hydroxyalkyl (meth)acrylate, and can solve problems such as quality deterioration and product purity reduction

Inactive Publication Date: 2004-01-21
NIPPON SHOKUBAI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, in any of the above-mentioned methods, as an impurity, dialkylene glycol mono(meth)acrylate (hereinafter referred to simply as "diadduct of epoxide") is likely to be used as a by-product. The product is produced, and there is a problem that the purity of the so-called product is reduced and the quality is deteriorated.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0010] The preparation method of the present invention is a preparation method for obtaining hydroxyalkyl (meth)acrylate by reacting raw material (meth)acrylic acid and epoxide in a batch manner (batch reaction) in the presence of a catalyst. And, it is characterized in that in this production method, the ratio of the total usage amount of the catalysts charged to the total usage amount of the supplied (meth)acrylic acid is defined as "catalyst concentration". Furthermore, when the value of the catalyst concentration calculated as the ratio of the total amount of catalyst used to the total supply amount of (meth)acrylic acid is defined as 1, (meth)acrylic acid and epoxide start to react in a state where the catalyst concentration exceeds 1. reaction (that is, a state where the concentration of the catalyst exceeds 1 at the start of the reaction).

[0011] In the present invention, ① in the presence of a catalyst, ② above a predetermined temperature (specifically 40° C.), ③ whe...

Embodiment 1-

[0063] 105 g of acrylic acid in the total supply of 420 g of acrylic acid, 2.10 g of chromium acetate as a catalyst, and 0.42 g of phenothiazine as a polymerization inhibitor were put into a 1 L SUS-316 autoclave with a stirrer ("relative to Chromium acetate concentration (2.0% by weight) of the amount of acrylic acid supplied" / "Chromium acetate concentration (0.5% by weight) relative to the total amount of acrylic acid supplied" = 4.0 (times)), the inside was replaced with nitrogen, and the temperature was raised to 80°C , the internal pressure is 0.1MPa. Ethylene oxide was supplied at 90g / h for 0.75 hours (67.5g), and then acrylic acid was supplied at 140g / h and ethylene oxide at 90g / h for 2.25 hours (acrylic acid 315g, ethylene oxide 202.5g), The reaction was carried out while maintaining 80°C. The reaction temperature after the completion of supply of acrylic acid and ethylene oxide was set at 80° C., and the reaction was continued until unreacted acrylic acid reached 0.1...

Embodiment 2-

[0067] 210 g of acrylic acid in the total supply of 420 g of acrylic acid, 2.10 g of chromium acetate as a catalyst, and 0.42 g of phenothiazine as a polymerization inhibitor were put into a 1 L SUS-316 autoclave with a stirrer ("relative to Chromium acetate concentration (1.0% by weight) of the amount of acrylic acid supplied" / "Chromium acetate concentration (0.5% by weight) relative to the total amount of acrylic acid supplied" = 2.0 (times)), the inside was replaced with nitrogen, and the temperature was raised to 80°C , so that the internal pressure is 0.1MPa. Ethylene oxide was supplied at 90 g / h for 1.5 hours (135 g), and then acrylic acid was supplied at 140 g / h and ethylene oxide at 90 g / h for 1.5 hours (210 g of acrylic acid, 135 g of ethylene oxide), and kept The reaction was carried out at 80°C. The reaction temperature after the completion of supply of acrylic acid and ethylene oxide was set at 80° C., and the reaction was continued until unreacted acrylic acid re...

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PUM

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Abstract

The present invention provides a novel production process for a hydroxyalkyl (meth)acrylate, in which it is possible that: in a batch reaction system, the amount of the hydroxyalkyl (meth)acrylate (which is the objective product) as produced is kept nearly on the same level as conventional and further, at the same time, there is suppressed the side production of the alkylene oxide's diaddition product (dialkylene glycol mono(meth)acrylate) that lowers the purity of the product to thus give a bad influence upon its quality. The present invention production process comprises the step of carrying out a batch reaction between (meth)acrylic acid and an alkylene oxide in the presence of a catalyst in order to produce the hydroxyalkyl (meth)acrylate; with the production process being characterized by arranging that the reaction should be initiated in a state of a catalyst concentration of more than 1, wherein the catalyst concentration is defined as the amount of the catalyst as used relative to the integrated amount of the (meth)acrylic acid as supplied and is assumed to be 1 in terms of the amount of the entire catalyst to be used relative to the amount of the entire (meth)acrylic acid to be supplied.

Description

technical field [0001] The present invention relates to a process for preparing hydroxyalkyl (meth)acrylates by reacting (meth)acrylic acid with epoxides in the presence of a catalyst. Background technique [0002] In the past, as the preparation method of (meth)acrylic acid hydroxyalkyl ester that batchwise reacts (meth)acrylic acid and epoxide, a batch of (meth)acrylic acid, epoxide and A method of reacting with a catalyst, or adding (meth)acrylic acid as a raw material and a catalyst together in a reactor, in which the epoxide is put into it successively (continuously or intermittently) at a constant or variable supply rate Methods for carrying out the reactions are conventional. In this way, because (meth)acrylic acid has a higher catalyst solubility than epoxide, and if epoxide is put into the reactor alone and heated at the initial stage, there is a danger of explosion, which requires special equipment, etc. , even in the former method of putting (meth)acrylic acid, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07B61/00C07C67/26C07C69/54
CPCC07C67/26C07C69/54
Inventor 石田德政上村政宏
Owner NIPPON SHOKUBAI CO LTD
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