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
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[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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