Preparation method for polyether alkyl hydroxyl acrylate
A technology of polyether alkyl hydroxy ester and alkyl acrylate hydroxy ester, which is applied in the field of fine chemicals, can solve the problems of limited capping rate of esterification, and achieve the effects of simple operation, less by-products and high product yield
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Embodiment 1
[0055] Clean the autoclave and fully dry it to check the airtightness of the device. Open still cover, add 150g of hydroxypropyl methacrylate, catalyst 1.3g and polymerization inhibitor 0.75g in still, tighten reaction still cover. The reactor was purged 3 times with nitrogen. Turn on the stirring and set it to 5Hz, fill the reactor with nitrogen to a gauge pressure of 0.2MPa, and then vent it, repeating this three times. Turn on high-speed stirring at 30Hz, turn on heating at 80°C, introduce ethylene oxide at a rate of 2.8g / min, control the reaction pressure to <3.5MPa, and keep the temperature in the kettle at 60±2°C. When the feeding of 765g of ethylene oxide is completed, the pressure of the kettle will not drop after 1.0h of heat preservation, and the temperature will be lowered to 30°C and vacuumed for 10min, then the material will be discharged. A transparent liquid was obtained by filtration, the yield of polyoxyethylene ether methacrylate was 96.8%, the distribution...
Embodiment 2
[0057] Clean the autoclave and fully dry it to check the airtightness of the device. Open still cover, add 150g of hydroxypropyl methacrylate, catalyst 1.3g and polymerization inhibitor 0.75g in still, tighten reaction still cover. The reactor was purged 3 times with nitrogen. Turn on the stirring and set it to 5Hz, fill the reactor with nitrogen to a gauge pressure of 0.2MPa, and then vent it, repeating this three times. Turn on high-speed stirring at 30Hz, turn on heating at 55°C, introduce ethylene oxide at a rate of 2.1g / min, control the reaction pressure to <3.5MPa, and keep the temperature in the kettle at 55±2°C. When the feeding of 765g of ethylene oxide is completed, the pressure of the kettle will not drop after 1.0h of heat preservation, and the temperature will be lowered to 30°C and vacuumed for 10min, then the material will be discharged. A transparent liquid was obtained by filtration, the yield of polyoxyethylene ether methacrylate was 96.1%, the distribution...
Embodiment 3
[0059] Clean the autoclave and fully dry it to check the airtightness of the device. Open still cover, add 150g of hydroxypropyl methacrylate, catalyst 1.3g and polymerization inhibitor 0.75g in still, tighten reaction still cover. The reactor was purged 3 times with nitrogen. Turn on the stirring and set it to 5Hz, fill the reactor with nitrogen to a gauge pressure of 0.2MPa, and then vent it, repeating this three times. Turn on high-speed stirring at 30Hz, turn on heating at 5°C, introduce ethylene oxide at a rate of 1.6g / min, control the reaction pressure to <3.5MPa, and keep the temperature in the kettle at 5-10°C. When the feeding of 765g of ethylene oxide is completed, the pressure of the kettle will not drop after 1.0 hours of heat preservation, and the material will be discharged after 10 minutes of vacuum. A transparent liquid was obtained by filtration, the yield of polyoxyethylene ether methacrylate was 95.0%, the distribution coefficient was 1.26, the color was 5...
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