Method for preparing ethylidene-urea ethyl acrylate
A technology of ethylene urea ethyl acrylate and acrylic acid, applied in the field of compound synthesis, can solve the problems of high reaction yield, harmful and toxic substances, etc., and achieve the effects of cheap raw materials and high production efficiency
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Embodiment 1
[0030] 72g acrylic acid (1mol), 65g N-hydroxyethyl ethylene urea (0.5mol), 8g catalyst (a mixture of aluminum sulfate and aluminum chloride with a weight ratio of 1:1), 200ml cyclohexane, 0.2g phenothiazine (Inhibitor) into the three-necked reaction bottle with reflux condenser and oil-water separator in turn. Stir and heat to 80°C, cyclohexane starts to boil and reflux with water. Insulate and react at 80°C for 6 hours until the water output in the oil-water separator no longer increases. Release the generated water from the water separator, continue to keep warm at 80°C for 1.5hr to evaporate and recover most (about 90%) of cyclohexane about 180ml, then evaporate excess acrylic acid under reduced pressure, stop heating, and cool down the reaction system To 30-40°C, add 200ml of absolute ethanol and 10g of sodium carbonate, and stir the reaction product for 45min to remove the catalyst and residual acrylic acid. Filtrate, distill ethanol off under reduced pressure to obtain...
Embodiment 2
[0032] 46g acrylic acid (0.64mol), 65g N-hydroxyethyl ethylene urea (0.5mol), 10g catalyst (a mixture of aluminum sulfate and aluminum chloride with a weight ratio of 1:1), 60ml cyclohexane, 0.1g phenothiene Put the oxazine (polymerization inhibitor) into the reaction three-neck flask with reflux condenser and oil-water separator in turn, stir and heat to about 83°C, cyclohexane starts to boil and reflux, continuously separates water, and reacts for 8 hours until it comes out of the oil-water separator. The amount of water does not increase any more, the reaction temperature rises to about 90°C, and most (about 70%) of cyclohexane continues to be distilled off and recovered. After the same post-treatment as in Example 1, 81 g of ethylene urea ethyl acrylate was obtained, with a yield of 88% and a product purity >= 92%.
Embodiment 3
[0034] 140g acrylic acid (1.94mol), 65g hydroxyethyl ethylene urea (0.5mol), 4g catalyst (a mixture of aluminum sulfate and aluminum chloride with a weight ratio of 1 to 1), 300ml cyclohexane, 0.14g phenothiazine ( Inhibitor) was added to the reaction three-neck flask equipped with reflux condenser and oil-water separator in turn, stirred and heated to 75°C, cyclohexane began to boil and reflux to continuously separate water, and the temperature rose to about 80°C after 6 hours of reaction until oil-water separation The amount of water output in the device will not increase any more, continue to distill and recover most (about 95%) of cyclohexane. After the same post-treatment as in Example 1, 82 g of ethylene urea ethyl acrylate was obtained, with a yield of 89% and a product purity >= 95%.
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