反应详情

温度

70 °C

In a 10 liter flask equipped with a stirrer, a capacitor and a dropping device, 3,500 g of ethyl acetate was charged and heated to 70° C. Then, 390 g (3.61 mol) of a vinylphosphonic acid monomer, 1,243 g (14.44 mol) of methacrylic acid and 52 g of AIBN were dissolved in 1,000 g of ethyl acetate and the obtained solution was added dropwise in a reactor over 4 hours. During the dropwise addition of a monomer solution, a white precipitate was produced. After heating and stirring for 2 hours while maintaining at 70° C., heating was stopped and the reaction solution was cooled to room temperature. The precipitate thus produced was collected by filtration under reduced pressure and then washed with 1,000 g of ethyl acetate. The precipitate was vacuum-dried at 40° C. for 24 hours to obtain a white fine crystal. Yield: 1,550 g

1. customIn a 10 liter flask equipped with a stirrer
2. additionthe obtained solution was added dropwise in a reactor over 4 hours
3. additionDuring the dropwise addition of a monomer solution
4. customa white precipitate was produced
5. temperatureAfter heating
6. temperaturewhile maintaining at 70° C.
7. temperatureheating
8. temperaturethe reaction solution was cooled to room temperature
9. customThe precipitate thus produced
10. filtrationwas collected by filtration under reduced pressure
11. washwashed with 1,000 g of ethyl acetate
12. customThe precipitate was vacuum-dried at 40° C. for 24 hours
13. customto obtain a white fine crystal