反応 #162259
ord-ca6eee362d3d46539288822cee8c8317
反応条件
後処理
- 1その他In a 10 liter flask equipped with a stirrer
- 2workup.ADDITIONthe obtained solution was added dropwise in a reactor over 4 hours
- 3workup.ADDITIONDuring the dropwise addition of a monomer solution
- 4その他a white precipitate was produced
- 5温度After heating
- 6温度while maintaining at 70° C.
- 7温度heating
- 8温度the reaction solution was cooled to room temperature
- 9その他The precipitate thus produced
- 10ろ過was collected by filtration under reduced pressure
- 11洗浄washed with 1,000 g of ethanol
- 12その他The precipitate was vacuum-dried at 40° C. for 24 hours
- 13その他to obtain a white fine crystal
実験手順
In a 10 liter flask equipped with a stirrer, a capacitor and a dropping device, 3,500 g of ethanol was charged and heated to 70° C. Then, 720 g (6.67 mol) of a vinylphosphonic acid monomer, 880 g (12.38 mol) of acrylamide and 52 g of AIBN were dissolved in 1,000 g of ethanol 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 ethanol. The precipitate was vacuum-dried at 40° C. for 24 hours to obtain a white fine crystal. Yield: 1,550 g