反应详情

In a 500 mL three-necked flask, N-vinylpyrrolidone (NVP, 90.02 g, 0.81 mol), acrylic acid (6.49 g, 0.09 mol), dimethyl sulfoxide (386.8 g), a polymerization initiator VA-061 (Wako Pure Chemical Industries, Ltd., 0.1408 g, 0.562 mmol) and 2-mercaptoethanol (2-ME, 43.8 μL, 0.63 mmol) were charged, and then equipped with a three-way stop-cock, a reflux condenser tube, a thermometer and a mechanical stirrer. The concentration of the monomer was 20% by weight. After degassing inside the three-necked flask using a vacuum pump and repeating replacement by argon three times, stirring was carried out at 50° C. for 0.5 hours, followed by temperature rise to 70° C. and further stirring for 6.5 hours. After completion of the polymerization, the polymerization reaction solution was cooled to room temperature and 100 mL of water was added, and then the solution was poured into 500 mL of acetone and the mixed solution was left to stand overnight. On the next day, 200 mL of acetone was further added and 100 mL of hexane was added, and then the supernatant was removed by decantation. The obtained solid component was washed seven times with acetone/water (=500 mL/100 mL). The solid component was dried overnight by a vacuum drying oven at 60° C. Liquid nitrogen was charged and the solid component was crushed by a spatula, and then dried by a vacuum drying oven at 60° C. for 3 hours. The thus obtained copolymer had a molecular weight of Mn: 35 kD, Mw: 130 kD (Mw/Mn=3.8).

1. customequipped with a three-way
2. customAfter degassing inside the three-necked flask
3. customfollowed by temperature rise to 70° C.
4. stirringfurther stirring for 6.5 hours
5. customAfter completion of the polymerization
6. customthe polymerization reaction solution
7. waitthe mixed solution was left
8. waitto stand overnight
9. customthe supernatant was removed by decantation
10. washThe obtained solid component was washed seven times with acetone/water (=500 mL/100 mL)
11. customThe solid component was dried overnight by a vacuum
12. customdrying oven at 60° C
13. additionLiquid nitrogen was charged
14. customthe solid component was crushed by a spatula
15. customdried by a vacuum
16. customdrying oven at 60° C. for 3 hours