反应详情

In a 300 mL three-necked flask, 2-hydroxyethyl methacrylate (HEMA, 17.1 g, 0.15 mol), acrylic acid (AA, 3.6 g, 0.05 mol), dimethyl sulfoxide (48.4 g) and a polymerization initiator VA-061 (Wako Pure Chemical Industries, Ltd., 0.0310 g, 0.124 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 30% 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 60° C. for 0.5 hours, followed by temperature rise to 70° C. and further stirring for 4.5 hours. After completion of the polymerization, the polymerization reaction solution was cooled to room temperature and 100 mL of ethanol was added, and then the mixed solution was poured into 500 mL of water and left to stand overnight. On the next day, the supernatant was discarded and the obtained solid component was further washed twice with 500 mL of water. 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: 61 kD, Mw: 267 kD (Mw/Mn=4.4).

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 4.5 hours
5. customAfter completion of the polymerization
6. customthe polymerization reaction solution
7. waitleft
8. waitto stand overnight
9. washthe obtained solid component was further washed twice with 500 mL of water
10. customThe solid component was dried overnight by a vacuum
11. customdrying oven at 60° C
12. additionLiquid nitrogen was charged
13. customthe solid component was crushed by a spatula
14. customdried by a vacuum
15. customdrying oven at 60° C. for 3 hours