反应详情

Zinc methacrylate (848 mg, 3.6 mmol), ethylene glycol dimethacrylate (678 ml, 3.6 mmol) and the radical initiator VAZO® (1,1′-azobis(cyclohexanecarbonitrile), Aldrich) (20 mg, 0.08 mmol) were dissolved in dimethylformamide (15 ml) in a borosilicate test tube. The solution was sonicated for 1 min and sparged with nitrogen. The test tube was covered with parafilm. The reaction mixture was stirred and placed in an oil bath which was then heated slowly over 1.5 hrs to 95° C. When the reaction mixture reached a temperature of 85° C., a precipitate started to form. Heating was continued for a total of 6 hrs and the polymer was left at room temperature overnight. The white polymer particles were filtered off and extracted with methanol in a Soxhlet apparatus for 8 hrs. The fines were removed by suspending particles in water and discarding the supernatant. This step was repeated until the supernatant was clear. The remaining polymer was filtered off and rinsed with methanol. The polymer was left to dry for 2 hours at room temperature, followed by overnight drying at 140° C.

1. customThe solution was sonicated for 1 min
2. customsparged with nitrogen
3. customplaced in an oil bath
4. temperaturewhich was then heated slowly over 1.5 hrs to 95° C
5. customa temperature of 85° C.
6. customto form
7. temperatureHeating
8. customwas continued for a total of 6 hrs
9. filtrationThe white polymer particles were filtered off
10. extractionextracted with methanol in a Soxhlet apparatus for 8 hrs
11. customThe fines were removed
12. filtrationThe remaining polymer was filtered off
13. washrinsed with methanol
14. waitThe polymer was left
15. customto dry for 2 hours at room temperature
16. waitfollowed by overnight
17. customdrying at 140° C.