反应详情

The methyl methacrylate-n-butyl acrylate diblock copolymer (150 g) was dissolved into 240 mL of toluene and placed into a 1 L reactor equipped with an agitator, a thermometer, a nitrogen gas inlet tube, a dropping funnel, and a reflux condenser. In a nitrogen atmosphere, 15 g of n-butylamine as a primary amine compound and 9 g of bis(2,2,6,6,-tetramethyl-4-piperidyl)sebacate as a HALS were added into the reactor, and stirring was performed at 50° C. for 5 hours. 1H NMR measurement and IR measurement confirmed that the thiocarbonylthio groups were converted into mercapto groups at a yield of 91%. The toluene solution of the polymer was poured into 1 L of methanol to precipitate the polymer, followed by filtration, washing with methanol, and drying. Next, the polymer was dissolved into 240 mL of toluene, and 264 mg of dichloride succinate as a polyvalent acyl halide used in method (vii) was added thereinto, followed by stirring at 60° C. for 6 hours. 1H NMR and GPC measurement confirmed that the mercapto groups were coupled at a yield of 94% by acylation. In the resultant methyl methacrylate-n-butyl acrylate-methyl methacrylate triblock copolymer, Mn=85,200 and Mw/Mn=1.66. The weight ratio of the individual constituents was the same as that before the coupling reaction.

1. customplaced into a 1 L reactor
2. customequipped with an agitator
3. customto precipitate the polymer
4. filtrationfollowed by filtration
5. washwashing with methanol
6. customdrying
7. dissolutionNext, the polymer was dissolved into 240 mL of toluene, and 264 mg of dichloride succinate as a polyvalent acyl halide
8. additionwas added
9. stirringby stirring at 60° C. for 6 hours
10. custombefore the coupling reaction