Toluene → Methyl Methacrylate/Butyl Acrylate Methyl Methacrylate

Beteiligte Stoffe

Reaktionsschritte

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.

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