Ammonia → alpha-Methylene-gamma-Butyrolactone Butadiene Acrylic Acid

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反応手順

A 150 mL round bottom flask with a magnetic stir bar is charged with 17 g (0.943 mol) of water, 0.01 g (6.49×10−5 mol) of sodium hydroxymethylsulfinate and 0.001 g (2.63×10−6 mol) of tetrasodium ethylene diamine tetraacetate. The reactor is heated to 80° C. under nitrogen. After 5 minutes at 80° C., 8 g of a monomer pre-emulsion consisting of 26.5 g (0.490 mol) of butadiene, 18.5 g (0.189 mol) of α-methylene-γ-butyrolactone, 1.5 g (2.50×10−2 mol) of acrylic acid, 1.332 g (3.82×10−3 mol) of sodium dodecyl benzenesulfonate (15% aqueous solution), 0.25 g (1.24×10−3 mol) of tert-dodecylmercaptan and 22 g (1.22 mol) of water is added by cannula over 3 minutes. Additionally, 1 g of an aqueous mixture consisting of 0.25 g (4.20×10−3 mol) of sodium persulfate and 7 g (0.389 mol) of water is added over 2 minutes. After stirring for 20 minutes at 80° C., the remainder of the monomer pre-emulsion and aqueous mixture is added uniformly over 300 minutes. When all additions were completed, the polymerization is allowed to stir for an additional 7 hours at 80° C. Upon completion, steam is passed through the mixture under reduced pressure and a solution of 0.25 g (1.62×10−3 mol) of sodium hydroxymethylsulfinate in 1 g (5.55×10−2 mol) of water is added slowly, with stirring. The pH of the dispersion is brought to 7 with 10% strength aqueous ammonia before the dispersion is dried under vacuum at elevated temperature for isolation.

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