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The homophase polymerization of acrylic acid is carried out in a solution of poly(butyl acrylate) trithiocarbonate (PBATC) in a mixed solvent 2-propanol–water. The phase diagram of the three-component PBATC-2-propanol–water system at 22°C is obtained. The homophase region of the compositions of semidilute solutions is determined. The homophase polymerization of AA in the three-component system at 70°C, in which the mixed solvent with respect to PBATC is similar in thermodynamic quality to the θ-solvent at 22°, yields solutions of the narrowly dispersed block copolymer butyl acrylate–acrylic acid. The content of the block copolymer in solutions is 15–23%, the MW of the copolymer is 10–20 × 10 3 , and the polydispersity coefficient is 1.12–1.16. As evidenced by dynamic light scattering, under normal conditions, the solutions contain nanoparticles with a diameter of up to 50 nm with a narrow size distribution.

Synthesis of Narrowly Dispersed Block Copolymer of Butyl Acrylate and Acrylic Acid in a Solution Acquiring Colloidal Properties during Cooling