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Poly(methyl methacrylate)-b-poly(tert-butyl acrylate) (PMMA-b-PtBA) block copolymers were prepared based on the new mechanism of 1,1-diphenylethylene (DPE) controlled radical polymerization in homogeneous systems. Firstly, monomer methyl methacrylate (MMA), initiator 2,2-azobisisoheptonitrile (ABVN) and a control agent DPE were solution polymerized to form DPE-containingPMMAprecursor. Then the second monomer tert-butyl acrylate (tBA) was simply heated in the presence of DPE-containing PMMA precursor used as macroinitiator, and block copolymers were synthesized successfully. The effects of polymerization temperature and solvent on molecular weight and molecular weight distribution of polymers throughout the polymerization were investigated. DPE-containing poly(styrene) precursor could not induce block polymerization.
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