Synthesis of well‐defined amphiphilic polymethylene‐b‐poly(ε‐caprolactone)‐b‐poly(acrylic acid) triblock copolymer via a combination of polyhomologation,ring‐opening polymerization,and atom transfer radical polymerization |
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Authors: | Cong Yuan Hui‐Chao Lu Qi‐Zheng Li Sen Yang Qiao‐Ling Zhao Jin Huang Liu‐He Wei Zhi Ma |
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Institution: | 1. Shanghai Institute of Organic Chemistry, Chinese Academy of Sciences, Shanghai 200032, People's Republic of China;2. Department of Chemistry, Zhengzhou University, Zhengzhou 450001, People's Republic of China |
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Abstract: | Well‐defined amphiphilic polymethylene‐b‐poly(ε‐caprolactone)‐b‐poly(acrylic acid) (PM‐b‐PCL‐b‐PAA) triblock copolymers were synthesized via a combination of polyhomologation, ring‐opening polymerization (ROP), and atom transfer radical polymerization (ATRP). First, hydroxyl‐terminated polymethylenes (PM‐OH; Mn = 1100 g mol?1; Mw/Mn = 1.09) were produced by polyhomologation followed by oxidation. Then, the PM‐b‐PCL (Mn = 10,000 g mol?1; Mw/Mn = 1.27) diblock copolymers were synthesized via ROP of ε‐caprolactone using PM‐OH as macroinitiator and stannous octanoate (Sn(Oct)2) as a catalyst. Subsequently, the macroinitiator transformed from PM‐b‐PCL in high conversion initiated ATRPs of tert‐butyl acrylate (tBA) to construct PM‐b‐PCL‐b‐PtBA triblock copolymers (Mn = 11,000–14,000 g mol?1; Mw/Mn = 1.24–1.26). Finally, the PM‐b‐PCL‐b‐PAA triblock copolymers were obtained via the hydrolysis of the PtBA segment in PM‐b‐PCL‐b‐PtBA triblock copolymers. The chain structures of all the polymers were characterized by gel permeation chromatography, proton nuclear magnetic resonance, and Fourier transform infrared spectroscopy. Porous films of such triblock copolymers were fabricated by static breath‐figure method and observed by scanning electron microscope. The aggregates of PM‐b‐PCL‐b‐PAA triblock copolymer were studied by transmission electron microscope. © 2012 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2012 |
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Keywords: | atom transfer radical polymerization (ATRP) block copolymers micelles polyhomologation polyolefins porous film ring‐opening polymerization triblock copolymers |
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