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In the present work, a block copolymer with hydrophilic alkyl sulfonated side groups and hydrophobic flexible alkyl ether side groups, poly(5\u2019\u2010hexyloxy\u20101\u2019,4\u2010biphenyl)\u2010<jats:italic>b<\/jats:italic>\u2010poly(2\u2019,4\u2019\u2010bispropoxysulfonate\u20101\u2019,4\u2010biphenyl) (HBP\u2010<jats:italic>b<\/jats:italic>\u2010<jats:italic>x<\/jats:italic>BPSBP), is designed and synthesized by copolymerization of the hydrophilic and hydrophobic oligomers. The oligomers are synthesized via a Pd\u2010catalyzed Suzuki cross\u2010coupling of 1,3\u2010dibromo\u20105\u2010hexyloxybenzene, and 3,3\u2019\u2010[(4,6\u2010dibromo\u20101,3\u2010phenylene)bis(oxy)]bis(propane\u20101\u2010sulfonate) or 1,4\u2010bis(4,4,5,5\u2010tetramethyl\u20101,3,2\u2010dioxaborolan\u20102\u2010yl)benzene. The good solubility and film\u2010forming characteristics are achieved via the introduction of flexible hexyloxy side groups, and high ion exchange capacity (IEC) is achieved via the introduction of high density of alkyl sulfonated side groups. The HBP\u2010<jats:italic>b<\/jats:italic>\u20100.5BPSBP has the highest IEC of 3.17\u2005mmol\/g, the highest proton conductivity of 43.5\u2005mS\/cm at 95\u2009\u00b0C and 90% relative humidity (RH) and low methanol permeability of 6.45\u00d710<jats:sup>\u22127<\/jats:sup>\u2005cm<jats:sup>2<\/jats:sup>\/s. Meanwhile, crosslinked HBP\u2010<jats:italic>b<\/jats:italic>\u2010<jats:italic>x<\/jats:italic>BPSBP exhibits promising water uptake, swelling ratio and low methanol permeability. These characteristics are attributed to the crosslinked structure and the hydrophilic\/hydrophobic nanophase separation morphology promoted by the poly(<jats:italic>m<\/jats:italic>\u2010phenylene) main chains, flexible alkyl ether groups, and alkyl sulfonated side groups.<\/jats:p>","DOI":"10.1002\/asia.202200109","type":"journal-article","created":{"date-parts":[[2022,3,21]],"date-time":"2022-03-21T13:48:42Z","timestamp":1647870522000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["Synthesis and Characterization of Poly(5\u2019\u2010hexyloxy\u20101\u2019,4\u2010biphenyl)\u2010<i>b<\/i>\u2010poly(2\u2019,4\u2019\u2010bispropoxysulfonate\u20101\u2019,4\u2010biphenyl) with High Ion Exchange Capacity for Proton Exchange Membrane Fuel Cell Applications"],"prefix":"10.1002","volume":"17","author":[{"given":"Kunyu","family":"Jin","sequence":"first","affiliation":[{"name":"Department of Chemistry Shanghai University  99 Shangda Road 200444 Shanghai P.\u2005R. 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