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Pre-oxidized acrylic fiber (POAF) and ferric sulfophenyl phosphate (FeSPP) are incorporated into polybenzimidazole (PBI) membrane for the first time to prepare high-temperature proton exchange membranes (PEMs). The strong hydrogen bonds formed between PBI/POAF and FeSPP lead to good dispersion of POAF and FeSPP, facilitate the construction of proton channels, and enhance the dimensional and mechanical stability of the membranes. PBI/FeSPP (30 wt%) shows good proton conductivity (5.43 × 10 −2 and 4.13 × 10 −2 S cm −1 at 180 °C at 50% and 0 relative humidity (RH), respectively) and improved dimensional and mechanical stability compared with pristine PBI. By incorporating 5 wt% POAF into PBI/FeSPP (30 wt%), the swelling ratios are halved and the mechanical strength is enhanced by almost 30% while the proton conductivity is slightly affected (3.84 × 10 −2 and 2.97 × 10 −2 S cm −1 at 180 °C at 50% and 0 RH for PBI/FeSPP (30 wt%)/POAF (5 wt%), respectively). This work offers a new route in the preparation of high-temperature PEMs with enhanced properties.

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