Hydrogen (H) as a fuel source presents a promising route toward decarbonization, though challenges in its storage remain significant. This study explores the synthesis and characterization of polytriphenylamine (PTPA) conjugated microporous polymers (CMPs) for H storage. Utilizing a combination of Buchwald-Hartwig (BH) coupling, the Bristol-Xi'an Jiaotong (BXJ) approach, and variations in monomer reactive site stoichiometry, a polymer with specific surface areas in excess of 1150 m g and micropore volume of 0.47 cm g is developed. H storage capacities are measured, achieving excess gravimetric uptakes of 1.65 wt.% at 1 bar and 2.51 wt.% at 50 bar and 77 K, with total capacities reaching 4.40 wt.% at 100 bar and 77 K. Net adsorption isotherms reveal advantages to H storage using PTPA adsorbents over traditional compression up to pressures of 10 bar at 77 K. High mass transfer coefficients of 4.95 min indicate a strong material affinity for H. This study highlights the impact of monomer ratio adjustments on the porosity and excess, total, and net H adsorption capacities of PTPA-based CMPs, offering insights into the importance of a non-stoichiometric monomer concentration when developing efficient CMP-based H storage materials.
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