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Electrochemical methanol reformation (ECMR) method has been identified as one of the most effective method for on-site hydrogen production. However, concentrated research towards the development of efficient inexpensive hydrogen evolution reaction (HER) electrocatalyst holds the pivotal role in realizing the hydrogen economy. In this context, for the first time N-graphene supported Pd (Pd/NG) was synthesised and employed as an HER catalyst in ECMR process. N-graphene was synthesised by modified Hummer's method followed by Pd deposition through hydrothermal route. The electrocatalytic activity of Pd/NG for hydrogen evolution was evaluated by CV and LSV techniques. Tafel slope of Pd/NG and Pt/C was calculated from LSV curves and was found to be 33 and 31 mV/decade, respectively. Exchange current density was found to be 3.6 and 3.2 × 10−4 A cm−2 for Pd and Pt catalysts, respectively. The enhanced electrocatalytic activity is majorly attributed to the N-doping and uniform distribution of Pd nano particles on graphene. Further, the performance of Pd/NG was also evaluated in single ECMR cell using Pt–Ru/C at anode and Pd/NG at cathode as electrocatalysts. The results indicated the suitability of Pd/NG as cathode electrocatalyst for HER in ECMR process.

Polymer electrolyte membrane (PEM)-based electrochemical methanol reformation has gained interest as a practical way to produce hydrogen than water electrolysis due to its low operating voltages. Development of alternative PEM for this application is of considerable interest in order to reduce the cost as well as increase the system efficiency. Presently, a novel SPVDF/ZrP composite membrane was synthesized as proton exchange membrane for hydrogen production using electrochemical methanol reformation (ECMR). PVDF-co-HFP granules were defluorinated by alkali treatment followed by sulfonation using chlorosulfonic acid to prepare sulfonated polymer. Inorganic zirconium phosphate (ZrP) was further added to increase proton conductivity. The membranes were characterized for their physicochemical properties, mechanical strength, and thermal stability. The enhancement in proton exchange capacity and water uptake with adequate dimensional stability was observed with dehydrofluorination and impregnation of ZrP. A novel electrolyzer consisting of Pt-Ru/C as anode electrode, same format as anode as cathode electrode and the SPVDF/ZrP composite membrane was assembled and its performance was tested for hydrogen production. It was found that SPVDF/ZrP composite membrane showed good electrochemical cell performance of 0.65 V at 0.15 A cm−2 current density at ambient temperature and gives scope for operating ECMR cell at higher current densities for to increase the hydrogen production rate which is comparable to the performance of commercial Nafion® 117 membrane.