Unannealed CuNiMoP electrocatalyst was found active in electrochemical oxidation of glycerol, providing over 60% conversion without optimization. Prompted by this result, the same catalyst was investigated for the thermochemical oxidation of glycerol. For the thermochemical oxidation of glycerol using the as-deposited electroless CuNiMoP catalyst, a 2 3 full factorial design of experiments (two level factorial experiment design with three factors) to assess the influence of temperature (A), reaction time (B) and pressure (C). The major reaction products detected by high performance liquid chromatography (HPLC) were glyceric, hydroxypyruvic, tartronic, oxalic and formic acids. The factors found to be most significant for the production of glyceric and tartronic acids were A, B, C, AB and BC. The highest percent conversion obtained for 30-min and 60-min catalysts was 10.6% and 9.4%, respectively. The presence of lactic acid was observed only for the 60-min as-deposited electroless CuNiMoP/Al 2 O 3 catalyst. The results suggest the feasibility of an inexpensive catalyst based on non-noble metals for the thermochemical oxidation of glycerol through the electroless deposition technique. Some differences exist between the thermochemical and electrochemical product selectivity of the CuNiMoP catalyst, and reasons are suggested for the observed differences.

Interest in glycerol oxidation to more useful products has risen significantly over the years. This has led to the development of several catalysts some of which are scarce, uneconomical and environmentally unfriendly. In this research, two catalysts prepared from red earth - ‘A1’ (calcined at 500°c) and ‘A2’ (calcined at 500°c and dealuminated) were characterized using x-ray fluorescence (XRF) and used to oxidize glycerol with O2 molecules for 240 mins. The XRF results showed that Al2O3 (31.3%), SiO2 (47.9%) and Fe2O3 (16.05%) were the predominant components in ‘A1’ while ‘A2’ showed a marked significant difference in Al2O3 (19.4%), SiO2 (72.1 %) and Fe2O3 (0 %). The selectivities of the oxidation products with A1 were 18.8 % glyceric acid (GLA), 13.1 % lactic acid (LCA), 1.66 % oxalic acid (OXA) and 1.24 % formic acid (FMA), while for A2 they were (20.4%) GLA and (17%) LCA. 88.1% glycerol was converted but selectivity towards any of the products was low.