Cobalt phyllosilicate was successfully synthesised via a simple template-free sol-gel technique at room temperature. The synthesised catalyst had been characterised by various physico-chemical analyses. The X-ray diffraction (XRD) pattern confirmed the formation of phyllosilicate as supporting material. Co-O bending vibration was detected in the Fourier-transform Infrared (FTIR) spectrum. The presence of cobalt in the silica matrix was confirmed by Energy-dispersive X-ray (EDX) analysis and atomic absorption analysis (AAS analysis). The sample showed a high specific surface area with 350.3 m2 g–1 and a bimodal pore size distribution. The solvent free mineralisation of cyclohexene was carried out in the temperature range 303–353K over cobalt phyllosilicate at atmospheric pressure resulting in 99.6% conversion and 98.2% selectivity to syngas at 353K. The catalyst can be reused for four cycles in the oxidation of cyclohexene. The catalyst was calcined to regain a good conversion. Cobalt phyllosilicate also showed excellent activity in the mineralisation of iso-octane and toluene.