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A highly acidic fullerene containing niobium phosphate catalyst demonstrating high thermal stability is synthesized by one pot Sol‐Gel EISA method. The ratio of niobium, phosphorous and surfactant plays a key role for the in‐situ fullerene generation. A thorough study of elemental, textural and chemical properties using different experimental techniques and an extensive catalytic investigation has been done using a series of catalysts synthesized by varying different parameters. The high conversion and selectivity for cyclohexanol and ethanol dehydration reaction and also five regeneration upto fine five consecutive cycle could be useful for conversion of biomass to fine chemicals.

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