A novel method was applied for the preparation of highly dispersed nickel-tin (Ni-Sn) alloy catalyst supported on aluminium hydroxide using a simple method at a relatively low temperature. The addition of Sn (1.04 mmol) on the Raney nickel supported on aluminium hydroxide (R-Ni/AlOH) to form Ni-Sn(3.0)/AlOH (3.0 is Ni/Sn ratio) alloy catalyst remarkably enhanced the selectivity towards hydrogenation of C=O rather than C=C in furfural giving high yield of furfuryl alcohol almost exclusively. The Ni-Sn(3.0)/AlOH (3.0 is Ni/Sn ratio) alloy was also found to be reusable without any significant loss of selectivity for at least six consecutive runs.