This paper studies the treatment of unsymmetrical dimethylhydrazine wastewater in Ni-Al-OH- system by catalytic reduction process. The reasonable technological conditions are acquired by orthogonally designed experiments. The results indicate that Ni hydrogenolysis has reliable,quantitative and efficient degradation potentiality and the catalytic reduction process holds considerable promise as a new approach to prevent environmental contamination by unsymmetrical dimethylhydrazine.