The iron-titanium solid solution catalyst with Fe3+/Fe2+ molar ratio of 1∶1 and a certain amount of Ti4+ were synthesized by ammonia co-precipitation method. It was compared with the iron titanium catalyst prepared by mechanical mixing grinding method. The effects of different preparation processes on the physicochemical properties and catalytic activity of catalyst were discussed. The physical and chemical properties of the catalyst were characterized by means of XRD, N2 adsorption-desorption, XPS, H2-TPR and NH3-TPD. The results show that the one-step ammonia co-precipitation method and the doping a certain amount of Ti are beneficial to increase the specific surface area of the catalyst, suppress oxide crystallization and crystal phase transformation, make the catalyst grain size smaller, and improve the low-temperature catalytic activity. At the same time, it shows that the catalyst prepared by mechanical mixing grinding is only a simple mechanical mixing between oxide crystals, which does not form a close coupling effect and can not effectively improve the catalytic performance.