The invention provides a ferro-cobalt micro-structural catalyst material, as well as a preparation method and application thereof. Compared with the prior art, the preparation method has the advantages that the ferro-cobalt alloy material having an ear-shaped structure is prepared by a solvothermal method under a mild reacting condition, and the appearance of the ferro-cobalt alloy material is not reported so far; the structure has excellent magnetic performance, the catalyst material can be quickly separated and reclaimed by utilizing magnet in a cyclically catalyzing experiment, and the catalyst can be conveniently washed and cyclically utilized; the ferro-cobalt alloy catalyst material is low in production cost, short in flow and low in requirement for equipment, is easy for scale-up experiments and can realize industrial production; and the ferro-cobalt alloy micro-structure can be used in p-nitrophenol reduction to show the advantages of high reaction speed, high catalyzing efficiency, good circulation effect, low cost and the like.