The invention relates to a preparation method of 2,2'-bistrifluoromethyl-4,4'-diaminobiphenyl. The preparation method comprises the steps: dissolving 2,2'-bistrifluoromethyl-4,4'-dinitrobipheny in a polar protic solvent, then adding a catalyst, heating up to 40-60 DEG C, dropwise adding 80% hydrazine hydrate, next heating up to carry out a reflux reaction, after the raw materials are subjected to complete reaction, cooling down to room temperature, filtering, distilling a solvent out of the filtrate, and precipitating a 2,2'-bistrifluoromethyl-4,4'-diaminobiphenyl crystal. By-products of the method adopting hydrazine hydrate for reduction are nitrogen and water, and substances harmful to the environment do not produced; moreover, the method has the advantages of simple reaction device investment, easy control of the reaction, recycled solvent, high yield, repeatability and the like. In today, concerns on ecology and environment are grown, and the method can become a supplement of a catalytic hydrogenation method and replaces a partial sodium sulfide reduction method and a metal reduction method.