The invention belongs to the technical field of sewage treatment and particularly relates to a preparation method of a novel liquid-state nano complex flocculant. The preparation method comprises thefollowing steps: step 1, taking waste liquid containing hydrochloric acid, corroded aluminum and oxidized ferric, discharged in production processes, as raw materials, and performing stirring treatment for reacting to generate an aluminum chloride and ferric chloride mixture solution; step 2: adding the aluminum chloride and ferric chloride mixture solution generated in the reaction to a sodium hydroxide solution, adjusting the solution to a certain pH value, and standing the solution for a period of time to obtain a polymeric aluminum ferric chloride (PAFC) solution; and step 3, adding the obtained PAFC solution to an organic cation polymer product to generate a nano flocculant. The nano complex flocculant prepared by the preparation method provided by the invention has the beneficial effects that the nano complex flocculant belongs to an efficient complex variety, and pesticide wastes are used as raw materials, so that waste utilization is realized, ecological environment protectionis realized, and green cyclic development of agriculture is promoted; and compared with a traditional solid-state product, the nano complex flocculant has the advantages of high reaction speed, full reaction, uniform concentration and greatly improved treatment efficiency.