The invention discloses a preparation method of an electrocatalyst with a PdCu alloy particle loaded NiFe-LDH (layered double hydroxide) metal nanosheet material. The nickel nitrate hexahydrate-urea-triethylene glycol-ferric chloride hexahydrate composite catalyst is prepared by compounding nickel nitrate hexahydrate, urea, triethylene glycol, ferric trichloride hexahydrate, NaBH4, copper chloride dihydrate and potassium chloropalladate. The preparation method comprises the following steps: firstly, dissolving nickel nitrate hexahydrate in a mixed solution of deionized water and triethylene glycol, then adding ferric trichloride hexahydrate, and adding urea after ultrasonic dispersion; the preparation method comprises the following steps: adding NiFe-LDH into a reaction kettle, heating, reacting, washing and drying the reaction solution, dissolving the obtained NiFe-LDH powder in deionized water, adding K2PdCl4 and CuCl2. 2H2O, adding a NaBH4 solution, stirring, carrying out centrifugal treatment, washing and drying a centrifugal product to obtain a final product, adding deionized water, isopropanol and naphthol, and uniformly mixing to obtain a catalyst solution. The method is simple in process, low in energy consumption, mild in condition, good in product morphology and suitable for large-scale production.