The invention provides a hydrothermal preparation method of a zinc oxide/two-dimensional layered titanium carbide composite material. The hydrothermal preparation method of the zinc oxide/two-dimensional layered titanium carbide composite material comprises the following steps of adding two-dimensional layered titanium carbide and Zn(NO<3>)<2>.6H<2>O to anhydrous ethanol, performing stirring for 2-5 hours, adding NaOH, then performing stirring for 0.5-1h, placing a mixed solution in a hydrothermal kettle, enabling the mixed solution to be subjected to a reaction at 100-140 DEG C for 6-10h, performing washing, and performing drying so as to obtain the zinc oxide/two-dimensional layered titanium carbide composite material. According to the hydrothermal preparation method disclosed by the invention, non-toxic raw materials are used, besides, a preparation process is simple, the technology is controllable, the cost is low, the synthesized zinc oxide/two-dimensional layered titanium carbide composite material is large in specific surface area, concurrently has excellent properties of zinc oxide and excellent properties of two-dimensional layered titanium carbide, and the application of the zinc oxide/two-dimensional layered titanium carbide composite material in the fields of photocatalysis, wastewater treatment, biosensors, supercapacitors, lithium ion batteries and the like is facilitated.