The invention discloses a method for preparing titanium carbide two-dimensional nanosheets by a high-temperature vulcanization heat treatment method, which comprises the following steps of S1, puttingsublimed sulfur and titanium sulfur carbon powder into a mortar, and sufficiently grinding at room temperature to sufficiently and uniformly mix, S2, after grinding is finished, pressing the evenly-mixed raw material powder into a wafer in a dry mode, and sealing the wafer in a vacuum quartz tube, S3, placing the quartz tube in a heat treatment furnace to be heated to different temperatures for heat preservation, reducing the temperature to the room temperature after reaction, and acquiring a sulfur powder and titanium carbide mixture material in the quartz tube, and S4, dissolving sulfur powder with carbon disulfide liquid, filtering, and washing with water to obtain the single-phase black titanium carbide material. According to the preparation method, a new simple way is provided for preparation of the titanium carbide two-dimensional nanosheet material, so that production and development of the titanium carbide two-dimensional nanosheet material are promoted, and compared with preparation of the two-dimensional nanosheet material through HF acid etching, the method has the advantages of being free of pollution, capable of achieving batch production easily, low in cost and the like.