The invention provides a nano-size layered double hydroxide and a step-by-step precipitation preparation method thereof. The preparation method comprises the following steps: based on a soluble salt of a metal and an alkali as raw materials, respectively precipitating metal ions constituting an LDH (layered double hydroxide) layer plate through step-by-step precipitation reaction and generating the LDH during the second-step precipitation process. As the activity of the hydroxide prepared by the first-step precipitation reaction is high, the LDH can fast nucleate and grow during the second-step precipitation, an obtained LDH sheet is thinner, the thickness of the layer plate is 5-15nm, the length of the layer plate is 50-150nm, and the specific surface area of a BET (Brunauer-Emmett-Teller) is 140-280m<2> / g, which is much larger than the specific surface area of the common LDH. By adopting the method, the shortcoming of small specific surface area during the preparation of the LDH through a co-precipitation method can be overcome. The preparation method adopted by the invention is simple and convenient, high temperature and high pressure are not required, special equipment is not required, sources of the raw materials are rich, and the cost is low. The layered double hydroxide can be widely applied to the fields of adsorption separation, catalysis, high polymer materials and the like.