The invention relates to a preparation method of a nanoscale molecular sieve@ graphene oxide coupled material. The technical scheme comprises the following steps: (1), sufficiently mixing nano-zeolitesilicon source and aluminum source solutions; (2), ageing, washing and drying the mixed solution at low temperature, so as to obtain molecular sieve amorphous precursor, and ensuring that the pH value is 8 after washing; (3), performing stirring, ultrasonic mixing and ageing on the molecular sieve amorphous precursor and graphene; (4), adding alkaline substance into the aged solution, and crystallizing, washing and drying a formed reaction solution, so as to obtain a product. The method has the beneficial effects that firstly, reagents adopted for reaction are available, low-in cost, green and pollution-free; secondly, molecular sieve crystal adopts nanoscale, and effective specific surface area is high; thirdly, nanoscale molecular sieve adopts a small packed structure, and a gas diffusion path is short; fourthly, the micropore utilization efficiency of the molecular sieve is improved through modes of cage expansion or cage opening; fifthly, the composite property of the material ishigher than that of other organic matter and inorganic matter.