The invention relates to a preparation method of a heterogeneous catalyst of organic coordination compounds of mesoporous structure metals, belonging to a preparation method of heterogeneous catalysts. Theterogeneous catalyst prepared by the prior art has the defects that the utilization ratio of surface active composition is limited, the direction of catalytic reaction can not be controlled easily, and the activity and the selectivity can not reach the optimal effect. In the invention, the preparation method of the heterogeneous catalyst of organic coordination compounds of mesoporous structure metals comprises the following steps of: mixing zirconium tetrachloride, 1,4-terephthalic acid and N,N-dimethylformamide solvent under the condition of microwaves, and stirring the mixture at room temperature until the solution is clear; adding the solution into a microwave reactor for microwave heating, removing the supernatant solution, and washing the residual solid matters with the N,N-dimethylformamide solvent; and drying the washed matters in a vacuum mode to obtain the heterogeneous catalyst. The invention has the advantages of simple process and easy operation; the prepared heterogeneous catalyst has efficient catalytic activity; and the catalyst can be recycled, thereby reducing the production cost and decreasing the environment pollution.