The invention discloses a preparation method of a porous covalent organic framework and application of the porous covalent organic framework in uranyl ion capture, belonging to the technical field of adsorption materials. The preparation method comprises the following step: carrying out an aldol condensation reaction on 2,5-dihydroxy-1,4-phthalaldehyde (DHBD) and 2,4,6-trimethyl-1,3,5-triazine (TMT) to prepare an olefinic bond porous covalent organic framework (DHBD-TMT). The DHBD-TMT prepared by the method disclosed by the invention has a large number of hydroxyl functional groups and a highly planar pi-conjugated structure, and can simultaneously realize multiple functions of selective adsorption, chemical reduction, photocatalytic reduction of uranium and the like, so the adsorption capacity of uranium is remarkably improved. Inductively coupled plasma mass spectrometry results show that DHBD-TMT has excellent adsorption performance on uranyl ions, and has the advantages of high adsorption capacity, good selectivity, excellent optical activity, high stability, good hydrophilicity and the like. Besides, the DHBD-TMT can reduce soluble uranium (VI) into insoluble uranium (IV) through chemical reduction and photocatalytic reduction under visible light irradiation, so uranium fixation is realized; and the DHBD-TMT is an efficient adsorbent for extracting uranyl ions.