The molecular formula of a semi-rigid double-imidazole organic-ligand-based transition metal compound containing N-S dicarboxylic acid is [Co2 (L) 2 (2-CMSN) 2 (H2O)]. H2O; [Cd (L) (2-CMSN) (H2O)]; [Zn (L) (2-CMSN)]. 2 H2O; [Cd (L) (ADTZ) (H2O)]; [Zn (L) (ADTZ)]. H2O, wherein L represents 1, 4-bis ( imidazol-1-methylene ) benzene, 2-CMSN represents 2-carboxylic acid methylene group root, and ADTZ represents 2,2'-(1,3,4-thiadiazol oxazol-2,5-diyl) dithio diethyl dianion root. A synthetic method of the transition metal compound comprises the following steps: adding Co<2+> or Zn<2+> and Cd<2+> nitrate, semi-rigid double-imidazole ligands, dicarboxylic acid containing N and S into deionized water, stirring, using NaOH solution to adjust pH, pouring the mixture into a high-pressure reaction kettle, increasing the temperature to realize hydrothermal reaction, cooling to obtain a bulk crystal, and washing and drying the bulk crystal to obtain the target product. The synthetic method of the compound is simple, the synthesis productivity is high, the cost of synthetic raw materials is low, the synthetic period is short and the electrical energy consumption is low; the compound is high in affiliation capacity of water-soluble pollutants, good in catalysis and degradation effects and environmental-friendly, and can be used as photocatalytic materials.