The invention discloses a preparation method of 1-(4-(4-(1H-1,2,4-triazolyl-1-yl)phenoxy)phenyl)-1H-1,2,4-triazole. The organic compound is prepared by heating 4,4'-dibromodiphenyl ether, triazole, potassium carbonate and copper oxide by a one-pot process. The preparation method has the characteristics of simple technological operation, low production cost and low environmental pollution, and is suitable for large-scale industrial production. The invention also discloses application of the 1-(4-(4-(1H-1,2,4-triazolyl-1-yl)phenoxy)phenyl)-1H-1,2,4-triazole in photoelectric materials.