To treat wastewater containing vat dyes, a newly method of based on MIL 53 (Al-Fe) @SiO2 was created and used in a combine to desegregated process toward off followed by adsorption. Coal fly ash was used in the synthesis of MIL 53 (Al-Fe) @SiO2. As compared to raw fly ash obtained by coal, the newly synthesized material, MIL 53 (Al-Fe) @SiO2, present remarkable changes in physical and chemical properties, which improve and become greater its adsorption capacity by three times. In adding, the FTIR examination and analyzed investigation shows that the Compared to MIL 53 (Al) and MIL 53 (Fe)@SiO2, freshly synthesis MIL 53 (Al-Fe) @SiO2 exhibits a reduced electron-hole recombination rate. 53 (Al)@SiO2. The highest adsorption capacity of the MIL 53 (Al-Fe) @SiO2 was 692.942 mg g1 and highest degradation of 89.89 and 99.98% when exposed to visible and UV light subjection, separately This study demonstrates that suggested MIL 53 (Al-Fe) @SiO2 outperforms the traditional materials in the removal of hazardous contaminants from industrial effluents. KEY WORDS: Vat dyes, MIL53(Al-Fe) @SiO2, Adsorption.