Glass was successfully recycled in the synthesis of mesoporous silica MCM-48 which was used as catalyst support for nickel oxide photocatalyst. The resulted products were evaluated using X-ray diffraction, scanning electron microscope and UV–Vis spectrophotometer. The precipitated nickel oxide is of Ni
2O
3 form and loading of it onto MCM-48 resulted in a reduction in the band gap energy from about 3.66 eV to about 2.4 eV. The role of MCM-48 as catalyst support for Ni
2O
3 in enhancing the adsorption capacity and photocatalytic properties of nickel oxide was evaluated through series of equilibrium studies and photocatalytic degradation of Congo red dye under visible light. Using of glass-based MCM-48 as catalyst support for Ni
2O
3 showed enhancing the adsorption capacity by 31.3 and 14.8% higher than the adsorption capacity of Ni
2O
3 and MCM-48, respectively. Also, the photocatalytic degradation percentage increased by about 67.3% relative to the Ni
2O
3 degradation percentage. The nature of MCM-48/Ni
2O
3 adsorption mechanism is chemisorption and occurs in multilayer form throughout the heterogeneous surface of the composite. The using of MCM-48 as support for Ni
2O
3 photocatalyst enhanced the adsorption capacity through increasing the total surface area. The loading process resulted in fixing of the Ni
2O
3 particles throughout the porous structure which producing more exposed active photocatalyst sites and active adsorption sites for the incident photons as well as preventing the nickel oxide particles from agglomeration. Based on the obtained results, supporting of Ni
2O
3 particles onto MCM-48 is promising active centers for the degradation of Congo red dye molecules.
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