An FeIII-based steel–natural framework denoted as MIL-100(Fe) coated with cobalt–aluminium layered double hydroxide (CoAl-LDH) nanoplates has been synthesized. The structural data was obtained by way of powder X-ray diffraction (PXRD), Fourier rework infrared spectroscopy (FT-IR), nitrogen sorption (BET and BJH), thermo-gravimetric evaluation (TGA), scanning electron microscopy (SEM) and related power dispersive X-ray (EDX), transmission electron microscopy (TEM) and diffuse reflectance UV–Vis spectroscopy (UV–Vis DRS) strategies. Such attribute strategies point out that the bonding between mesoporous CoAl-LDH nanosheets and open steel websites of steel–natural frameworks results in non-covalent composite formation. Additionally, CoAl-LDH linkers add the characteristic of mesoporosity to MIL-100(Fe). Moreover, the Fe–O bonds ensuing from the coordination of floor –OH teams within the layered double hydroxide construction to FeIII atoms of the crystal create distinctive optical properties within the hybrid construction, enhancing its photoreactivity. Then again, the dearth of pore quantity adjustments and variations among the many optical properties point out a non-covalent composite formation between MIL-100 (Fe) and CoAl-LDH. The CoAl-LDH/MIL-100(Fe) as a photocatalyst confirmed noticeable photocatalytic efficiency as in comparison with its cardio alcohol oxidation response elements underneath seen mild irradiation. Additionally, it’s noteworthy that the kind of product depends upon the response situations. The related assessments have been carried out when it comes to stability and reusability and confirmed excessive photocatalytic effectivity after being reused as much as ten instances. Moreover, the retrieved CoAl-LDH/Fe-MOF nanocomposite underwent FT-IR and PXRD analyses, which confirmed the soundness of the catalyst throughout cardio alcohol oxidation.