In the present work, a highly efficient mixed matrix membrane (MMM) for humic acid (HA) removal was developed. Multiwalled carbon nanotubes (MWCNTs) were functionalized in the presence of 3-methacryloxypropyl trimethoxysilane using the co-condensation method and were subsequently loaded with TiO2 (prepared via the sol–gel route). The as-prepared material was then incorporated into a PES polymer solution to prepare a fMWCNT-TiO2/PES hybrid membrane via non-solvent induced phase inversion. The microstructure of the membrane was characterized using Fourier transform infrared spectroscopy, atomic force microscopy, scanning electron microscopy, water contact angle, thickness, porosity, and pore size. The fMWCNT-TiO2/PES hybrid membrane was tested for the removal of HA and antifouling performance. The results show that the surface hydrophilicity of the membranes was greatly improved upon the addition of the fMWCNT-TiO2 particles. The results show that 92% of HA was effectively removed after 1 h of filtration. In comparison with pristine membrane, the incorporation of fMWCNT-TiO2 nanoparticles led to enhanced pure water flux (99.05 L/m2 h), permeate flux (62.01 L/m2 h), higher HA rejection (92%), and antifouling improvement (RFR: 37.40%, FRR: 86.02%). Thus, the fMWCNT-TiO2/PES hybrid membrane is considered to be a great potential membrane for the improvement of ultrafiltration membranes.