Many reasons have caused a worldwide water stress problem. Thus, the recycling of wastewater streams has been extensively studied. In this work, eco-friendly mixed matrix membranes (MMMs) were fabricated, characterized, and tested for the removal of two separate dyes from simulated waste streams. The environmentally friendly nano activated carbon (NAC) was extracted from water hyacinth to be impregnated as a membrane nano-filler to enhance the neat membrane performance. The extracted NAC was further studied and characterized. Cellulose acetate (CA)-based membranes were obtained by phase inversion and electrospinning mechanisms. All four synthesized blank and MMMs were characterized via scanning electron microscope (SEM) and contact angle to study their structure and hydrophilic nature, respectively. However, the membrane with optimum performance was further characterized using Fourier transfer infrared (FTIR) and X-ray diffraction (XRD). The four prepared cast and electro-spun, blank, and mixed matrix CA-based membranes showed an acceptable performance in the removal and selectivity of methylene blue (MB) dye over Congo red (CR) dye with a removal percentage ranging from 31 to 70% depending on the membrane used. It was found that the CA/NAC hybrid nanofiber membrane possessed the highest removal efficiency for MB, where the dye concentration declined from 10 to 2.92 mg/L. In contrast, the cast blank CA membrane showed the least removal percentage among the synthesized membranes with only 30% removal. As a result, this paper suggests the use of the CA/NAC hybrid membrane as an alternative and cost-effective solution for MB dye removal.