The negative environmental impacts of industrial activity have been felt day-to-day, encouraging global actions to reduce the waste generation of harmful and persistent pollutants. Microemulsion synthesis of silica-coated iron oxide magnetic nanoparticles offers a high potential for several applications; however the process generates hazardous wastes that are difficult to treat and dispose of. In this study, cyclohexane and methanol were separated using phase decantation, distillation, and temperature reduction. The recovered solvents were reused in the same synthesis more than 20 times and the recovered surfactant IGEPAL (R) CO-520 was reused twice, suggesting the method applied has potential for continuous recycling.