This report describes an efficient hybrid treatment process that recycles semiconductor wastewater by reverse osmosis (RO) and advanced oxidation process (AOP) with metal-immobilized catalysts based on activated carbon. High-loading organic wastewater was pretreated biologically using a membrane bioreactor, and the remaining organic compounds were filtered by RO and oxidized chemically by AOP. The recycling of the final effluent to ultrapure water (UPW) was evaluated using a pilot-scale UPW production system. AOP with a metal catalyst improved the oxidation of low-molecular-weight organic compounds, such as acetonitrile and acetaldehyde, in electronics wastewater. The pilot-scale RO and AOP with a metal catalyst were performed under optimal conditions and satisfied the water quality standards for UPW. We conclude that the proposed hybrid process is a powerful tool that can be used to recycle electronics wastewater and satisfy the water quality standards for UPW.