Abstract: Plutonium, as a crucial strategic element, plays an indispensable role in key fields such as nuclear power generation, nuclear weapon manufacturing, and isotope battery development. At the same time, plutonium is a highly toxic radioactive nuclide, and its leakage into the environment can cause profound harm to the ecosystem. Therefore, in the nuclear fuel cycle, efficient separation technologies for plutonium are not only critical to energy security and national defense security but also closely related to ecological security, making their value and significance self-evident. Due to plutonium’s multiple oxidation states, complex aqueous chemical behavior, and the radiolytic effects by its radioactivity, the efficient separation and recovery of plutonium have always been one of the core challenges in nuclear fuel reprocessing, while also being essential for environmental protection and the control of radioactive contamination. Addressing this challenge is crucial for both improving the sustainability of nuclear energy and minimizing the environmental impact of radioactive waste. This paper offers a comprehensive review of recent progress in plutonium chemical separation, focusing on separation and purification technologies represented by solvent extraction and solid phase separation methods. The review first examines the use of solvent extraction techniques, where various extractants such as organophosphorus compounds, amides, and water-soluble ligands are employed. The paper discusses the structural regulation strategies and selectivity enhancement mechanisms of these extractants, which aim to improve the efficiency of plutonium separation. Key factors such as donor atom availability, solvent-solute interactions, and solvent characteristics are explored to better understand their impact on extraction performance. Additionally, the review evaluates solid phase separation methods, comparing the use of functionalized silica-based materials, resin materials, carbon materials, and covalent organic frameworks(COFs) for plutonium adsorption. These materials offer different advantages in terms of selectivity, adsorption capacity, and stability under harsh conditions. The paper highlights the role of surface area, pore structure, and functional group properties in enhancing plutonium adsorption and discusses the limitations of each material. The ability of these materials to withstand high radiation fields and acidic environments, which are common in nuclear waste reprocessing, is also assessed. The paper concludes by assessing the practical applications and future research directions in the field of plutonium separation technologies. It highlights the need for the development of more efficient, cost-effective, and environmentally sustainable separation methods. As plutonium recovery becomes more critical in nuclear fuel reprocessing, the advancement of innovative materials and separation techniques will play a key role in addressing global energy and environmental challenges. Continued research into novel extractants and solid phase adsorbents, as well as the optimization of existing methods, is essential for improving the efficiency and sustainability of plutonium recovery in the nuclear industry.