Abstract: The supply chain of medical ⁹⁹Tc^m in the world is still very fragile, so the development of ⁹⁹Mo-⁹⁹Tc^m separation devices and processes based on non-fission 99Mo is very important to improve the security of ⁹⁹Tc^m supply in China. Activated carbon fiber (ACF) is a molybdenum technetium chromatographic separation material with excellent performance, which can be used to prepare non-fission ⁹⁹Mo-⁹⁹Tc^m chromatographic generator with multi-column selective reverse generator (MSIG) structure. Based on the modification and evaluation of ACF, a three-column ⁹⁹Mo-⁹⁹Tc^m separation and purification process was developed by using an automatic non-fission ⁹⁹Mo-⁹⁹Tc^m generator, and the sodium pertechnetate ⁹⁹Tc^m injection obtained by this device was used to label MDP and MIBI kits. The yield of ⁹⁹Tc^m in ⁹⁹Mo-⁹⁹Tc^m simulated solution by nonfission ⁹⁹Mo-⁹⁹Tc^m generator three-column separation process was 78%. The resulting sodium pertechnetate ⁹⁹Tc^m injection, radiochemical purity and labeling rate of MDP and MIBI kits all met the requirements of Chinese Pharmacopoeia. The three-column selectivity inversion ⁹⁹Mo-⁹⁹Tc^m generator based on ACF is expected to be used to extract ⁹⁹Tc^m from non-fission ⁹⁹Mo.