In order to improve the physical adsorption of the composite curing agent and improve the solidification treatment effect of the waste mud, the adsorption materials and adsorption processes were studied. Through the study of orthogonal experiments, the effects of polyvinyl alcohol (PVA) concentration, spinning voltage, spinning distance and other factors on the diameter, fibre uniformity and fibre morphology of PVA nanofibers were explored, with the optimal preparation conditions for the preparation of PVA nanofibers studied. The adsorption properties of PVA nanofibers for Pb2+ and Cu2+ were studied, and the Langmuir and Freundlich theoretical models were used to fit the adsorption isotherms to determine the adsorption model; the adsorption kinetics were fitted using quasi-first-order and quasi-second-order kinetic equations to determine the type of adsorption. The research has a theoretical reference for the exploration of the physical adsorption of composite curing agents and the solidification of waste mud.