The co-contamination of manganese ions (Mn²⁺) and ammonia nitrogen (NH₄⁺) caused by the stockpiling of manganese residue poses a serious threat to the ecological environment. In this study, a series of the composite was prepared from red mud, bentonite, and corn straw via oxygen-limited pyrolysis. The effects of pyrolysis temperature and raw material ratio on the material properties were investigated, and the synergistic remediation performance of the composites for Mn²⁺ and NH₄⁺ in manganese residue-contaminated soil was evaluated through a 180-day soil column experiment. The results showed that the composite prepared with a raw material ratio of 1:1:1 at a pyrolysis temperature of 700 °C exhibited the largest specific surface area and the most developed pore structure, achieving a Mn²⁺ removal rate of 92.72% ± 0.85% in aqueous solution. In the soil column experiment, the material prepared at 700 °C gave the highest immobilization rate for soil Mn²⁺ (96.22% ± 0.5%), whereas the combined addition of materials prepared at 700 °C and 500 °C achieved the best removal efficiency for NH₄⁺ (99.33% ± 0.23%). Mechanistic studies revealed that the stabilization of Mn²⁺ is primarily attributable to alkaline precipitation and mineral lattice solid solution induced by the composite, leading to the formation of stable spinel phases (e.g., (Fe,Mn)₃O₄) and insoluble manganese phosphate-carbonate salts. The removal of NH₄⁺ is proposed to proceed via adsorptive enrichment by the porous structure and Fe⁰-mediated Fenton-like catalytic oxidation, ultimately converting NH₄⁺ to N₂ gas. The 180-day monitoring results demonstrated that the remediation effect continuously increased over time, indicating good long-term stability of the composite. This study provides an efficient, low-cost functional material derived from solid waste for the remediation of manganese residue-contaminated soil and offers a theoretical basis for the synergistic resource utilization of multiple solid wastes.

Tantalum and niobium are critical strategic rare refractory metals; however, most associated tantalum–niobium resources are characterized by ultra-low grade, finely disseminated grains, and severe argillization, which causes pronounced slime coating of gangue mica on valuable mineral surfaces and impedes efficient recovery via gravity separation. In this study, an innovative beneficiation route combining sodium silicate pre-dispersion conditioning with shaking-table gravity separation was proposed to recover a spodumene-dominant pegmatitic lithium ore containing trace associated Nb–Ta minerals, with mica as the major slime-forming gangue. Process mineralogy analysis revealed that the raw ore has a total (Nb,Ta)₂O₅ grade of only 0.019%, with the main valuable minerals being columbite-(Mn), columbite–tantalite, and tantalite, whereas layered mica minerals constitute the primary argillization gangue that readily generates micro-fine slimes smaller than 5 μm. Single-factor tests demonstrated that the optimal grinding fineness was 84.4% passing 200 mesh, and the optimal feed pulp density for gravity separation was 28.6%. Adjusting pulp concentration alone, without a dispersant, yielded a Nb₂O₅ concentrate grade of merely 0.144%, as severe slime coating greatly limited separation selectivity. Following the introduction of sodium silicate for pre-dispersion, the separation performance improved markedly at the optimal dosage of 300 g/t: the concentrate Nb₂O₅ grade reached 1.28% (8-fold higher than the blank test), and the Ta₂O₅ grade increased to 0.47% (85-fold higher than the blank test). Multi-scale characterization, including zeta potential measurements, ultraviolet–visible (UV–vis) diffuse reflectance spectroscopy, Fourier-transform infrared spectroscopy (FTIR), and X-ray photoelectron spectroscopy (XPS), was employed to elucidate the dispersion mechanism of sodium silicate. The results confirmed that sodium silicate undergoes selective chemisorption on mica surfaces by forming Si–O–Al bonds with surface Al–OH active sites, which substantially increases electrostatic repulsion between mineral particles and eliminates mica slime coating on tantalum–niobium minerals. In contrast, sodium silicate exhibits only weak physical adsorption on tantalum–niobium mineral surfaces, with no evident chemical bonding. This work provides a low-cost, eco-friendly pretreatment–gravity separation coupling technology for the efficient enrichment of argillized ultra-low-grade tantalum–niobium associated ores and offers theoretical guidance for the green utilization of complex tantalum–niobium tailings and low-grade mineral resources.