The ultrasound assistance synthesis strategy of the polymeric composite is based on free radical polymerization of polyallylamine hydrochloride (PAH) cationic polyelectrolyte, with vinyl sulfonic acid (VSA) anionic monomer with microporous crystalline alumino silicate clinoptilolite clay. The P(AH-co-VSA)/clinoptilolite polymeric composite was fully characterized by fourier transform infrared spectroscopy, energy dispersive X-ray, thermogravimetric analysis, and scanning electron microscope. FTIR demonstrated the presence of PAH and VSA, confirming the composition of the prepared composite. It was also used to map the energy-dispersive X-ray to affirm the interdependence of the clinoptilolite into the polymeric matrix. Consequently, the physicochemical characteristics of this copolymer may be adjusted using VSA and PAH suitable combinations. Batch experiments were applied and maximal sorption capacities for studied ions Nd3+, Ce3+, Y3+, Gd3+, and Eu3+ were 36.6, 50.2, 55.9, 57.2, and 57.7 mg/g, respectively. Sorption kinetics and equilibrium isotherm were conducted. Experimental isotherms of studied ions were successfully fit to pseudo-second-order model, langmuir isotherm model. The Dubinin–Radushkevich (D–R) isotherm was found to be applicable and suggesting that, the sorption occurs via a ion exchange reaction. The breakthrough data were measured in a fixed bed column, and variable process factors were examined, including bed depth, flow velocity, and initial metal ion concentration. The experimental work was then focused, for continuous investigations, on Ce3+, Eu3+, and Y3+ to represent light, intermediate, and heavy lanthanides respectively. The overall bed capacity and total metal ion adsorption increased when the flow rate increased. They reduced with rising initial metal ion concentration and bed depth, and reached 22.8, 31.4, and 28.5 mg/g for Ce3+, Eu3+, and Y3+ metal ions, respectively.
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