In this study, an innovative method was investigated for resloving the problem involved in iron–nickel nanoparticles reuse in dye removal. The completely oxidized nanoparticles, once used for dye removal, were separated from the solution and reduced with different concentrations of sodium borohydride. After SEM and EDAX analyses, 54 experiments were carried out using RSM method by applying Box–Behnken model. The obtained high coefficient of determination and very small P‐value (<0.0001) demonstrated that the model was appropriate to characterize the actual relationship between the response and input values. In this model, six independent variables including sodium borohydride concentration, contact time, shaking speed, time passed from oxidation, dye concentration, and nanoparticles concentration were studied to optimize the removal of Acid Red 14. According to ANOVA analyses and the obtained graphs, it was observed that the shaking speed of reducer solution and nanoparticles concentration were the most effective parameters, whereas the interval between oxidation of nanoparticles and their further reduction had no significant impact on removal efficiency. By maximum dye removal with the lowest reducer and nanoparticles concentration in optimum conditions predicted by the model ([NaBH4] = 2 g L−1, contact time = 104 min, shaking speed = 43 rpm, time passed = 0 day, [dye] = 200 mg L−1, [NPs] = 0.4 g L−1), the removal efficiency of 92.57% would be achieved. © 2016 American Institute of Chemical Engineers Environ Prog, 35: 1646–1656, 2016
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