This paper presents the results of a novel study on the direct synthesis of nickel oxide nanoparticles from a synthetic pregnant leach solution (PLS) as a middle stage product of hydrometallurgy process of nickel production. To increase the nickel proportion in the initial PLS, electrodeionization was utilized in the presence of EDTA to form an anionic complex ([Ni-EDTA]2−) with Ni2+ cations, allowing their separation from cobalt cations through the EDI process. Subsequently, the Fenton process was applied to synthesize nickel oxide nanoparticles from the complex containing solution. The proposed hybrid process was conducted in two different modes of one-stage and two-stage EDI process followed by the Fenton process. Different analysis methods including AAS, XRD, FE-SEM, and ICP were used for qualitative and quantitative evaluations. The analyses’ results revealed that by implementing one-stage EDI process followed by Fenton process resulted in producing nickel oxide nanoparticles with an average particle size of 45 nm and purity of about 98 %. Also, it was seen that about 81 % of initial nickel content of the initial PLS was recovered as nickel oxide nanoparticles. In the case of two-stage EDI process, 100 % pure nickel oxide nanoparticles with average size of 55 nm and recovery of 65 % was produced. The results showed that the innovative hybrid EDI/Fenton process can be considered as a promising approach for direct synthesis of high purity nickel oxide nanoparticles from PLS. However, it should be noted that there was a trade-off between purity of nickel oxide and nickel recovery from PLS.
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