Extraction of nickel from laterites, especially low-grade limonitic ores has been facing challenges related to the lack of an effective beneficiation method. A chemo-physical laterite ore processing comprising oxalic acid leaching followed by size separation of the leach residue was recently introduced by the authors as a novel method to collect small amounts of nickel values dispersed in the ore matrix into distinct oxalate particles to form an intermediate product. In the present work, the ammonia leaching of such intermediate product containing about 12 wt% NiC2O4·2H2O was accomplished. Factors such as initial ammonia concentration (NH3: 2.5–25 wt%), temperature (T: 20–50 °C), pulp density (S/L: 50–200 g/L), and sonication were examined in a series of agitated leaching tests. It was found that under the conditions of 25% NH3, T = 50 °C, S/L = 200 g/L, and 15 min of sonication, about 93% of nickel is dissolved resulting in a pregnant leach solution (PLS) with a nickel content of 7.4 g/L. Besides, the activation energy for dissolution of nickel oxalate in ammonia solution was found to be about 71 kJ mol–1 from a kinetic analysis of leaching data. The PLS was subsequently deammoniated by either boiling or vacuum-assisted gentle heating to reclaim the nickel as an oxalate salt. Electron microscopic analysis of nickel oxalate precipitates formed from ammonia solutions exhibited rod-like morphology with high aspect ratio. Deammoniation under boiling led to well-shaped and distinct particles (∼150 nm width), while the precipitates obtained under partial vacuum were splintered and finer (∼40 nm width). The pyrolysis at 400 °C in an air atmosphere of the nickel oxalate particles from the boiling and the vacuum-assisted deammoniation methods generated mesoporous NiO nanorods with average widths of about 100 and 30 nm, and specific surface areas of about 45 and 70 m2 g−1, respectively.
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