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Cobalt precipitation by reduction with sodium borohydride

University of British Columbia

The reaction of cobalt reduction with borohydride is very complicated. Various authors obtained different reaction stoichiometries and have proposed a number of mechanisms. There are conflicting claims about the removal of cobalt from zinc electrolyte with sodium borohydride. The present research has focused on the stoichiometry of cobalt reduction with borohydride and on the removal of cobalt from zinc sulphate solution. Cobalt reduction with borohydride releases hydrogen ions resulting in a decrease in the pH of the solution. The efficiency of cobalt reduction increased with increasing concentration of NaOH in the reducing solution. The NaOH in the reducing solution neutralized the hydrogen ions released during cobalt reduction. The best reduction efficiency without the precipitation of cobalt hydroxide is one mole of sodium borohydride to reduce one mole of cobalt (II). If the pH was controlled at 4, the maximum reduction efficiency was about 81 % for a ten-minute addition time and the addition of more sodium borohydride did not increase the reduction efficiency. The reduction efficiency increased with increasing pH from nil at pH 2 to 96% at pH 6 and decreased with increasing temperature. X-ray diffraction patterns and TEM patterns of the recovered precipitates showed them to be amorphous. After a two-hour heat-treatment at 500 °C, the X-ray diffraction pattern of the precipitate showed well-defined peaks due to C 0 2 B with the main peak attributable to cobalt. The single crystal TEM pattern obtained was consistent with that of C 0 2 B . The particle size was about 20-100 nm. The atom ratio of Co to B increased with increasing temperature. The reduction of cobalt ions in the absence of interfering species was completed within several seconds. The time for the reduction of most of the cobalt ions decreased with increasing temperature from 24 seconds at 5 °C to less than 2 seconds at 35 °C. Zinc ions had a dramatic inhibitory effect on cobalt reduction. Several tens of iumol/L of zinc ions completely inhibit cobalt reduction with borohydride. The main cause of inhibition is that zinc ions compete with those of cobalt for borohydride ions and zinc borohydride forms and hydrolyzes rapidly. The resulting zinc ions react further with borohydride. Zinc ions catalyze the hydrolysis of borohydride. Zinc ions also have an inhibitory effect on nickel, cadmium and lead reduction.

Thesis/Dissertation

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2009-02-06

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http://hdl.handle.net/2429/4232

Materials Engineering

University of British Columbia

UBCV

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