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Separation of Cobalt and Nickel Using CYANEX 272 for Solvent Extraction

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Separation of Cobalt and Nickel Using CYANEX 272 for Solvent Extraction 2/2/2021 Separation of Cobalt and Nickel using CYANEX 272 for Solvent Extraction In the presence of other contaminates in sulphate based leaching solution Caroline Kihlblom BOLIDEN MINERAL AB Supervisor: Mohammad Khoshkhoo Examiner: Kerstin Forsberg 2021-04-07 Abstract This project aimed to examine the separation of cobalt and nickel using solvent extraction (SX) with the extractant CYANEX 272 (C272). It was intended to investigate the Co-Ni separation in a sulphate-based leach solution in presence of other contaminants. This is an area of interest because of the difficulty of separating metals of similar properties within the field of hydrometallurgy. Batch tests, with varying modifiers and diluents, were carried out to examine the effect of organic phase composition on phase separation. The effect of pH on equilibrium was investigated by constructing equilibrium curves. Through various shaking tests, different separation parameters were studied. McCabe-Thiele diagrams were constructed to predict design parameters. In order to simulate a continuous 3-stage countercurrent solvent extraction, batch tests were performed. Scrubbing, as means of impurity removal was also investigated. Finally, the product’s purity was examined by the help of crystallization. The organic feed mixture that resulted in a sufficient phase separation consisted of C272, tributyl phosphate and naphtha. At pH 4, equilibrium curves showed that equilibrium was either not reached or affected by competing metal ions. A standard equilibrium curve appearance was seen at pH 4.5, resulting in that the theoretical required stages for extraction was calculated to 3 stages (A/O=1). However, a McCabe-Thiele diagram did not give an accurate representation of the more complex case (presence of contaminants). Batch simulation results gave a cobalt recovery of 69% and 100% at pH 4.5 and 4.8, and a nickel recovery of 0% and 3%, respectively. A recommended pH-value for solvent extraction could not be stated, because the choice must be based on operation specifications. Therefore, several different aspects (Co recovery, purity, and economical etc.), must be accounted for. A similar pH-trend was shown in scrubbing, where an increase of pH resulted in an increase of metal ions’ organic concentration. For stripping, acid test results proved 24 g/L sulphuric acid to give the highest cobalt concentration, with a marginal difference in concentration of impurities. An overview of the entire SX process, indicated that extraction, scrubbing, and stripping were all successful operations. The extraction stage showed a Co and Ni recovery of 99% and 0.02%, respectively, and a separation factor of 14250. Distribution results indicated that Al was difficult to remove and was transferred with Co into the product. Therefore, this element must be removed before SX. From noticing an increase of Co:Ni ratio throughout the process, solvent extraction was considered an effective separation method for cobalt and nickel separation. A considerably high purity of cobalt sulphate was produced. However, impurities Al and Ca were also detected in the product. Increasing the acetone volume in crystallization resulted in an increase of Co purity. An increase of the cobalt sulphate crystals formed was observed when increasing the acetone volume, where no impurities were detected. Key words: Solvent extraction, Cobalt-Nickel separation, CYANEX 272, pregnant leach solution 1 (48) 2021-04-07 Table of Contents 1 INTRODUCTION ............................................................................ 4 1.1 Aim and objectives .......................................................................... 5 1.2 Scope .............................................................................................. 5 1.3 Boliden mineral ab .......................................................................... 6 2 BACKGROUND .............................................................................. 7 2.1 Solvent extraction ........................................................................... 7 2.1.1 Extraction ........................................................................................ 7 2.1.2 Scrubbing ........................................................................................ 7 2.1.3 Stripping .......................................................................................... 7 2.1.4 Solvent Extraction Chemistry .......................................................... 8 2.2 Seperation of cobalt and nickel ....................................................... 8 2.2.1 Solvent extraction in sulphate solutions .......................................... 8 2.2.2 Selectivity ........................................................................................ 9 2.2.3 Extractant and diluent ................................................................... 10 2.2.4 Impurities ...................................................................................... 12 2.3 Definitions ..................................................................................... 13 2.3.1 Distribution coefficient ................................................................... 13 2.3.2 Separation factor ........................................................................... 13 2.3.3 McCabe-Thiele diagram ................................................................ 14 3 METHODS AND MATERIALS ..................................................... 16 3.1 Materials ....................................................................................... 16 3.2 Experimental set-up ...................................................................... 17 3.2.1 Process overview .......................................................................... 17 3.2.2 Effect of saponification and organic phase composition ............... 18 3.2.3 Effect of pH on extraction equilibrium ........................................... 19 3.2.4 Batch Simulation of Continuous Multistage Countercurrent Solvent Extraction ...................................................................................... 19 3.2.5 Scrubbing tests ............................................................................. 21 3.2.6 Stripping tests ............................................................................... 21 3.2.7 Crystallization of Cobalt ................................................................ 21 3.2.8 Analytical methods ........................................................................ 22 4 RESULTS AND DISCUSSIONS ................................................... 24 4.1.1 Effect of saponification and organic phase composition ............... 24 4.1.2 Effect of pH on extraction equilibrium ........................................... 26 4.1.3 Batch Simulation of Continuous Multistage Countercurrent Solvent Extraction ...................................................................................... 29 4.1.4 Scrubbing ...................................................................................... 33 4.1.5 Stripping ........................................................................................ 34 4.1.6 Solvent extraction overview .......................................................... 35 4.1.7 Overall distribution and process summary .................................... 38 4.1.8 Crystallization of Cobalt ................................................................ 39 4.1.9 Source of error .............................................................................. 40 2 (48) 2021-04-07 5 CONCLUSION .............................................................................. 41 5.1 Future research ............................................................................. 43 6 ACKNOWLEDGMENTS ............................................................... 44 7 BIBLIOGRAPHY .......................................................................... 45 8 APPENDIX .................................................................................... 47 8.1.1 Effect of pH on extraction equilibrium ........................................... 47 8.1.2 Batch simulation of continuous multistage countercurrent solvent extraction ...................................................................................... 47 8.1.3 Stripping ........................................................................................ 47 8.1.4 Crystallization of cobalt ................................................................. 48 Table of Figures Figure 1: pH-dependency of Co, Ni and Ca extracted in a sulfate solution using CYANEX 272 ....................................................................................................... 10 Figure 2: Molecular structure of Di (2,4,4-trimethylpentyl) phosphinic acid (CYANEX 272)11 .................................................................................................. 11 Figure 3: Different metal ion extractions (in %) with Cyanex 272 vs. pH 9 ......... 12 Figure 4: Schematic of a McCabe-Thiele diagram5 .............................................. 15 Figure 5: A flowsheet of the overall experimental solvent extraction design....... 17 Figure 6: Batch simulation of 3-stage countercurrent solvent extraction. The red and black lines represent the aqueous and organic phase, respectively. Note that SX A3 was not conducted, but is presented for the sake of visualization. ........... 20 Figure 7: Continuous countercurrent solvent extraction, where the aqueous raffinate and organic extract are denoted with an R and
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