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Institute of Minerals and Materials Technology (CSIR) Bhubaneswar-751 013, Odisha, India

Processing of Ni-Laterite Bacterial Leach Liquor for Recovery of Zn, Mn, Co and Ni Using Solvent Extraction. By K.C. Nathsarma. Institute of Minerals and Materials Technology (CSIR) Bhubaneswar-751 013, Odisha, India. Hydro & Electrometallurgy Department: Mission & Goal.

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Institute of Minerals and Materials Technology (CSIR) Bhubaneswar-751 013, Odisha, India

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  1. Processing of Ni-Laterite Bacterial Leach Liquor for Recovery of Zn, Mn, Co and Ni Using Solvent Extraction By K.C. Nathsarma Institute of Minerals and Materials Technology (CSIR) Bhubaneswar-751 013, Odisha, India

  2. Hydro & Electrometallurgy Department: Mission & Goal • To assist public / private sector organizations / industries in developing processes for extraction of metals from: • Ores and concentrates. • Lean, complex, off-grade ores and minerals. • wastes generated by metallurgical & allied industries (tailings, residues, sludges and effluents).

  3. Role of the Department • To develop processes and products. • Exploit primary and secondary resources. • Employ hydro- & electro-metallurgical routes. • Prepare feasibility reports. • Develop basic and detailed engineering process packages. • Assist in environment pollution abatement.

  4. Atmospheric & Pressure Leaching 1400 L Autoclave for Pressure Leaching • Batch Autoclaves (300 ml – 1400 L) • Continuous Autoclaves (500 LPH) • Stirred Tank Reactors (0.5 kL – 1 kL) • 1400 L Autoclave for Pressure Leaching

  5. Solid-Liquid Separation • Thickeners • Filters (Vertical leaf, Candle, Chamber) • CCD Units • 1 ton Filter Press 1 ton Filter Press

  6. Solvent Extraction • Mixer Settlers • 26 Stages 200 L/h aqueous SX Unit. 26 Stages 200 L/h Aqueous SX Unit

  7. Rectifiers and Potentiostat Charge-Discharge Unit 100 kg/day electrowinning Unit Electrowinning 100 Kg/day metal Electrowinning Cells

  8. Membrane Technology • Supported liquid membrane (6 L/h) • Reverse Osmosis, Nano-filtration & Ultra-filtration membrane integral system (1 kL/h)

  9. M/s Rubamin Pvt. Ltd. 100 tpy plant was set up for recovery of cobalt from scrap/sludge M/s Shalina Corporation Ltd. 135 tpy plant was set up for cobalt carbonate M/s S.K. Enterprises & M/s Pantnagar Fertilizers Copper and zinc from spent catalyst at 250 kg per day Major Achievements Nickel Technology Proving Plant

  10. Recovery of Nickel by Solvent Extraction

  11. Nickel Bioleaching Pilot Plant at IMMT, Bhubaneswar (10 ton) Activation of COB in Rotary Kiln One ton Nickel bioleaching of Chromite Overburden, Sukinda Bacterial Generation Tank Nickel cathode after electrowinning.

  12. Process Flowsheet

  13. Composition of the Ni-Laterite Bacterial Leach Liquor

  14. Precipitation of metal ions from Ni-laterite leach liquor using CaCO3

  15. Precipitation of Fe, Al and Cr from the Ni-laterite bacterial leach liquor with CaCO3

  16. Precipitation of Fe, Al and Cr from the Ni-laterite bacterial leach liquor with CaCO3

  17. Chemical reactions

  18. Main findings • The Ni-laterite bacterial leach liquor was processed for metal separation. • Treatment with CaCO3 at pH 4.4 precipitated 100% Fe, 96.98% Al, and 70.42% Cr. • The remaining Al and Cr was precipitated at pH 5.4 using 50% NH3 solution leading to quantitative precipitation of Al and Cr with minor losses of Ni, Co and Mn. • Extraction of all the metal ions increased with increasing equilibrium pH and extractant concentration. • Stripping of all the Metal-LO was carried out with H2SO4.

  19. Extraction of Zn

  20. Effect of equilibrium pH on extraction of Zn with 0.1M TOPS-99

  21. Plot of Log DZn vs. equilibrium pH

  22. Effect of [TOPS-99] on extraction of Zn

  23. Plot of LogDZn vs. Log [TOPS-99]

  24. McCabe-Thiele plot for extraction of Zn with 0.1M TOPS-99

  25. Stripping of Zn-LO with H2SO4

  26. McCabe-Thiele plot for stripping of Zn-LO with 15 kg/m3 H2SO4

  27. Main findings • Extraction of Zn • It was carried out with 0.1M TOPS-99 in 3-stages at O:A ratio of 1:4. The Zn-LO contained 0.321 kg/m3 Zn leading to 97.9% extraction. • Stripping of Zn-LO was carried out with 15 kg/m3 H2SO4 in 2-stages at O: A ratio of 9:2.

  28. Extraction of Mn

  29. Extraction of Mn (contd.)

  30. Main findings • Extraction of Mn • It was carried out with 0.04M NaTOPS-99 in 2-stages at 1:1 phase ratio. The LO contained 0.1573 kg/m3 Mn leading to 93.34% extraction. • The Mn-LO was stripped with 15 kg/m3 H2SO4 in 2-stages at O:A ratio of 9:1. The strip solution contained 1.4157 kg/m3 Mn.

  31. Effect of equilibrium pH on extraction of cobalt with 0.005 M NaCyanex 272

  32. Plot of Log DCo vs. equilibrium pH.

  33. Effect of [Extractant] on extraction of cobalt

  34. Plot of Log DCo Vs. Log[Cyanex 272]

  35. McCabe-Thiele plot for extraction of cobalt using 0.0125M Cyanex 272

  36. Scrubbing off Ni from the Co-LO with CoSO4 solution at 1:1 phase ratio.

  37. Scrubbing off Ni from Co-LO with CoSO4 solution at O:A =10:1

  38. Scrubbing off Ni from the Co-LO with 7.5 kg/m3 CoSO4 at different O:A ratios

  39. Stripping of Co-LO with H2SO4.

  40. McCabe-Thiele plot for stripping of Co-LO with 60 kg/m3 H2SO4

  41. Stripping of Co-LO with oxalic acid

  42. McCabe-Thiele plot for stripping of Co-LO with 1.5 N oxalic acid

  43. Main findings • Extraction of cobalt • It was carried out with 0.0125M Cyanex 272 in 3-stages at 1:1 phase ratio. The LO contained 0.0169 kg/m3 Co and 0.0205 kg/m3 Ni. • The scrubbing off Co-LO with 12.5 kg/m3 CoSO4 solution at O:A ratio of 10:1 expelled 0.02 kg/m3 Ni. The 0.75 kg/m3 Co-LO was stripped to 94.5% with 60 kg/m3 H2SO4 in 2-stages at O:A ratio of 10:1. • The Co-LO was also stripped with 1.5 N oxalic acid in 2-stages at O:A ratio of 4:1. The stripping was 97.16%.

  44. Extraction of Ni

  45. Effect of equilibrium pH on extraction of Ni& Plot of Log DNi Vs. equilibrium pH

  46. Effect of [Extractant] on extraction of Ni & Plot of Log DNi Vs. Log[Extractant]

  47. McCabe-Thiele plot for extraction of Ni with 0.12M NaD2EHPA & Stripping of Ni-LO

  48. COB leach liquor (pH 1.84) Precipitation with CaCO3 (pH 4.4) Filtrate Precipitation with NH4OH(pH 5.4) 0.1M TOPS-99 Filtrate Stripping with H2SO4 ZnSO4 SX of Zn 0.04M NaTOPS-99 Stripping with H2SO4 SX of Mn MnSO4 0.0125 M Na Cyanex 272 Stripping with H2SO4 SX of Co CoSO4 0.12 M NaTOPS-99 SX of Ni Stripping with H2SO4 NiSO4 A Conceptual Flow sheet for Processing of Overburden Leach Liquor to recover of Zn, Mn, Co and Ni values.

  49. Other Relevant activities • Treatment of complex sulphide • Copper converter slag • Recovery of metal values from cobalt cake (Cu, Ni, Co, Zn by SX) • Nickel extraction • Polymetallic nodule • Solvent extraction of uranium from phosphoric acid

  50. Metallurgy of Deep-sea Manganese Nodule of Indian Ocean Pilot Plant at Udaipur Ni-Co SX Section Mining site ~2000 km from the nearest Indian Port Nodule distribution : 7-10 kg/m2

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