Solid-Liquid Extraction Engr. Elisa G. Eleazar CHE135-1P: SEPARATION PROCESSES 1 Outline Mechanism 1. 2. 3. Representation of Equilibrium Data Equilibrium Stage Model for Leaching Learning Objectives Explain the mechanism of Solid-Liquid Extraction Perform equilibrium and material balance calculations for Liquid-Liquid Extraction Perform solid-liquid extraction calculations CHE135-1P: SEPARATION PROCESSES 2 Mechanism Solid-Liquid Extraction (Leaching) involves the removal of a soluble fraction (solute or leachant) of a solid material by a liquid solvent Overflow solvent + most of the solute Underflow solids wet with almost pure solvent CHE135-1P: SEPARATION PROCESSES Wash Stages used to reduce the concentration of solute in the liquid portion of the underflow The solute diffuses from inside the solid into the surrounding solvent. Applications: • Removal of copper from ore using sulfuric acid • Extraction of sugar beets using hot water • Recovery of proteins and other natural products from bacterial cells 3 Representation of Equilibrium Data Ponchon-Savarit Diagram Right Triangle Diagram 6 1 0,9 kg inert/kg soln 5 0,8 0,7 4 0,6 Xsolvent 3 0,5 0,4 2 0,3 0,2 1 0,1 0 0 0,1 0,2 0,3 0,4 0,5 kg solute / kg soln CHE135-1P: SEPARATION PROCESSES 0,6 0,7 0,8 0 0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1 Xsolute 4 Representation of Equilibrium Data The experimental data on the retention of oil by livers are given below. Construct (a) right triangular diagram; (b) Ponchon-Savarit diagram for the system. kg liver oil in 1 kg solution kg solution in 1 kg oil-free liver CHE135-1P: SEPARATION PROCESSES 0 0.10 0.20 0.30 0.40 0.50 0.60 0.65 0.70 0.72 0.205 0.242 0.286 0.339 0.405 0.489 0.600 0.672 0.765 0.81 5 Equilibrium Stage Model for Leaching Assumptions: • The solid feed consists of a solute that is completely soluble in the solvent and an inert substance that is not. • Leaching is rapid such that it is completed in a single leaching stage. • All overflow streams are assumed to be free of solids. CHE135-1P: SEPARATION PROCESSES S Mass flow rate of inert solids V Mass flow rate of entering solvent or overflow liquid L Mass flow rate of underflow liquid y Mass fraction of solute in the overflow x Mass fraction of solute in the underflow If conditions of equilibrium are met, the concentration of the solution leaving a stage is the same as the concentration of the solution adhering to the inerts. The equilibrium relationship is, therefore, xe = ye. 6 Equilibrium Stage Model for Leaching An ideal leaching or washing stage is one where: Any entering solid solute is completely dissolved into the liquid in the stage (assuming that the liquid contains sufficient solvent). The composition of the liquid in the stage is uniform throughout, including any liquid within pores of the inert solid. Solute is not adsorbed on the surfaces of the inert solid. The inert solids leaving in the underflow from each stage are wet with liquid, such that the mass ratio of solvent in that liquid (or the total liquid) to inert solids is constant from stage to stage. Because the composition of the liquid in the stage is uniform throughout, the concentration of solute in the overflow is equal to that in the liquid portion of the underflow (equilibrium assumption). Overflows contain no solids. Solvent is not vaporized, adsorbed or crystallized in a stage. CHE135-1P: SEPARATION PROCESSES 7 Equilibrium Stage Model for Leaching A finely divided solids feed, F, of 150 kg/h, containing 1/3 water-soluble Na2CO3 and 2/3 insoluble ash is to be leached and washed at 30ο°C in a two-stage, countercurrent system with 400 kg/h of water. The leaching stage consists of an agitated vessel that discharges the slurry into a thickener. The washing stage consists of a second thickener. Experiments show that the sludge underflow from each thickener will contain 2 kg of liquid (water and carbonate) per kg of insoluble ash. Assume ideal stages. a. Calculate the percent recovery of carbonate in the final extract. b. If a third stage is added, calculate the amount of additional carbonate that will be recovered. CHE135-1P: SEPARATION PROCESSES 8 Equilibrium Stage Model for Leaching In the previous example (part b), leaching was assumed to be completed in one stage, with two additional stages provided for washing. The recovery of the solute in the extract was 89.8%. Recalculate this example, assuming that ½ of the carbonate is leached in the first stage and the remaining ½ on the second stage, leaving only the last stage as a true washing stage. CHE135-1P: SEPARATION PROCESSES 9 Equilibrium Stage Model for Leaching Graphical Solution Using Ponchon-Savarit Diagram XC,yc mass fraction solvent yN+1 Difference Point: yA3 πΌππ‘πππ πππ‘πππ: πΏ0 ππΏ πππ πΏπ ππ+1 yA2 yA1 π 1 ο xN xA3 xA2 xA1 From VL, draw a vertical line to the underflow locus: xA0 Connect R1 and ο πΌππ‘πππ πππ‘πππ π€ππ‘β ππππ’π : π2 XA,yA mass fraction solute ο CHE135-1P: SEPARATION PROCESSES 10 Equilibrium Stage Model for Leaching Graphical Solution Using Ponchon-Savarit Diagram Oil is to be extracted from halibut livers by means of ether. The solution retention data are given below: kg liver oil in 1 kg solution kg solution in 1 kg oil-free liver 0 0.10 0.20 0.30 0.40 0.50 0.60 0.65 0.70 0.72 0.205 0.242 0.286 0.339 0.405 0.489 0.600 0.672 0.765 0.81 Halibut livers contain 0.257 mass fraction oil. If 95% of the oil is to be extracted and the strong solution from the system is to contain 0.7 mass fraction oil, determine: a. quantity and composition of discharged solids b. kg of ether (oil-free) required to treat 1,000 kg of feed c. number of ideal stages required d. number of actual stages required if the stage efficiency is 70% CHE135-1P: SEPARATION PROCESSES 11 Equilibrium Stage Model for Leaching McCabe-Smith Graphical Solution CHE135-1P: SEPARATION PROCESSES 12 Equilibrium Stage Model for Leaching McCabe-Smith Graphical Solution Two tons (4,000 lb) per day of waxed paper containing 25 wt% soluble wax and 75 wt% insoluble pulp are to be dewaxed by leaching with kerosene in a continuous, countercurrent contacting system. The wax will be completely dissolved by the kerosene in the leaching stage L. Subsequent washing stages will be used to reduce the wax content in the liquid adhering to the pulp leaving the last stage N, to 0.2 lb wax/100 lb pulp. The kerosene entering the system is recycled from a solvent-recovery system and contains 0.05 lb wax per 100 lb kerosene. The final extract is to contain 5 lb wax per 100 lb kerosene. Experiments show that the underflow from each stage will contain 2 lb kerosene per lb insoluble pulp. Determine the number of washing stages required. CHE135-1P: SEPARATION PROCESSES 13 Equilibrium Stage Model for Leaching McCabe-Smith Algebraic Solution When the solution retained by the inerts is constant: π₯π − π¦π+1 log π¦πΏ − π¦1 π= π¦1 − π¦π+1 log π¦πΏ − π₯π use mass fractions and total liquid flow rates CHE135-1P: SEPARATION PROCESSES When the solvent retained by the inerts is constant: ππ − ππ+1 log ππΏ − π1 π= π1 − ππ+1 log ππΏ − ππ use mass ratios and solute-free solvent flow rates 14 Equilibrium Stage Model for Leaching McCabe-Smith Algebraic Solution Determine the number of ideal, continuous, countercurrent washing stages for the previous example using McCabe-Smith Algebraic solution. CHE135-1P: SEPARATION PROCESSES 15 Equilibrium Stage Model for Leaching McCabe-Smith Algebraic Solution A countercurrent extraction system is to treat 100 kg/min of sliced sugar beets with fresh water as solvent. Analysis of the beets is as follows: water 48% sugar 12% pulp 40% If 97% sugar is to be recovered and the extract phase leaving the system is to contain 15% sugar, determine the number of cells required: a. if each kg of dry pulp retains 3 kg of solution b. if each kg of dry pulp retains 3 kg of water CHE135-1P: SEPARATION PROCESSES 16 Outline Mechanism 1. 2. 3. Representation of Equilibrium Data Equilibrium Stage Model for Leaching Learning Objectives Explain the mechanism of Solid-Liquid Extraction Perform equilibrium and material balance calculations for Liquid-Liquid Extraction Perform solid-liquid extraction calculations CHE135-1P: SEPARATION PROCESSES 17 Solid-Liquid Extraction Engr. Elisa G. Eleazar CHE135-1P: SEPARATION PROCESSES 18