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CHAPTER 3: SOLID – LIQUID

EXTRACTION / LEACHING

CHAPTER / CONTENT

Introduction to Leaching Process
Principles of Leaching
Single Stage Calculation
Multi Stage Countercurrent system

Leaching equipment

Introduction to Leaching Process
Widely used in the metallurgical, natural product and food industries
under batch, semi – continuous or continuous condition.
The major difference between Leaching and LLE centers about the
difficulty to transport the solid or the solid slurry from stage to stage.

Leaching is also known as solid – liquid exraction
In leaching, to separate the desired solute constituent or remove the
undesirable solute component from the solid phase, the solid is contacted with
a liquid phase.
The two phases are in intimate contact and the solute or solutes can diffuse
from the solid to the liquid phase, which causes a separation of the
components originally in the solid.
This process is called liquid – solid leaching or simply leaching

Introduction to Leaching Process

Leaching process for biological substances
An important such process is to leach sugar from sugar beets with hot water.
In production of vegetable oils, organic solvents such as hexane, acetone and
ether are used to extract the oil from peanuts, soybeans, flax seeds, castor beans,
sunflower seeds, etc.

In pharmaceutical industry, many different pharmaceutical products are
obtained by leaching plan roots, leaves and stems.
For ‘instant’ coffee, ground roasted coffee is leached with water and soluble tea
is produced by water leaching of tea leaves.
Tannin is removed from tea barks by leaching with water.

Introduction to Leaching Process
Leaching process for inorganic and organic materials
Used in metal – processing industries
In metal ores, the desired metal components usually occur with a large amount
of undesirable constituents and leaching is used to obtain these metal
components in the form of metal salts.
E.g.: Copper salts are leached by dissolving raw copper ores by using sulfuric
acid or ammoniacal solutions.
E.g.: Nickel salts are leached using sulfuric acid – ammonia – oxygen mixures.
Gold is leached using an aqueous sodium cyanide solution.

the rate of transfer of the solvent into the solid can be rather slow or rapid.Principles of Leaching The solvent must be transferred from the bulk solvent solution to the surface of the solids. . Finally. The rate of the solvent transfer from the bulk solution to the solid surface is quite rapid. This solvent transfer usually occurs initially when the particle are first contacted with the solvent. the solute is transferred to the bulk solution. Next. The solute then diffuses through the solid solvent mixture to the surface of the particle. However. the solvent must penetrate or diffuse into the solids.

The resistance to mass transfer to the solute from the solid surface to the bulk solvent is generally quite small compared to the resistance to the diffusion within the solid itself. . If the solid is made of porous the diffusion through the porous solid can be described by an effective diffusivity.Principles of Leaching The rate of diffusion of the solute through the solid and solvent to the surface of the solid is often the controlling resistance in the overall leaching process and can depend on a number of different factors.

Calculation in Leaching SINGLE – STAGE LEACHING COUNTER – CURRENT MULTISTAGE LEACHING .

y1.Single – stage Leaching Process flow Overflow solution V1. x2 Underflow solution L1. solute – free solid. N0. N1. B Mass of overflow solution xA Composition of A at overflow solution Mass of liquid in slurry solution yA Composition of A at slurry solution Mass of dry. Mass of dry.solute (B)/Mass of solution retained (L) Material balance is divided into 3 parts: Totalsolution balance L0 y A0  V2 x A2  L1 y A1  V1 x A1  MxAM Comp. A balance Solid balance B  N 0 L0  0  N1 L1  0  N M M L0  V2  L1  V1  M . x1 Feed Slurry L0. y0. B V L B N Solvent Feed V2.

100 kg of soybean containing 20 wt% oil is leached with 100 kg of fresh hexane solvent.Single – stage calculations Example 1 In a single – stage leaching of soybean oil from flaked soybeans with hexane.5 kg insoluble solid/kg solution retained. . Calculate the amounts and compositions of the overflow V1 and the underflow slurry L1 leaving the stage. The value of N for the slurry underflow is essentially constant at 1.

y0. N0. B Information given: Feed slurry = 100 kg containing 20 wt% oil Entering solvent.5 kg B/kg (A+C) . y1. B Solvent Feed V2. x1 Feed Slurry L0.Single – stage calculations Solution 1 Overflow solution V1. x2 Underflow solution L1. N1. V2 = 100 kg N = 1.

20 x 100 A = 20 kg Mass of B = 0.0 .0 L0 A  C 20  0 Coordinate for L0 (yA0 .80 x 100 B = 80 kg Mass of C = 0 kg C = 0 kg y A0  A A 20    1.Single – stage calculations Solution 1 Find coordinate at L0. 4. N0) = (1.0 L0 A  C 20  0 N0  B B 80    4. Mass of A = 0.0) .

N2) = (0 .Single – stage calculations Solution 1 Find coordinate at V2. 0) . Mass of A = 0 A = 0 kg Mass of B = 0 B = 0 kg Mass of C = 100 kg C = 100 kg x2  A A 0   0 V2 A  C 0  100 N2  B B 0   0 V2 A  C 0  100 Coordinate for V2 (x2 .

0  1000  120x AM x AM  0.Single – stage calculations Solution 1 From material balance calculations: Total solution balance: L0  V2  L1  V1  M 20  100  M M  120 kg Component A balance: L0 y A0  V2 x A2  MxAM 201.167 .

Construct straight vertical line through point M in order to find value V1 and L1 .167 . NM) = (0.Single – stage calculations Solution 1 Solid balance: B  N 0 L0  N1 L1  N M M N 0 L0  N M M 420  N M 120 N M  0.667 Coordinate for M (xM . 0.667) Plot coordinate M in the graph.

2 0.5) 0.5 2 N versus y A L1 1. N1) = (0.5 3 N 2. y A From figure. 0) Coordinate for L1 (y1 .5 N versus x A V1 0 0 V2 0.167 .6 x A.4 0. Coordinate for V1 (x1 .Single – stage calculations Solution 1 L0 4 3. N1) = (0.5 1 M 0.8 1 . 1.167 .

1 Solid balance: B  N 0 L0  N1 L1  N M M N1 L1  N M M 1.667120 L1  53.Single – stage calculations Solution 1 From material balance calculations: Total solution balance: L1  V1  M L1  V1  120 V1  120  L1  Eq.5L1   0.36 kg .

(1) V1  120  L1 V1  120  53.64 kg .36  Eq.Single – stage calculations Solution 1 From material balance calculations: From Eq.1 V1  66.

5 min break… .

This slurry contacted with 100kg of pure hexane in a single stage so that the value of N for the outlet underflow is 1.5kg insoluble solid/kg solution retained. .9-2-Textbook. Determine the amount and compositions of the overflow V1 and the underflow L1 leaving the stage.Tutorial: 12. page 835 A slurry of flakes soybeans weighing a total of 100kg contains 75kg of inert solids and 25kg of solution with 10wt% oil and 90wt% solvent hexane.

6) Coordinate V1 (0.0) Coordinate L1 (0. 0.5) L1= 50 kg V1=75 kg .0) Coordinate V2 (0.0) Coordinate M (0.02.1.02.1.02.Answer: Coordinate Lo (0. 3.

N1. L1 + V1 = M V1= 125-L1 Solid balance.Solution balance.L1=B 1.5 (L1)=75 L1=50 kg Therefore V1=125-50 = 75kg .

. The solvent feed is 80 kg of solvent containing 3 wt% of soybean oil. 100 kg of soybean containing 22 wt% oil is leached with hexane.9-1 In a single – stage leaching of soybean oil from flaked soybeans with hexane. The value of N for the slurry underflow is essentially constant at 1. Calculate the amounts and compositions of the overflow V1 and the underflow slurry L1 leaving the stage.Example 12.5 kg insoluble solid/kg solution retained.

xA yA Composition of A at overflow solution Composition of A at slurry solution . x1 Underflow solution Feed Slurry LN. B L0. N0.Multi – stage counter current Leaching Process flow Overflow solution Solvent Feed VN+1. solute – free solid. yN. NN. y0. xN+1 V1. B V L B Mass of overflow solution Mass of liquid in slurry solution Mass of dry.

The slurry phase L composed of inert solid (B) and liquid phase of A and C is the continuous underflow from each stage.Multi – stage counter current Leaching The ideal stages are numbered in the direction of the solids or underflow stream. and it dissolves solute as it moves along. The solvent (C) – solute (A) phase or V phase is the liquid phase that overflows continuously from stage to stage countercurrently to the solid phase. The flow rate of solid is constant throughout the process . Composition of V – denoted by x Composition of L – denoted by y Assumption: The solid B is insoluble and is not lost in the liquid V phase.

A balance Solid balance .Multi – stage counter current Leaching L0  VN 1  LN  V1  M Totalsolution balance L0 y A0  VN 1 x AN 1  LN y AN  V1 x A1  MxAM B  N 0 L0  N N LN  N M M Comp.

The leached solids are to contain 120 kg oil. The inlet flow per hour of fresh solvent mixture contains 1310 kg benzene and 20 kg oil. Data (B3) are tabulated below as N kg inert solid B/kg solution and yA kg oil A/kg solution Calculate the amounts and concentrations of the stream leaving the process and the number of stages required. .Multi – stage counter current Leaching Example 2 A continuous countercurrent multistage system is to be used to leach oil from meal by benzene solvent (B3). The process is to treat 2000 kg/h of inert solid meal (B) containing 800 kg oil (A) and also 50 kg benzene (C).

NN. B Information given: Feed slurry (L0): A = 800 kg/h B = 2000 kg/h C = 50 kg/h Entering solvent (VN+1 ) A = 20 kg/h B = 0 kg/h C = 1310 kg/h . B L0. N0. x1 Underflow solution Feed Slurry LN. xN+1 V1.Multi – stage counter current Leaching Solution 2 Overflow solution Solvent Feed VN+1. yN. y0.

xN+1 V1. NN. B Information given: Underflow solution (LN): A =120 kg/h B = 2000 kg/h C = ?? kg/h . N0. B L0. y0. x1 Underflow solution Feed Slurry LN. yN.Multi – stage counter current Leaching Solution 2 Overflow solution Solvent Feed VN+1.

Mass of A = 800 kg/h Mass of B = 2000 kg/h Mass of C = 50 kg/h y A0  A A 800 800     0.35 L0 A  C 800  50 850 Coordinate for L0 (yA0 . N0) = (0.94 L0 A  C 800  50 850 N0  B B 2000 2000     2.94 . 2.Multi – stage counter current Leaching Solution 2 Find coordinate at L0.35) .

0) .015 .015 A  C 20  1310 1330  B 0  0 A  C 20  1310 Coordinate for VN+1 (xN+1 .Multi – stage counter current Leaching Solution 2 Find coordinate at VN+1. NN+1) = (0. Mass of A = 20 kg/h Mass of B = 0 kg/h Mass of C = 1310 kg/h xN 1  A VN 1 N N 1  B VN 1  A 20 20    0.

Multi – stage counter current Leaching Solution 2 Find coordinate at LN.67 Plot New Coordinate (x .1 = 1. 1.67 y If x = 0.67 x 0. N = 16.1. NN yN B N N LN B 2000     16.67) . N) = (0.67 A yN A 120 LN  N  16.1 . Mass of A = 120 kg/h Mass of B = 2000 kg/h Mass of C = ?? kg/h Slope of graph.

8 1 . y A 0.4 -0.4 0.6 0.2 -1 0 VN 1 0.2 -2 -3 -4 -5 -6 -7 x A.Multi – stage counter current Leaching Solution 2 3 2 LN L0 1 0 N -0.

015  2180x AM x AM  0.94  13300.Multi – stage counter current Leaching Solution 2 From material balance calculations: Total solution balance: L0  VN 1  LN  V1  M L0  VN 1  M 850  1330  M M  2180 kg Component A balance: L0 y A0  VN 1 xN 1  MxAM 8500.376 .

916 Coordinate for M (xM . Point at x – axis = V1 . 0.916) Plot coordinate M in the graph.376 . NM) = (0.35850  N M 2180 N M  0.Multi – stage counter current Leaching Solution 2 From material balance calculations: Solid balance: B  N 0 L0  N N LN  N M M N 0 L0  N M M 2. Construct line from point LN to point M until it cross at x – axis.

592 . 0) Coordinate for LN (y1 .2 N -0.0) 0. N1) = (0.Multi – stage counter current Leaching 3 LN 2 M 1 V1 0 -0. 2. y A Coordinate for V1 (x1 .4 -1 0 VN 1 0.4 -2 -3 -4 -5 -6 -7 From figure. N1) = (0.12 .6 0. L0 x A.2 0.8 1 .

592  21800.Multi – stage counter current Leaching Solution 2 From material balance calculations: Total solution balance: V1  2180  LN  Eq.592LN  819.12  V1 0.56  0. 1 into equation above LN 0.472LN  470.376 0.592  21800.376 Insert Eq.12LN  1290.62 kg .12  2180  LN 0. 1 Component A balance: LN y N  V1 x1  MxAM LN 0.88  LN  997.68 0.

38 kg Construct operating point: Connect L0 with V1 & LN with VN+1. The cross line – operating point.Multi – stage counter current Leaching Solution 2 From material balance calculations: Total solution balance: V1  2180  LN  Eq. Total stages: 4 stages .62 V1  1182.1 V1  2180  997.

6 0.Multi – stage counter current Leaching Solution 2 Construct the stages: 3 LN 2 L3 N -1 0 VN 1 0. y A 0.2 L1 M 1 -0.2 -2 -3 -4 -5 P L0 V1 0 -0.8 1 .4 L2 -6 -7 x A.4 0.

5 min break…. .

where N is kg inert solid/kg solution retained and yA is kg oil/kg solution . The feed rate is 1000 kg of fresh livers per hour.Tutorial 12. The final exit overflow solution is to contain 70 wt% oil. The retention of solution by inert solids (oil free liver) of the liver varies as follow. page 835 Fresh halibut livers containing 25.10-4 Textbook.7 wt% oil are to be extracted with pure ethyl ether to remove 95 % of the oil in a countercurrent multistage leaching process.

page 835 .Tutorial 12.10-3 Textbook.

Types of Equipments for Leaching FIXED – BED LEACHING MOVING BED LEACHING AGITATED SOLID LEACHING .

The leached sugar solution flows out the bottom onto the next tank in series. extraction of pharmaceuticals from barks and seeds and other processes. The cover is removable so that sugar beet slices called cossettes can be dumped into the bed.Fixed – Bed Leaching Used in beet sugar industry and is also used for extraction of tanning extracts from the tanbark.8-1 shows a typical sugar beet diffuser or extractor. . About 95% of the sugar in beets is leached to yield an outlet solution from the system of about 12 wt%. Figure 12. Heated water at 344 K to 350 K flows into the bed to leach out the sugar.

sometimes precooked. Used widely in extracting oil from vegetable seeds such as cottonseeds. . often partially dried and rolled or flaked. The solvents used are particularly hydrocarbons such as hexane and the final solvent – vegetable solution called miscella may contain some finely divided solids. peanuts and soybeans. The seeds are usually dehulled first.Moving – Bed Leaching There are number of devices for stagewise countercurrent leaching where the bed or stages moves.

Sometimes thickeners are used as combination contactor – agitators and settlers – shown in Figure 12.Agitated Solid Leaching When the solid can be ground fine abou 200 mesh (0.8-3. Continuous countercurrent leaching can be accomplished by placing the number of agitator in series. . it can kept in suspension by small amounts of agitation. with setttling tanks or thickeners between each agitator.074 mm).

or material balance relation and the equilibrium relations between the two streams are needed as in LLE. .Equilibrium Relations in Leaching To analyze single – stage and countercurrent – stage leaching. * This means the solution in the liquid phase leaving a stage is the same as the solution that remains with the solid matrix in the settled slurry leaving the stage. The solute in the entering solid dissolved completely in the first stage. The solid – liquid stream is called underflow or slurry stream. an operating line equation. The settled solid leaving a stage always contains some liquid in which dissolved solids is present. No adsorption of the solute by the solid. Assumptions made by achieving the equilibrium relations: Sufficient solvent is present so that all the solute in the entering solid dissolved in the solvent.

Equilibrium Relations in Leaching Consequently. N = 0 For underflow. Equilibrium diagrams for leaching: The concentration of inert or insoluble solid B in the solution mixture or the slurry mixture can be expressed in kg (lbm) units: N kg B kg solid lb solid   kg A  kg C kg solution lb solution For overflow. N value depending on the solute concentration in the liquid. The amount of solution retained with the solids in the settling portion of each stage may depend the density and viscosity of liquid in which the solid is suspended. . the concentration of oil or solute in the liquid or overflow stream is equal to the concentration of solute in the liquid solution accompanying the slurry or underflow stream.

Equilibrium Relations in Leaching The composition of solute A in liquid will be expressed as wt fractions: xA  kg A kg solute overflow liquid  kg A  kg C kg solution yA  kg A kg solute  kg A  kg C kg solution  liquid in slurryor    underflow liquid   .

QUIZ 2 45 minutes .

The leached solids are to contain 120 kg oil. determine a) The exit flows compositions (xA1. b) Number of stages required . The inlet flow per hour of fresh solvent mixture contains 1310 kg benzene and 20kg oil.QUIZ 2 (45 minutes) A continuous countercurrent multistage system is to be used to leach oil from meal by benzene solvent. overflow V1 and the underflow LN leaving the stage. If the value of N for the outlet underflow is constant at 1. The process is to treat 2000 kg/h of inert solid meal containing 800 kg oil and also 50kg benzene.85kg solid/kg solution. yAN.