Solid - liquid extraction_4

Solid liquid extraction calculation : Counter current contact 2

• N stage countercurrent extraction cascade

• flow rates are expressed on solid free basis

• solution concentrations in overflow and underflow are given in mass fraction of solute on
solid free basis [ XC or YC ] kg C / kg (B+C)

Final
Feed Under flow

Final
overflow Solvent
Solid liquid extraction calculation : Counter current contact 3
For Envelope 1 (1 to N stages)
xCF
X CF =
• Solid free mass balance of (B+C) F   S   LN  V1  M  (9.9a) x BF + xCF
yCS
YCS =
• Solute C balance: F  X C F   S  YC S   LN X C LN  V1 YCV1  M  X C M  (9.9b) yBS + yCS

M' = total amount of non-solid that is solvent (B) and solute (C) entering cascade

F X C F   S YC S 
XCM' = mass fraction of solute in M’ XC M  (9.10)
F   S
Final
Feed Under flow

Final
overflow Solvent
Solid liquid extraction calculation : Counter current contact 4
Envelope II (first n stages)
• mass balance equation for (B + C) F   Vn1  Ln  V1 (9.11)

Difference point
(for Envelop I) F   S   LN  V1  M  (9.9a)
F   V1  LN  S   

(for Envelop II), using Eq. 9.11, F   V1  Ln  Vn1  LN  S    (9.12)

• Here Δ is difference point

Under flow

Feed

overflow

Solvent
Solid liquid extraction calculation : Counter current contact 5

F   V1  Ln  Vn1  LN  S    (9.12)

• point Δ is intersection point of lines F’ V‘1’ and L’N S'

• points L'n and V'n (equilibrated points ) lie at terminal of tie

line for all ideal stages n
• L'n-1 and V'n : operating points (concentration of streams
entering or leaving a stage)

Under flow

overflow Solvent
Solid liquid extraction calculation : Counter current contact 6
Determination of number of Ideal stages

• equilibrium data used to plot underflow and overflow

curves

• Locate points F‘, S' and L'N on Ponchon-Savarit

diagram

• L’N located at final underflow composition XCN

xCN
X CN 
x BN  xCN
Solid liquid extraction calculation : Counter current contact 7
Determination of number of Ideal stages

F X C F   S YC S 
• points M' located on F'S‘ at XC M 
F   S

• L'NM' is joined and extended to meet overflow curve at

point V'1
Solid liquid extraction calculation : Counter current contact 8

• F’ V'1 and L’N S’ lines drawn and extended to intersect

at difference point Δ
Solid liquid extraction calculation : Counter current contact 9

• Vertical line through V'1 is drawn to have Tie line V'1 L'1
Solid liquid extraction calculation : Counter current contact 10

• Join Δ and L'1 (for stage n=1)

• line Δ L'1 (operating line for n=1) intersects overflow

curve at V'2 (L'1 , V'2 operating points)
Solid liquid extraction calculation : Counter current contact 11

• Draw vertical tie line from V'2 which intersects underflow

curve at L'2

• Join Δ and L‘2 to get operating line for stage n=2

• Operating line ΔL‘2 (n=2) intersect overflow curve at V’3

• Proceeding similarly number of stages can be determined

for L’N
Example 12
• Crushed oil seeds containing 28 mass% oil is to be extracted with hexane to reduce oil content
to 0.8% in underflow. One Kg of solvent is used per kg of the feed. Determine the number of
stages required.

Equilibrium data :
Overflow(100 kg), solution Underflow(100 kg), slurry
WA (kg) WB (kg) WC(kg) W'A (kg) W'B(kg) W'C(kg)

0.3 99.7 0.0 67.2 32.8 0.0

0.45 90.6 8.95 67.1 29.94 2.96
0.54 84.54 14.92 66.93 28.11 4.96
0.70 74.47 24.83 66.58 25.06 8.36
0.77 69.46 29.77 66.26 23.62 10.12
0.91 60.44 38.65 65.75 20.9 13.35
0.99 54.45 44.56 65.33 19.07 15.6
1.19 44.46 54.35 64.39 16.02 19.59
1.28 38.50 60.22 63.77 14.13 22.10
1.28 34.55 64.17 63.23 12.87 23.90
1.48 24.63 73.89 61.54 9.61 28.85
 13
• Basis : Feed = 100 kg ; Solvent 100 kg
Feed : solvent = 1:1

F = 100 Kg (28% oil)

F’= 28 Kg Solid free basis

XCF’ = 0.28/0.28 = 1

S = S’ = 100 kg (oil free)

YCS’ = 0 Solid free basis

ZF’ = 72 kg solid / 28 kg oil = 2.57

Solid free basis
ZS’ = 0 ( solid =0 )
 Underflow(100 kg), slurry 14
W'A (kg) W'B(kg) W'C(kg)

67.2 32.8 0.0

For Nth stage 67.1 29.94 2.96
66.93 28.11 4.96
• Underflow contains 66.58 25.06 8.36

• Oil content = 0.8 kg (0.8 % of 100 kg feed )

• associated mass of solvent (obtained by linear interpolation of given data) :

 32.8  29.94  
w  32.8  
'
B   0.8  32.03 kg
 2.96  

• Associated mass of carrier/meal :

wA'  100  (32.03  0.8)  67.17 kg

 w 'C w' A 15
XC  ' ZL  '
w C  w' B w C  w' B X CN , Z L' N
0.0244, 2.046
For Nth stage ( solid free basis)

• Solute content in underflow

wC' 0.8
X CN  '   0.0244
wC  wB 0.8  32.03
'

• Carrier content
X CM '  0.219
w' A 67.17
Z L' N  '   2.046
w C  w B 32.03  0.8
'

• For Solute concentration in overall mixed stream M’

X CM ' 
 28 1.0   0
 0.219
100  28
 16

• Locate points F’(1, 2.57), and S’(0, 0)

• locate L’N on underflow curve for XCN = 0.0244. (ZL’N=2.046)

• Join S’F’

• locate point M’ on S’F’ at XCM’ = 0.219

• Join L’N M’ and extend it to meet overflow line at V’1

• L’N S’ and F’V‘1 lines are joined and extended to meet at the

difference point ∆.
 17
• number of stages determined by graphical construction

• Draw vertical tie line through V’1 to meet underflow line at L’1

• Join L’1 ∆ that intersects overflow line at V‘2 and so on

• Number of stages : 3
Solid liquid contacting strategy 18
• Solid liquid contacting is broadly of two types
• fix bed contact
• dispersed contact in agitated tank or vessel

Fixed bed contacting

• simplest equipment
• open or closed vessel with perforated support plate placed near bottom
• solid rest on support plate
• Liquid is fed at top of bed
• Fixed bed contacting main key of two types
• percolation
• full immersion
Fixed bed contacting 19
1. Spray percolation
• liquid is distributed at top and trickles down through bed of solid

• solvent is recirculated till

• certain solute concentration is reached in solvent
or
• solute concentration in bed reduces to desired extent

• Disadvantage :
• channeling of solvent through bed
• extraction remains incomplete on poor contact of bed with
solvent
Fixed bed contacting 20
2. Full immersion
Two ways :

1. solid is kept dipped in liquid for predetermined

time and drained thereafter
• used solvent is taken for recovery of solute

2. solvent enters packed bed of solid

continuously at bottom and leaves at top
keeping bed fully immersed
• Recycling of solution is done if necessary
Dispersed Contacting 21
• Solid and extracting solvent are agitated in a vessel of suitable shape, size and design

• Different types of agitators are in use depending upon characteristics of solid

• Solid-liquid contacting is followed by separation of inert from solution and recovery of product
from solution
Solid liquid contacting equipment 22

• Solid liquid contacting done in :

• batch equipment

• continuous equipment
Batch equipment 23
• percolation leaching (fixed bed contacting) is batch process

• Used for oil extraction from seeds

• Mechanically agitated tank used

• Number of tanks arranged in series to form batch contact battery

• After extraction is complete, miscella (oil, solvent and some solid),

is removed

• Residual solvent in exhausted meal recovered by passing steam Desolventizer

through it (Desolventizer)

http://www.crownironasia.com/Sections.asp?ID=40
Multi Batch extraction 24
• Each vessel is charged with solid

• Fresh solvent enters vessel containing solids having lower solute concentration

• It flows to vessel containing solutes of higher content

• At one end of battery relatively strong extract contacts a fresh batch of solid and rich liquid
from vessel is taken for further processing

• Exhausted solid leaves battery at other end

Continuous contact equipment 25
• Used in vegetable oil extraction and food process industries

• operated in countercurrent mode

Vertical basket or Bollman extractor

• Consists of number of baskets fixed to an endless chain

having a descending and ascending sections, enclosed in a
vapour-tight chamber

• Each basket has a wire mesh bottom

• Two chambers at bottom collect the liquid percolating

through baskets in two sections
Vertical basket or Bollman extractor 26
• Solid seeds fed from hopper into basket at top of descending
section

• Partially enriched solvent , half Michelle, is sprayed on this

solid

• Liquid percolates through slowly moving basket and collects

at one of bottom chamber and taken to solute recovery

• Fresh solvent is sprayed on top basket in ascending section

• This liquid percolates through rising baskets and collects in

other chamber at bottom in form of half Miscella

• This half Michelle is sprayed at top basket of descending

section as stated before

• Percolation of liquid occurs countercurrent to solid movement

in ascending section but co-current in descending section
Horizontal basket extractor 27
• Widely used for oil extraction from seeds

• Consist of train of horizontal basket fitted to a drive chain enclosed in a big chamber

• Each basket has wire mesh or perforated bottom

• Below train of moving baskets, compartments

are placed
Horizontal basket extractor 28
• When an empty basket reaches feed point, it gets loaded with solid from feed Hopper

• As loaded basket advances, it is sprayed with miscella from a bottom compartment

• Liquid percolates through solid in each basket and leaves through perforated or wire mesh
bottom and collects below

• Liquid collected from a chamber is pumped to

previous chamber giving partial countercurrent effect
Horizontal basket extractor 29
• Before a basket makes a complete turn, nearly exhausted solid is sprayed with fresh solvent

• Rich extract from collection chamber is taken out for further processing

• Exhausted solid taken out

• Device is enclosed in vapour-tight housing to avoid leakage of solvent vapour

https://youtu.be/yTlt3-puecY
Continuous belt extractor 30
• Consist of perforated endless moving belt

• Solid is fed at one end of moving belt

• Fresh solvent is fed at solid discharge end and percolates through bed of solid on the belt

• Liquid drains into catch basins placed at bottom of belt and is recirculated to top of adjacent
section of bed
• Used for extraction of sugar from sugarcane or beet

https://www.desmetballestra.com/oils-fats/extraction/solvent-extraction/lm
Rotocel Extractor 31
• Consist of rotating basket with number of cells (15 to 18) fixed to a central Rotor

• Each cell is fitted with hinged perforated screen bottom so that solvent can percolate through
solid feed

• Solvent sprayed on top of a cell

• fresh solid enters device at one end

Rotocel Extractor 32
• Below rotating shell a circular tank is placed, divided into a number of compartments, to
receive extract from one or more cells

• Miscella from a compartment is pumped and sprayed on next basket in counter current
direction

• Exhausted solid removed by opening hinged bottom

• Empty compartment continues to rotate

and then again receives fresh feed

https://youtu.be/xj5WQKSBQs8