Documenti di Didattica
Documenti di Professioni
Documenti di Cultura
SOLID-LIQUID EXTRACTION
Table of Contents
Introduction 1
Leaching Process for Biological Substances 5
Leaching Process for Inorganic and Organic Materials 5
Preparation of Solids for Leaching 6
Types of Equipment 7
Equipment Design
Design Problem 14
Design Description 14
Design Selection 14
Parts and Function 15
Data and Assumption 15
Design Considerations 16
Design Requirements 17
Design Calculation 18
Design Specification 27
LEACHING
Leaching is the process by which constituents of a solid material are released into a
contacting water phase. Although some species may be more of an environmental concern
than others, the leaching process is indiscriminant such that all constituents (e.g., major or
minor matrix components as well as inorganic, organic and radionuclide contaminants) are
released under a common set of chemical phenomena which may include mineral
dissolution, desorption and complexation, and mass transport processes. In turn, these
phenomena are affected by certain factors that can alter the rate or extent of leaching. Among
these factors are:
The process itself is universal, as any material exposed to contact with water will
leach components from its surface or its interior depending on the porosity of the material
considered.
Another term for this is lixiviation, or the extraction of a soluble particle from its
constituent parts. In a typical leaching operation, the solid mixture to be separated consists
of particles, inert insoluble carrier A and solute B. The solvent, C, is added to the mixture to
selectively dissolve B. The overflow from the stage is free of solids and consists of only
solvent C and dissolved B. The underflow consists of slurry of liquid of similar composition
in the liquid overflow and solid carrier A. In an ideal leaching equilibrium stage, all the solute
is dissolved by the solvent; none of the carrier is dissolved. The mass ratio of the solid to
liquid in the underflow is dependent on the type of equipment used and properties of the
two phases.
the semipermeable cell walls, while the undesirable albuminous and colloidal
components cannot pass through the walls.
For the leaching of pharmaceutical products from leaves, stems, and roots,
drying of the material before extraction helps rupture the cell walls. Thus, the solvent
can directly dissolve the solute. The cell walls of soybeans and many vegetable seeds
are largely ruptured when the original material are reduced in size to about 0.1mm
to 0.5mm by rolling or flaking. Cells are smaller in size, but the walls are ruptured and
the vegetable oil is easily accessible to the solvent.
Fixed-Bed Leaching
Fixed bead leaching is used in the beet sugar industry and is also used for the
extraction of tanning extracts from tanbark, for the extraction of pharmaceuticals from barks
and seeds, and in other processes. The figure shows a typical sugar beet diffuser or extractor
is shown.
The cover is removable, so sugar beet slices called cossettes can be dumped into the
bed. Heated water at 344 K to 350 K flows into the bed to leach out the sugar. The leached
sugar solution flows out the bottom onto the next tank in series. Countercurrent operation
is used in the Shanks system. The top and bottom covers are removable so that the leached
Solid-Liquid Extraction | Leaching
7
Baoas, Christine B.
PAMANTASAN NG LUNGSOD NG MAYNILA
University of the City of Manila
College of Engineering and Technology
Department of Chemical Engineering
beets can be removed and a fresh charge added. About 95% of the sugar in the beets is
leached to yield an outlet solution from the system of about 12 wt%.
Batch Stirred Tanks agitated by coaxial impellers (turbines, paddles, or propellers) are
commonly used for batch dissolution of solids in liquids and may be used for leaching fine
solids. Insofar as the controlling rate in the mass transfer is the rate of transfer of material
into or from the interior of the solid particles rather than the rate of transfer to or from the
surface of particles, the main function of the agitator is to supply unexhausted solvent to the
particles while they reside in the tank long enough for the diffusive process to be completed.
The agitator does this most efficiently if it just gently circulates the solids across the tank
bottom or barely suspends them above the bottom.
The leached solids must be separated from the extract by settling and decantation or by
external filters, centrifuges, or thickeners, all of which are treated elsewhere. The difficulty
of solids-extract separation and the fact that a batch stirred tank provides only a single
equilibrium stage are its major disadvantages.
There are a number of devices for stagewise countercurrent leaching where the bed
or stage moves instead of being stationary. These are used widely in extracting oil from
vegetable seeds such as cottonseeds, peanuts, and soybeans. The seeds are usually dehulled
first, sometimes precooked, often partially dried, and rolled or flaked. Sometimes
preliminary removal of oil is accompanied by expressions. The solvents are usually
petroleum products, such as hexane. The final solvent – vegetable solution, called miscella,
may contain some finely divided solids.
b. Bollman Extractor
In the figure, an enclosed moving-bed bucket elevator is shown. This is called the
Bollman extractor. It is a bucket-elevator unit designed to handle about 2000 to 20,000 kg/h
(50 to 500 U.S. tons/day) of flaky solids (e.g., soybeans). Buckets with perforated bottoms
are held on an endless moving belt. Dry flakes, fed into the descending buckets, are sprayed
with partially enriched solvent (“half miscella”) pumped from the bottom of the column of
ascending buckets. As the buckets rise on the other side of the unit, the solids are sprayed
with a countercurrent stream of pure solvent. Exhausted flakes are dumped from the buckets
at the top of the unit into a paddle conveyor; enriched solvent, the “full miscella,” is pumped
from the bottom of the casing. Because the solids are unagitated and because the final
miscella moves cocurrently, the Bollman extractor permits the use of thin flakes while
producing extract of good clarity. It is only partially a countercurrent device, however, and
it sometimes permits channeling and consequent low stage efficiency. Perhaps for this
reason, it is being displaced in the oil extraction industry by horizontal basket, pan, or belt
percolators.
c. Hilderbrandt Extractor
The Hildebrandt total-immersion extractor is shown in the figures. The helix surface
is perforated so that solvent can pass through countercurrently. It consists of three screw
conveyors arranged in a U shape. The screws are so designed to compact the solids during
their passage through the unit. The design offers the obvious advantages of countercurrent
action and continuous solids compaction, but there are possibilities of some solvent loss and
feed overflow, and successful operation is limited to light, permeable solids. The solids are
charged at the top right, conveyed downward, across the bottom, and then up the other leg.
The solvent flows countercurrently.
A somewhat similar but simpler design uses a horizontal screw section for leaching
and a second screw in an inclined section for washing, draining, and discharging the
extracted solids.
d. Rotocel Extractor
Rotocel extractors have all the advantages and disadvantages associated with basket
type extractors. They have an added advantage of compact size, high throughput and better
energy efficiency.
e. Kennedy Extractor
EQUIPMENT DESIGN
Design Problem
Rubber seed kernel (550.70 kg) is needed to be leached off using n-Hexane (1,652.10
kg) in order to recover the rubber seed oil which will be later be processed to produce
glycerol. Design a stirred batch extractor for this process.
Design Description
Leaching process is the removal of a solute constituent from a solid, by contacting the
solid with a liquid phase which is the solvent. The two phases are in intimate contact and the
solute(s) can diffuse from the solid to the liquid phase which results in the complete
separation of the components which are originally in the solid (Geankoplis, 2003). A batch
stirred tank extractor is used to recover the oil component of rubber seed kernels using n-
Hexane as solvent. The process is conducted at 50oC for a total contact time of 2 hours.
Design Selection
The tank is cylindrical with torispherical top and bottom since it’s dealing with
solution under ambient temperature and the inner pressure is less than 150 psig.
Torispherical heads are used under inner pressure that is less than 150 psig according to
Silla, H. (pg.281). Pitched-blade turbine with four blades at 45o is used due to its application
for liquids or suspensions containing small particles (Principles of Transport Processes and
Unit Operations by Geankoplis, 3rd Edition, pg. 142).
Parts Functions
Converts electrical energy into mechanical energy that is
Motor
transmitted to the impeller through the shaft
Impeller and Shaft Provides uniform mixing to the mixture
Outlet Exit Stream
Solids Inlet Inlet of solid reactants
Liquid Inlet Solvent inlet
Tank Consists of the shell and torispherical head and bottom
Leg Provides support to the whole vessel
Data and Assumptions
1. The feed rate of ground rubber seed kernel is 550.70 kg per batch.
2. The feed rate of n-Hexane is 1,652.10 kg (2.5m2) per batch.
3. The density of the ground rubber seed kernel is 0.480 g/cm3 or 480 kg/m3.
4. The density of n-Hexane is 0.660 g/cm3 or 660 kg/m3.
5. The reaction temperature is 50oC and the residence time is 120 minutes.
Solid-Liquid Extraction | Leaching
15
Baoas, Christine B.
PAMANTASAN NG LUNGSOD NG MAYNILA
University of the City of Manila
College of Engineering and Technology
Department of Chemical Engineering
Design Considerations
1. A vertical cylindrical tank with torispherical top and bottom is chosen since this type
of closure is the most commonly used end enclosure for vessels up to operating
pressure of 10 bar. (Chemical Engineering Design, Sinott (2005), Volume 6, Fourth
Edition, pg. 817)
2. The height of the tank body to internal diameter ratio is 1:1. (Unit Operations of
Chemical Engineers, McCabe et. al. (2001), 6th Edition, pg. 241)
3. For a torispherical head, the crown radius, L, is equals the inside diameter, D, of the
cylindrical vessel. (Table 10-65, Silla (2003), pg. 10-140)
4. Type 302 Stainless Steel (18% Cr, 9% Ni, 0.15% Cmax) is chosen since it is primarily
used for general process equipment. (Plant Design and Economics for Chemical
Engineers by Peters and Timmerhaus, 4th Edition, Table 4, pg. 426)
5. The number of baffles is usually 4. (Unit Operations of Chemical Engineers, McCabe et.
al. (2001), 6th Edition, pg. 241)
6. Impeller’s rotational speed, N = 200 rpm. (Principles of Transport Processes and Unit
Operations by Geankoplis, 3rd Edition, pg. 142)
7. The corrosion allowance is 2.0 mm. (Chemical Engineering Design, Sinnott (2005),
Volume 6, Fourth Edition, pg. 813).
8. The efficiency of the double-welded butt joint is 80% based upon a material factor Fm
of 1.00. This type of welded joint was selected because the are stronger than single-
welded joints and may be used for either longitudinal or circumferential seams.
(Process Equipment Design, Hesse and Rushton, pg. 84)
9. A 20% factor of safety for batch reactor. (Plant Design and Economics for Chemical
Engineers, Timmerhaus, 4th Edition, pg. 37)
10. The filling capacity of the reactor is 80% of the volume, measured at the top tangent
line to allow vapor space. (Rules of Thumb for Chemical Engineers, Hall, 5th Edition, pg.
150)
Design Requirements
1. Batch Time
2. Capacity of the Tank
3. Tank Diameter
4. Tank Height
5. Shell Thickness
6. Head and Bottom Thickness
7. Impeller Design
a. Diameter
b. Length
c. Width
d. Elevation
8. Baffle Design
a. Width
b. Number of Baffles
9. Tank Insulation
10. Power Requirement
Design Calculations
tB = tF + tH + tR + tE
tB = (10 + 20 + 120 + 10) mins = 160 min
𝐷 = 1.91 𝑚
𝑼𝒔𝒆 𝑫 = 𝟐. 𝟎 𝒎
4. Tank Height
Height of the Body,
𝐻𝑇 = 𝐷
𝑯𝑻 = 𝟐. 𝟎 𝒎
Height of Head,
HH = 0.10H
𝐻𝐻 = 0.10 (2.0𝑚)
𝑯𝑯 = 𝟎. 𝟐𝟎 𝒎
Height of Bottom,
HH = 0.10H
𝐻𝐻 = 0.10 (2.0𝑚)
𝑯𝑯 = 𝟎. 𝟐𝟎 𝒎
Total Height of the Tank,
𝐻 = 𝐻𝑇 + 𝐻𝐻 + 𝐻𝐵
𝐻 = 2.0 + 0.20 + 0.20
𝐻 = 2.40 𝑚
𝑼𝒔𝒆 𝑯 = 𝟐. 𝟒𝟎 𝒎
5. Shell Thickness
𝑷𝒓
𝒕= +𝑪
𝑺𝑬 − 𝟎. 𝟔𝑷
(Plant Design and Economics for Chemical Engineers, Peters and Timmerhaus, pg.
537)
Where:
t = maximum wall thickness, in
P = maximum allowable working pressure, psi
r = inside radius with corrosion allowance, in
L = crown radius
Rk = knuckle radius, Rk = 0.06L
𝑅𝐾 = 0.06𝐿
𝑅𝐾 = 0.06(2.0 𝑚)
𝑅𝐾 = 0.12 𝑚
From Table 13.2 in pg. 812 of Chemical Engineering Design, Sinnott (2005),
Solid-Liquid Extraction | Leaching
21
Baoas, Christine B.
PAMANTASAN NG LUNGSOD NG MAYNILA
University of the City of Manila
College of Engineering and Technology
Department of Chemical Engineering
𝑁
𝑓 = 165
𝑚𝑚2
𝑁 𝑚𝑚2 1𝑙𝑏
𝑓 = 165 (645.16 ) ( )
𝑚𝑚2 𝑖𝑛2 4.482𝑁
𝑙𝑏
𝑓 = 23,750.8702
𝑖𝑛2
1 𝐿
𝐶𝑆 = (3 + √
4 𝑅𝐾
1 2.0 𝑚
𝐶𝑆 = (3 + √
4 0.12 𝑚
𝐶𝑆 = 1.7706
3.2808𝑓𝑡 12 𝑖𝑛
𝐿 = (2.0𝑚) ( )( )
1𝑚 1 𝑓𝑡
𝐿 = 78.7392 𝑖𝑛
𝑃𝑇 𝐿𝐶𝑆
𝑡𝑠 = +𝐶
2𝐽𝑓 − 𝑃𝑇 (𝐶𝑠 − 0.2)
𝑙𝑏
(22.2923
𝑖𝑛 2 ) (78.7392 𝑖𝑛)(1.7706)
𝑡𝑠 = + 0.07874
𝑙𝑏 𝑙𝑏
2(0.85) (23,750.8702 2 ) − (22.2923 2 ) (1.7706 − 0.2)
𝑖𝑛 𝑖𝑛
𝑡𝑠 = 0.1552 𝑖𝑛 = 3.9419 𝑚𝑚
𝑼𝒔𝒆 𝒕𝒔 = 𝟒𝒎𝒎
7. Impeller Design
Solid-Liquid Extraction | Leaching
22
Baoas, Christine B.
PAMANTASAN NG LUNGSOD NG MAYNILA
University of the City of Manila
College of Engineering and Technology
Department of Chemical Engineering
(Table 3.4-3.c, Dimension of Turbine and Tank, Principles of Transport Processes and
Unit Operation by Geankoplis, 3rd Edition, pg. 143)
a. Diameter of Impeller
𝐷𝑎
= 0.5
𝐷𝑇
(Table 3.4-1.c, Dimension of Turbine and Tank, Principles of Transport
Processes and Unit Operation by Geankoplis, 3rd Edition, pg. 144)
Where:
Da = impeller diameter, m
DT = tank diameter, m
Computing for Impeller Diameter,
𝐷𝑎
= 0.5
2.0 𝑚
𝐷𝑎 = 1.0 𝑚
𝑼𝒔𝒆 𝑫𝒂 = 𝟏. 𝟎 𝒎
b. Length of Impeller
Where:
C = elevation of impeller, m
DT = tank diameter, m
Computing for the elevation of impeller,
𝐶 1
=
2.0 𝑚 3
𝐶 = 0.67 𝑚
𝑼𝒔𝒆 𝑪 = 𝟎. 𝟕𝟎 𝒎
8. Baffle Design
a. Width of the Baffle
𝐽 1
=
𝐷𝑇 12
(Table 3.4-1.c, Dimension of Turbine and Tank, Principles of Transport
Processes and Unit Operation by Geankoplis, 3rd Edition, pg. 144)
Where:
J = width of the baffle, m
DT = tank diameter, m
Computing for the width of the baffle,
𝐽 1
=
2.0 𝑚 12
𝐽 = 0.17 𝑚
𝑼𝒔𝒆 𝑱 = 𝟎. 𝟐𝟎 𝒎
b. Number of Baffles
Based from Unit Operations of Chemical Engineers by McCabe et. al, the usual
number of baffles are 4 therefore,
NB = 4
9. Tank Insulation
𝑘𝐽 𝐵𝑡𝑢
𝑄 = 1,452,334.68 = 1,376,547.6741
𝑏𝑎𝑡𝑐ℎ 𝑏𝑎𝑡𝑐ℎ
𝑼𝒔𝒆 𝑷 = 𝟒. 𝟕𝟓 𝒉𝒑
Design Specifications