Universidad de la Sabana

Puente del Común Campus, Bogotá North Highway Km.7

Chía, Cundinamarca, Colombia.

Professor Jairo Rubiano

Universidad de la Sabana
Faculty of Engineering
Chemical engineering Department

Dear Professor Jairo Rubiano

The aim of this practice is to leach Oil (Solute) form Flour (Solid Matrix) using Benzene as
Solvent a in a Counter current system. The management Solid-Extraction was performed in
UOP 4 MKII employing 11 kg of flour and 12 L of Benzene.

Initially, both kind of extraction was contemplated, but considering cost of operation, initial
investment and the energy consumption is more suitable a Counter current operation for the
recovery of oil.

Later, you can observe a simple methodology that explains the handle of the Solid-Liquid
Extractor. Some assumptions were considered in the readjustment and Sizing of streams one of
them is the total distribution of Oil in the flour. These assumptions born from Industrial Leaching
of Oil.

The results are largely logical, but they are not exact since there were many shortcomings.

Cordially,

María Camila Velandia León

Jennifer Nicol Pantano Guerra

Juan José Villalobos Mora

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Characterization of Solid-Liquid Extraction

Case study: Extraction of Oil from Flour

María Camila Velandia León

Jennifer Nicol Pantano Guerra

Juan José Villalobos Mora

Chemical Engineering Laboratory

Professor Jairo Rubiano

Assigned: April 21, 2020

Limit day: May 5, 2020

Presented: May 5, 2020

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 INDEX

Abstract.............................................................................................................................. 5
1. Introduction................................................................................................................... 5
2. Objectives...................................................................................................................... 6
2.1 General Objective:...................................................................................................6
2.2 Specific Objectives:.................................................................................................6
3. Theorical Framework....................................................................................................6
3.1 Leaching:.................................................................................................................. 6
3.2 Case of Study.........................................................................................................10
3.3.1 McCabe Thiele Diagram..................................................................................10
4.Materials and Procedures............................................................................................11
4.1 Materials:................................................................................................................ 11
4.2 Reagents:............................................................................................................... 11
4.3 Procedure:......................................................................................................... 11
4.3.1 Calibration curves of pumps:.......................................................................11
4.3.2 Calibration Curve of Conductivity:...............................................................12
4.3.3 Extraction:......................................................................................................12
5. Results................................................................................................................. 13
6. Analysis of results:..................................................................................................15
6.1 Readjustment of Solvent:.................................................................................15
6.2 Sizing:................................................................................................................ 15
7. Conclusions.............................................................................................................. 17
7.1 Recommendations....................................................................................................17
8. References................................................................................................................ 17

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List of figures and Graphics

No Title Pag.
.

1 Figure 1. Three-stage solid-liquid extraction diagram. 7

Figure 2. Typical fixed bed apparatus for leaching beet

2 9
sugar.

3 Figure 3. Bollman type mobile bed leaching equipment. 9

4 Figure 4. Countercurrent leaching using thickeners. 10

5 Figure 5. McCabe-Thiele diagram. 11

6 Figure 6. Calibration Curve Pump 1. 12

7 Figure 7. Calibration Curve Pump 2 12

8 Figure 8. Counter current McCabe Thiele Diagram 14

9 Figure 9. Crossflow McCabe Thiele Diagram. 15

10 Figure 10. McCabe-Thiele Diagram 17

11 Figure 11. Hazard Pictograms. 17

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Abstract

For generations different sectors of the industry have implemented ingredients, compounds and
pigments of natural compounds for the development of products in different fields.
Sometimes the extraction of these compounds can be complicated at an industrial level.

On the other hand, this session is based in case of study used as reference for the construction
of steps. Some readjust are made for the development of this leaching in Armfield UOP4 MKII
using a Counter current configuration with 3 steps, getting a composition of 0.12 wt.% in the
solid matrix.

1. Introduction

Leaching is a common process in the pharmaceutical, cosmetic and food industries to obtain
natural ingredients such as flavorings. During the production of different products this type of
extraction have an important role in the extraction of oils, animal and vegetable fats, washing of
precipitates, vitamins manufacturing and others [1].

This extraction consists in the removal of a soluble component (solute) contained in a solid using
a liquid phase (solvent), the mass transfer process must have a strong contact between the two
phases in the surface of the solid, the inert solid is part of the system that is insoluble in the
solvent [2].

On the other hand, in some fields the compound of interest could be the inert solid or the solute
in the inert solid, is important to consider that due to the quantity of solvent needs to be adjusted
for both cases.

The performance of the extractions depends on the state of the solids, in different fields, this
extraction occurs after process of milling, crushing and sieving. For industrial uses is necessary
to use solvents certain characteristics, like the preservation of CO 2 emission, levels if toxicity,
recovery in subsequent process, price, availability and the energetic costs [2].

2. Objectives

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2.1 General Objective:
 Determinate the suitable configuration for the recovery of Oil.

2.2 Specific Objectives:

 Afford the request concentration in the solid matrix.
 Provide an appropriate methodology for the usage of the system.

3. Theorical Framework

Currently solid-liquid extraction plays a very important role in different industrial processes such
as the extraction of oils, animal and vegetable fats, washing of precipitates, and in the obtention
of meals like Sugar, Teas, coffee, colorants, vitamins and among others [1].

Forward the extraction process is important to consider the characteristics of solute in order to
select a competent substance with high levels of solubility. On the other hand, the porosity of the
draw material should be check due to a high porosity of the material can expedite the
transference of solute between phases. [2].

The passage of the solute to the solvent can be carried out by means of the following
considerations:

a. Chemical reactions do not take place between the substances that make up the sample,
since they would give rise to other different compounds.
b. There must be a constant temperature, since temperature is an influential factor when it
comes to talking about the amount of solute that dissolves in each of the phases.

The usage of this extraction can change with the type of solid matrix in which the solute is found.
If there is a porous matrix the extraction process is called washing, while with a solid matrix the
extraction is denominated leaching.

3.1 Leaching:

Unitary operation where the process of extraction of a solid material through a liquid occurs, the
removal of a soluble fraction in the form of a solution from an impermeable and insoluble solid
phase with which it is associated. Separation usually involves selective dissolution, with or
without diffusion.
The leaching mechanism may include a simple physical solution or solution facilitated by a
chemical reaction. The rate of solvent transport in the mass to be leached or of the soluble

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fraction in the solvent or solution (the extract of the insoluble material, or some combination of
these rates may be important. [2].

Leaching systems are distinguished by the cycle of operation (intermittent, continuous or

intermittent with multiple lots); by the direction of the currents (concurrent, countercurrent or
hybrid flow); by the number of stages (a single stage, multiple stages or differential stage) and
by the contact method (spray percolation, immersion percolation or solids dispersion) [3].
In general, all four categories should be applied to fully stipulate a leaching system. Regardless
of the mechanism and method of operation, it is evident that the leaching process will be favored
by the increase in surface area per unit volume of solids that must be leached and by the
decrease in the radial distances that must be crossed. inside the solids.

The equipment to be used is The Armfield UOP4 MKII use a multi-stage continuous process,
which provides a Counter current flow of the solvent and the solid phase. A batch extraction
vessel is also incorporated to allow demonstration of fixed bed leaching with open or closed-
circuit circulation.

Figure 1. Three-stage solid-liquid extraction diagram.

 The process and operating conditions: The main parameters to determine or identify are the
solvent to use. The compositions and quantities of the initial and final streams, the leaching
cycle (intermittent or continuous), the contact method and the specific selection of the
extractor [4].

 Temperature: The leaching temperature should be selected in such a way that the best
balance of solubility, vapor pressure of the solvent, diffusivity of the solute, selectivity and

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 sensitivity of the product obtained. In some cases, the temperature does not influence the
extraction.

 Compositions and quantities of the initial and final streams are basically with an arbitrarily
given quantity, the capacity of the plant (the speed of production of the extract or the speed
of purification of the raw material to be extracted) [5].

 Stage Efficiency: Consider a simple batch leaching operation, in which the solid is to be
leached with a larger amount of solvent than necessary to dissolve all soluble solute; in said
operation the solid does not preferentially absorb either the solvent or the solute. If an
adequate contact time between the solid and the solvent is provided, all the solute dissolves;
the mixture is then a suspension of insoluble solids immersed in a solute solution in the
solvent. The insoluble phases are then physically separated by sedimentation, filtration, or
drainage, and the entire operation constitutes a single stage. If the mechanical separation of
the solid and the liquid were perfect, there would have been no solute associated with the
solid leaving the operation and the complete separation of the solute and the insoluble solid
would have been achieved in a single stage. This would be an ideal stage, with stage
efficiency of 100%. In practice, the efficiency of the stages is generally considerably less
than this [6].

Leaching a solute from the internal parts of a solid can be relatively slow. The solids formed by
an insoluble substance structure can be described in terms of the shape of the pores that make
it up by means of a factor. [7]

*Note: This factor is a function of the solid, independent of the nature of the solute and is
a measure of the complexity of the path through which the solute diffuses.

In Industrial leaching process some equipment can be used such as:

 Fixed bed equipment: it is used in the sugar industry using water for leaching and
introducing the slices in dividers called “cossetes”. Thanks to the lid and removable bottom
you can feed more food that you want to leach. [8]

8
 Figure 2. Typical fixed bed apparatus for leaching beet sugar.

 Equipment with moving bed: with this device it is possible to leach in countercurrent in
stages. There the bed or stage is mobile and petroleum products are used as solvents. This
equipment is widely used in the extraction of different oils. [8]

Figure 3. Bollman type mobile bed leaching

equipment.

 Solid Agitator Equipment: Used when the solid can be ground and continuous
countercurrent leaching is accomplished by using several agitators in series with settling
tanks. [8]

Figure 4. Countercurrent leaching using thickeners.

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3.2 Case of Study.

“It desired to compare a system for leaching the oil present in flour, using benzene as a solvent.
In the process, 2000 kg/h of solid flour containing 800 kg of oil will be treated with 50 kg of
benzene. The new controlled mix contains 1310 kg/h of benzene and 20 kg/h of oil. The leached
solids must contain 120 kg of oil. Sedimentation experiments like the real process in the
extractor indicate that the retained solution depends on the concentration of the oil in solution.
Tabulated data for N kg of inert solid, B / (kg of solution) and Y kg of oil A / kg of solution are
shown below. Calculate the quantities and quantities that come out of the process and the
number of steps required”.

Settling Experiments
Ya N
0 2
0,1 1,98
0,2 1,94
0,3 1,89
0,4 1,82
0,5 1,75
0,6 1,68
0,7 1,61

Table N° 2 Settling Experiments.

3.3.1 McCabe Thiele Diagram.

Using the following diagram, constructed by Settling experiments reported in the Table 1. The
number of stages necessary to achieve the desired concentration at Solid matrix can be
determinate.

Figure 5. McCabe-Thiele diagram.

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4.Materials and Procedures
4.1 Materials:
 Conductometer  Metal spatula
 Tubes (1L, 500 mL)  100 mL breaker (x10)
 Balance  Glass stirrer
 250 mL volumetric balloons (x5)  Breaker (500 mL)

4.2 Reagents:
 Flour  Benzene
4.3 Procedure:
4.3.1 Calibration curves of pumps:

Firstly, in previous session the calibration of these pump was considered, in this case the
Graphic 1 and the Graphic 2 can release the power and the real flow in each engine.

Figure 6. Calibration Curve Pump 1

Figure 7. Calibration Curve Pump 2

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4.3.2 Calibration Curve of Conductivity:

The calibration curve can make using different dilutions of Flour in Benzene and their
conductivity without any king of heating.

4.3.3 Extraction:

Check that extractor is switched off and rotatory controls are set to minimum on the front of the
console. Fill the solvent tank with 12 L of Benzene and fill collection spaces, allowing one
spaces between each one, with 20 mm depth using Benzene through the mesh at the base of
the rotor. Add Benzene in the third space until eater drains through the pipeline to the recovery
vessel.

Connect pumps with their hoses and set the speed of the pump one to the maximum to purge air
from the first stage (first space), until water drips form the sprinkler. Then repeat the same, with
the other ones. After priming, it may be necessary to up the level of solvent in the first and
second throughs.

*Note: The final trough will always run empty.

Adjust the suitable Benzene rate using the calibration curve, for this case all pumps must pump
200 mL/min (Power 4). Verify the level in each stage, due to changes in equilibrium can be
caused by flow rate variations. Please verify the extractor using the following instructions.

1. Check the right-hand trough (stage 1): If the level is falling reduce the speed of pump
two. If the level is rising increase the speed of pump two.
2. Check the middle trough (stage 2): If the level is falling reduce the speed of pump
three. If the level is rising increase the speed of pump three. Do not adjust the speed of
pump one during the exercise. It will be necessary to check the levels at regular intervals
and to make small adjustments when required.

Configurate the rotor cell with a typically speed (5). Put 14 kg of untreated Flour in the hopper
and allow space between cells in the rotatory wheel. In this case, select 18°C of
temperature in the control pane.

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*Note: Dispose 30-50% of the solid, avoid overload in the hopper, please put only 4 kg of
flour in the hopper. When the Solids level are near to the screw put more flour until
complete 11 kg.

Use the calibration curve for the measurement of concentration trough the extraction at each
step form a disposed range of time. When the system achieves the desirable concentration in
the extract. Please turn off the engine starting with the hopper screw, then the rotor cell and the
pumps beginning with the third until the first.

5. Results

Considering the initial amounts proposed in the case of study and the request concentration in
the solid matrix. Counter current and Crossflow configuration were contemplated, in the first one
3.8 steps are necessary to achieve the required concentration and in the second one 3 steps
reaches a concentration of 0.09 wt. %, but is necessary to use more solvent in comparison with
a Counter current system. Benzene stream contains 0.012 wt. % of oil at the beginning of the
process. Drawing of stages in both cases was possible using Equation 1 and Equation 2

Equation 1 F+ S=M Equation 2 F y A 0+ S y VN +1=M y m

In Counter current system, determination and location of mixing point in McCabe-Thiele diagram
can guide de drawing of operation lines of Underflow and Overflow, the interception of these two
lines is known as Δd. Figure 5 contains number of stages and the reference lines. Overflow
leaves the extractor with a concentration 0.6 of Oil with 1163.3 kg/h and the Underflow leaves
the extractor with a Composition of 0.12 of Oil and 1016.7 kg/h.

However, in the Crossflow system, compositions leave each stage in equilibrium. Equation 3
relate the solid matrix composition with the solution and determinates the Overflow at each
stage, for this case the inlet of Benzene is the same for all stages. On the other hand, the mixing
point changes with the pass of the Underflow trough each stage, because, new quantity of
Benzene enters and remove part of Oil. Figure 6 contains these distribution of each mixing
points during stages and the concentration of solid matrix during the leaching.

B
Equation 3 U=
N

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 Figure 8. Counter current McCabe Thiele Diagram.

Figure 9. Cross Flow McCabe Thiele Diagram.

6. Analysis of results:

Given the initial characteristics of the case of study, some readjustments are provided to
execute this extraction in small scale getting the same percentage of Oil in the solid matrix.
Counter current system is the suitable configuration due to employs less aggregate of Benzene,
However Armfield UOP 4 MKII only works with a Counter current system and 3 stages. For the
adaption of the extraction, firstly is necessary to consider changes in the Counter current
system, Then the appropriate sizing.

6.1 Readjustment of Solvent:

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Changes in the initial weight of benzene allows reduction in the number of steps in comparison
with the Counter current system presented in case of study. To accomplish the separation in the
3 steps is necessary to increase the inlet of Benzene in a 30%. Table N 3 represents quantities
do each component in the readjustment.

Flour (kg) 2000

Underflow (kg/h) 850
Benzene (kg/h) 1900
Benzene (L) 2170,3

Table N 3 Rate flows.

6.2 Sizing:

After the recalculation of Benzene load to perform the leaching in three stages has been
determined, a scaling factor is used to readjust the initial proportions of Flour and Benzene
provided by the study case to the suitable quantities for the extractor UOP 4 MKII. The following
expression represent the scaling factor.

SM
Equation 4 Scaling Factor =
O
2000 kg
Scaling Factor =
2170.3(L)
Scaling Factor =0.39 kg /L
Where:
 SM: Solid Matrix
 O: Overflow

Considering the capacity in the vessel of the UOP 4 MKII extractor (13 L). The proposed
proportion of Benzene for the leaching is (12 L).
SM=Sizing Factor∗12 L
U =11 kg of Flour

Figure 7 represents the number of steps and the operation lines during the leaching in the UOP
4 MKII extractor, in this instance 2.7 steps are necessary to perform the handle of flour
adequately, but regarding the efficiency of the UOP 4 MKII extractor and the no ideal absorption
of Benzene with Oil is advisable use 3 Stages.

15
 Figure 10. McCabe-Thiele Diagram

Another point to consider is their chemical characteristics of Benzene as solvent, stating with
their inflammability that could generate fire in contact with heat or any kind of spark laying the
security of the process and the personal health of all collaborators.
Under other conditions, present high harmful level to the health involving future complications as
Cancer or Chronical respiratory diseases. In any case can generate intensive irritations on the
skin and other parts of
the body such as eyes,
hair and neck. [8]

Figure 11. Hazard Pictograms.

7. Conclusions

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Finally, an adequate configuration for the leaching was provided regarding the amount of
benzene, number of steps and capacity of extractor. This was possible with the comparisons
between Crossflow and Counter current configuration. Furthermore, the required concentration
of Oil in the Underflow was achieved in the case of study and in operative practice using a clear
methodology in the handle of the engine, reporting procedures in order with specific values of
each streams, power values of pumps and other devices such as rotatory cell and hopper screw.
This report can help small scale leaching in the future.

7.1 Recommendations

 Check equipment status and the initial concentration of Oil in Benzene, it could be
different from this practice.
 Avoid usages of high amounts of flour in the Hopper, it can overload so quickly and
delay the extraction.
 Use all the Personal protective equipment, remember that you are working with
benzene.
 If you are going to use another solvent, employ experimental settling data for the
construction of ternary diagram.

8. References

[1] Universitat de Barcelona. Operaciones básicas en el laboratorio de química: Extracción. Retrieved 3

May 2020, from : http://www.ub.edu/oblq/oblq%20castellano/extraccio_tip.html

[2] RAMOS, C.; KÜCKE, M. Revisión crítica de los métodos de medida de la lixiviación de nitrato en
suelos agrícolas. Estudios en la Zona no Saturada del Suelo, 1999, vol. 4, p. 25-32.

[3] Phillip. C Wankat. Ingeniería de procesos de separación, Segunda edición. Editorial Pearson Prentice
Hall. Año 2007

[4] Armfield. (2010). SOLID/LIQUID EXTRACTION UNIT. Instruction Manual.

[5] Equipment for engineering education. Thermal process engineering: extraction. Retrieved 3 May 2020
from: http://www.gunt.de/index.php?
option=com_gunt&task=gunt.list.category&lang=en&category_id=244&level=3 consultado el 4 de abril de
2018

[6] Procesos bio - Extracción sólido-líquido,” 2016. [Online]. Retrieved 3 May 2020, from
http://procesosbio.wikispaces.com/Extracción+sólido-líquido.

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[7] F. Fajardo, “Transferencia de Materia,” 2010. Retrieved 3 May 2020, from:
https://fjarabo.webs.ull.es/Practics/Oba/ObaFiles/AMater.pdf [Accessed: 03-Apr-2018].

[8] Christie J. Geankoplis. (1998). PROCESOS DE TRANSPORTE Y OPERACIONES UNITARIAS.

México: COMPAÑÍA EDITORIAL CONTINENTAL, S.A. DE C.V.

[9] Resumen de Salud Pública: Benceno (Benzene) | PHS | ATSDR. (2020). Retrieved 3 May 2020, from:
https://www.atsdr.cdc.gov/es/phs/es_phs3.html

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