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 measure and analyze the change in the concentration of Sodium
Bicarbonate in the absorbent porous materials (pellets) in the presence of a diluent (water).

The management of extraction was performed in an Open loop configuration with water as
solvent for the extraction of Sodium Bicarbonate. For this case 100 g of pellets were used as
absorbent porous material in the procedure.

Previously a calibration curve of Concentration Vs Conductivity was made at 20°C and 35°C for
the determination of the concentration at certain time. The power of the pump was adjusted
considering the previous calibration curve, which provides a flow of 2.95 ± 0.5 ml/s.

To take the conductivity, aliquots of the solvent were taken with the solute extracted from the
pellets, in volumes of approximately 100 ± 5 ml and with time intervals of 3 ± 0.5. Starting with
time 0 and the first drop or sample part that came out of the equipment.

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

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 Presented: May 5, 2020

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 Washing:.................................................................................................................. 7
3.2 Leaching:.................................................................................................................. 7
3.3. Case of Study..........................................................................................................7
3.3.1 McCabe Thiele Diagram....................................................................................7
3.3.2 Counter Current and Crossflow configuration...............................................8
4. Sizing.............................................................................................................................. 9
5. Materials and Procedures.............................................................................................9
5.1 Materials:.................................................................................................................. 9
5.2 Reagents:.................................................................................................................9
5.3 Procedure:...........................................................................................................9
5.3.1 Calibration curves of pumps:.........................................................................9
5.3.2 Calibration Curve of Conductivity:...............................................................10
5.3.3 Extraction:......................................................................................................10
7. Conclusions.............................................................................................................. 11
7.1 Recommendations....................................................................................................11
8. Nomenclature........................................................................................................... 11
9. References................................................................................................................ 11

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List of figures and Graphics

No Title Pag.
.

1 Solid-Liquid extraction Principles. 6

2 Solid-Liquid extraction in Batch Open Loop Configuration 7

3 Graphic N° 1. Calibration Curve Pump 1 10

4 Graphic N° 2. Calibration Curve of conductivity at 20°C. 11

5 Graphic N° 3. Calibration Curve of conductivity at 35 °C. 11

6 Graphic N° 4. Concentration Profile at 20°C.   12

7 Graphic N° 5. Concentration Profile at 20°C 13

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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,
therefore, this purpose of this report is the extraction of Oil from flour using Benzene as solvent.

This separation was achieved using the solid-liquid extraction methodology or more commonly
known as leaching. This extraction procedure was carried out, implementing a countercurrent
configuration in Solid-Liquid extractor (UOP5-A) achieving a low concentration of oil in the flour.

1. Introduction

Solid-liquid extraction 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 [4].

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 of the solvent 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 Soil.

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 solvent 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 Washing:
3.2 Leaching:
3.3. 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.

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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° 1 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.

Graphic N° 1 McCabe-Thiele diagram.

3.3.2 Counter Current and Crossflow configuration.

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, but is necessary to use more solvent in comparison with a
Counter Current system. In determination of stages is necessary to determine the mixing point

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located in the middle of feed and solvent compositions. Equation 1 and Equation 2 represents
mixing point.

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

In Counter current system, the interception between operation lines can guide de drawing of
stages as can be seen in the Graphic N°2. However, in the Crossflow system, compositions
leave each stage in equilibrium. Equation 3 relate the solid matrix composition with the solution.
B
Equation 3 U=
N

Graphic N° 2 Counter current McCabe Thiele Diagram.

Graphic N° 3 Cross Flow McCabe Thiele Diagram.

For this session, is important to employ a Counter Current system instead of Crossflow system
since the quantity of solvent is least and

4. Sizing
The performance of the Solid-Liquid extractor UOP5-A have

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

5.2 Reagents:
 Flour  Benzene
5.3 Procedure:
5.3.1 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.

Graphic N° 4. Calibration Curve Pump 1

Graphic N° 5 Calibration
Curve Pump 2

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5.3.2 Calibration Curve of Conductivity:

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

5.3.3 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 solvent 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 16 kg of untreated Flour in the hopper of
the spiral material feeder and adjust the same space of the rotor cell. 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, for this reason, please
put only 7.5 kg of flour in the hopper. When the Solids level are near to the base of the
hopper put more flour until complete 16 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, then the rotor cell and the pumps
beginning with the third until the first.

7. Conclusions

7.1 Recommendations

8. Nomenclature

Symbol Definition

Table 3.  Nomenclature.

9. References

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

Disponible en http://www.ub.edu/oblq/oblq%20castellano/extraccio_tip.html Consultado el 4 de
abril 2018

[2] Aplicaciones industriales del proceso de extracción. Disponible en

http://tesis.uson.mx/digital/tesis/docs/20590/Capitulo3.pdf consultado el 4 de abril de 2018

[3] Equipment for engineering education. Thermal process engineering: extraction. Disponible
en 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

[4] Universidad de Granada, “EXTRACCIÓN SÓLIDO-LÍQUIDO Y RECUPERACIÓN DEL

DISOLVENTE: OBTENCIÓN DE ACEITE DE GIRASOL,” 2015.

[5]     “procesosbio - Extracción sólido-líquido,” 2016. [Online]. Available:

http://procesosbio.wikispaces.com/Extracción+sólido-líquido. [Accessed: 03-Apr-2018].

[6]     A. I. Dueñas-Rivadeneira, U. I. Alcívar-Cedeño, E. I. Sacon-Vera, L. Bravo-Sánchez III,

and G. Villanueva-Ramos III, “Determinación de las condiciones de extracción de compuestos

11
fenólicos a partir de Chuquiraga Jussieuijf Gmel usando la lixiviacion de muestras sólidas
Determination of Extraction conditions of Phenolic Compounds using Chuquiraga Jussieuijf
Gmel solid sam,” Dep. Procesos Agroindustriales. Univ. Técnica Manabí, 2016.

[7]    P. Garcia-Salas, A. Morales-Soto, A. Segura-Carretero, and A. Fernández-Gutiérrez,

“Phenolic-Compound-Extraction Systems for Fruit and Vegetable Samples,” Molecules, vol. 15,
no. 12, pp. 8813–8826, Dec. 2010.

[8] F. Fajardo, “Transferencia de Materia,” 2010. Available:              

https://fjarabo.webs.ull.es/Practics/Oba/ObaFiles/AMater.pdf [Accessed: 03-Apr-2018].

[9] Rodríguez, H. (2015). Transferencia de Materia. Available:     

https://fjarabo.webs.ull.es/Practics/Oba/ObaFiles/AMater.pdf [Accessed: 03-Apr-2018].

[10]   F. Segovia Gómez, J. J. Corral, and M. P. Almajano, “JORNADES DE RECERCA EUETIB

2013 Estudio cinético de la extracción Sólido-Líquido de los compuestos polifenólicos del
Residuo del Aguacate,” 2016.

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