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

1
 Characterization of Solid-Liquid Extractor

Case study: Extraction of Solid-Liquid Mixture

María Camila Velandia León

Jennifer Nicol Pantano Guerra

Juan José Villalobos Mora

Chemical Engineering Laboratory

Professor Jairo Rubiano

Assigned: March 10, 2020

Limit day: March 24, 2020

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 Presented: March 24, 2020

INDEX
Abstract.............................................................................................................................. 5
1. Introduction................................................................................................................... 5
2. Objectives...................................................................................................................... 6
2.1 General Objective:...................................................................................................6
2.2 Specific Objectives:.................................................................................................6
3. Theorical Framework....................................................................................................6
4.1 Materials:.................................................................................................................. 9
4.2 Reagents:.................................................................................................................9
4.3 Procedure:................................................................................................................ 9
4.3.1 Pellets Preparation:..............................................................................................9
4.3.2 Conductivity Curve...............................................................................................9
4.3.3 Extractor Operation..............................................................................................9
4.4.4 Average of Sodium Bicarbonate..........................................................................9
5. Results and Discussion..............................................................................................10
5.1. Calibration Curve of Pump...................................................................................10
5.2 Calibration Curve of Conductivity at 20°C and 35°C...........................................10
5.3 Concentration Profiles..........................................................................................12
5.4 Recovery:............................................................................................................... 13
6. Analysis of Results and Discussion.......................................................................14
7. Conclusions and Advices........................................................................................15
7.1 Recommendations....................................................................................................15
8. Nomenclature........................................................................................................... 15
9. References................................................................................................................ 16

3
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

4
Abstract

For generations different sectors of the industry have implemented ingredients, compounds and
pigments of natural compounds for the development of products of different kind of procedures
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 salts (sodium
bicarbonate) from a prepared solid called Pellets1, their preparation consisted of 83.3 g of
potassium bicarbonate in 500 mL this solution conform 135g of pellets [1].

This separation was achieved using the solid-liquid extraction methodology or more commonly
known as leaching. This extraction procedure was carried out, implementing two tests, one at 20
° C and the other at 35 ° C. The extractor (UOP5-A) was used in Batch Open Loop
Configuration. Where conductivities were constantly evaluated at a certain time in order to verify
changes in the composition of the extract.

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].

1
Pellets: Solid prepared material, made for simulations.

5
 2. Objectives

2.1 General Objective:

 Determinate variations in the solubility with the alteration of the temperature.

2.2 Specific Objectives:

 Employ analytic methods for the control and monitoring of the process.
 Achieve a recovery al least of 50%.

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].

Secondly, the solvent and the draw material are deposited in a vessel. With the pass of some
minutes the second phase attached the solute and this new phase is called extract. The
recovery never reaches to 100%, the remaining percentage of solute stay in the particles of the
draw material, the following image present the phases and steps presented during the Solid
-Liquid extraction.

Figure 1. Solid-Liquid extraction Principles.

Following the Figure 1, the distribution of the phases in the system are:

1. Second phase (solvent) 3. Solute

2. Draw material 4. Portable Phase

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 5. Extract.

Open loop extraction: The extraction tank is filled with the solvent, then more solvent is
pumped from the bottom to the top in order to cross all the inert solid, extracting all possible
solute.

Figure 2. Solid-Liquid extraction in Batch Open Loop Configuration

At the same time, the differences in solubility between the solute and the solvent are related by
means of the partition coefficient, which remains constant since the concentrations of the solute
in each solvent are always the same.

Kd=Ya/ Xa

For highly diluted systems Kd will be constant, whereas at higher concentrations Kd often
becomes a function of concentration. The solvent should be easy to separate from the diluent,
either as a fully or partially immiscible system [3].

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

a. The solutions must be diluted, since Henry's Law is only fulfilled in these cases.
b. Chemical reactions do not take place between the substances that make up the sample,
since they would give rise to other different compounds.
c. 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.

7
Nernst's distribution law or distribution law is a generalization that governs the distribution of a
solute between two immiscible solvents. In other words, when a certain amount of solute is
distributed between two immiscible solvents, an equilibrium state is reached in which both the
chemical potential and the fugacity of the solute are the same in the two phases [7]

Therefore, if we consider two solvents «A» and «B» that form two separate phases when in
contact and we suppose that a small amount of solute «i» dissolve in both phases forming two
ideal solutions in equilibrium, the quotient of mole fractions of the solute in the two phases can
be expressed as follows:

Equation 1

Where:

x: molar fraction of solute. N: Partition coefficient

μ: Fugacity T: Temperature

R: Constant of ideal gases P: Pressure

However, if solutions are sufficiently diluted, this coefficient can be found from the constants of
Henry's law for "i" in solvents "A" and "B", symbolized by KH [8]:

Equation 2

In the ideal case that the solute in both phases are very similar, the assumption of equivalent
concentration can take [4]:  

Equation 3

4. Materials and Procedures

4.1 Materials:
 Glass stirrer  Balance

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  250 mL volumetric balloons (x5)  Thread
 500 mL beaker  Coifs
 Conductivity meter  50mL,100mL and 500 mL test tubes
 Metal spatula (x5).
 100 mL beakers (x10)
4.2 Reagents:
 Sodium Bicarbonate  Pellets 
4.3 Procedure:
4.3.1 Pellets Preparation:

The preparation of pellets must be prepared two days before the practice. For this instance, 24 g
of sodium bicarbonate are diluted in 250 mL of distilled water and mixed with the 362.5 g virgin
pellets. It is left to act for a day so that the solute and the pellets mix. After 24 hours, the solid
extracts should be dried in an oven.
4.3.2 Conductivity Curve  

Starting with the solutions at environmental temperature each curve was made using different
dilutions and with their conductivity. This process is the same for the curve at 35°C.
4.3.3 Extractor Operation

The equipment must be configured in batch open loop. Then fill the feed tank with water,
highlighting that it must be verified that the flexible hoses are correctly connected and located in
the corresponding discharge tanks. Turn on the equipment, where the pumps are subsequently
purged with water, as are all the tube connections. Place the previously prepared pellets into the
coif. Open the valve to allow the passage of the solvent and thus generate the solid-liquid
contact. Adjust pump speed and temperature as you prefer and take the conductivity at the
discharge nozzle from a disposed range of time.

4.4.4 Average of Sodium Bicarbonate

For complex reasons the added amount of Sodium bicarbonate is unknown. Considering this
situation, a uniform distribution of Solute is considered and the percentage. Both extractions had
the same quantity of pellets in their batch Vessel. The Percentage of sodium Bicarbonate is 21%
using:

9
 A 0 Mass
Equation 4 X A0 =
Total mass

83.3 NaHCO ₃
X A0 =
316.8 g Pellets+ 83.3 g NaHCO ₃

X A0 =0.21

21% of Solute is assumed in the Inlet of the process.

5. Results and Discussion

5.1. Calibration Curve of Pump

Firstly, in previous session the calibration of this pump was considered, in this case the equation
4 can release the power and the real flow in the engine. For both extraction the power employed
was 2 Kw, pumping 94.391 (mL/min).

Equation 5 y=36.169 x +22.053

Graphic N° 1. Calibration Curve Pump

1

5.2 Calibration Curve of Conductivity at 20°C and 35°C

As previously mentioned, this curve of calibration take place with the values of the solutions
prepared at 20°C. First for all the conductivity of the water was measured in 159,6 µS.
The estimation and the monitoring of the extraction can be realized with the use of the equation
supplied by the Graphic 1.
Equation 6 y=67712 x 2−11491 x−825.58

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

The Table 1 represent each data.

Table 1. Calibration Curve of conductivity at 20°C.  

Then, with the same way the Calibration curve at 35 °C was developed and the correspondent
equation is:

Equation 7 y=7338,3 x +94,913

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

11
 Table 2. Calibration Curve of conductivity at 35°C.  

5.3 Concentration Profiles

Using the Equation 4 for the first extraction, the values of concertation can be determinate.
However, it was necessary to debug some calculations to preserver the continuity in both
profiles. The Table 3 represent changes in the concentration with the increase of the time at
20°C.

Table 3. Concentration Profile at 20°C.  

Graphic N° 4. Concentration Profile

at 20°C.  

12
However, for the second extraction the temperature takes places because due to it can give
information about the correct developing of the extraction.

Table 4. Concentration Profile at 20°C

Graphic N° 5. Concentration Profile at 20°C

5.4 Recovery:

Coif 1 and Coif 2 refers to extraction 1 and extraction respectively.

Table 5. Recovery

13
 6. Analysis of Results and Discussion

Considering all the results obtained, it is possible to determine that a leaching system is affected
by variables such as temperature, type of solvent, amount of solute and flow of solvent. Due to
the final recovery can increase or decrease as well as the operating time.

At the operational level, the aim is to obtain the maximum recovery of solute using the least
amount of resources. This is not evident in either of the two leaching cases since a considerable
amount of solvent was used and the amount recovered was not significant. The recovery values
are 17% in the first extraction and 68% in the second one.

For the first case, a constant concentration profile was not obtained in despite of this the
purification carried out at the beginning, illustrated in the Graphic N°4. Variations could occur by
the presence of systematic errors by the part of the users during the conductivity measurement
of the samples, as well as the characterization of a supersaturated system produce
accumulations of Sodium Bicarbonate in little porous regions of the solid cutting of the transfer.

Compared with the second extraction at 35 ° C, the results are more consistent, because the
concentration profile have a constant decrease and their variations are equal during all the
lixiviation process, since, with increasing temperature, the solubility of the solute in the solvent
increases directly proportional, it would also increase the solvent diffusion coefficient in the solid
particles, increasing the extraction speed, which would mean a lesser amount of solvent needed
and the recovery is optimum. However, at very high temperatures the product gets damages
inducing the evaporation of the solvent.

From another point of view, this increase in kinetic energy in molecular bonds causes breaks
between those molecules joined by weak bonds, increasing the vibration in the atomic structure
[5]. Some of the particles in the medium are altered by the constant distributions of Sodium
Bicarbonate molecules that are coming out with the past of solvent.

On the other hand, the pressure does not generate high changes in the leaching system, it is
assumed that the pressure losses are negligible, which does not affect the equilibrium stages,
and mas transfer conditions are the same.[6]

14
Another important factor to carry out the leaching is the type of solvent to be used, in this case
the water does not have great absorption properties. Therefore, the use of other solvents is
recommended in order to optimize energy costs and investments.

Using another solvents can improve the productivity in the lixiviation , organic solvents have a
good performance for separation process, p-xylene, propyl acetate, acetyl acetate and butyl
acetate can generate good results, commonly Hexane and Benzene can used for extractions but
their secondary restrictions represents more problems. The selection of any type of solvent must
be done in the comparison between partition constant. [7]

7. Conclusions and Advices

Finally, increments in temperature affects proportionally the solubility and the recovery of
Sodium Bicarbonate. Analytical methods were a great way for the treatment and determination
of the measurements obtained for each of experiments. On the other hand, they facilitated the
interpretation of results immediately. Second lixiviation overcome the threshold, providing
moderate percentage of Solute.

7.1 Recommendations

In order to generate a contact between the pellets and the water, it is necessary to wrap the
pellets in a filter paper and tie them with a nylon to the edge of the batch vessel firmly.

It is necessary to observe and follow the connections of the pumps with the pipes because they
are not in operation or are not, therefore a water spill can be generated.

Only turning on the temperature switches when the water is flowing in the equipment or this
could cause damage to it.

8. Nomenclature

Symbol Definition

X A0 Weight Percentage of Sodium Bicarbonate

R Gas constant.

KH Henry’s law for solvents coeffiencts.

Table 3.  Nomenclature.

15
 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
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.

10. Annexes’

16
Figura 3. Experimental data registry

17