Laboratorio de Operaciones de separacin

Facultad Ingenieria - Ingenieria qumica

Universidad de La Sabana

DETERMINATION OF OPERATING PARAMETERS

AND OPERATING CONDITIONS OF THE
SOLID-LIQUID EXTRACTOR
Santiago Moreano Rojas - Lina Vanessa Beltrn Franco. Estudiantes de Ingeniera Qumica
Universidad de La Sabana. Facultad de ingeniera. Campus del Puente del Comn, km. 7, Autopista
norte de Bogot. Cha, Cundinamarca Colombia. Febrero 24 de 2017.

1. SUMMARY

The objective of this practice was to determine the correct values of operation in terms of temperature
and operating flow in order to have the best extraction speed of the system. In order to determine
these variables, different runs were performed, substituting porous polymer granules containing
potassium bicarbonate or also called pellets after each run. At the end of each test we measured the
conductivity of the liquid extracted to establish the percentage recovered in the process. There were
studied three different flow rates which were 5, 7 and 9 at a constant temperature (19,4 C).
Calculating the distribution coefficient, we were able to determine the amount of adsorbate adsorbed
per gram of solid. The maximum value of Kd obtained was 1,4 mL/g, the best working conditions are
high flow rates and room temperature. We can conclude that the higher the flow rate of solvent the
faster the solute is going to be extracted from the solid matrix.

2. INTRODUCTION

The separation method called solid-liquid extraction is also referred to as lixylation, in this process one
or more soluble components of a solid are extracted by contacting the latter with a liquid selective
solvent. This process is widely used in the mining industry, to extract inorganic, soluble substances,
from solid minerals, also in the pharmaceutical industry to remove products with important properties
of roots and leaves of the plant. There are even organic substances obtained from their natural state
through this process, such as sugar, coffee or tea.

As for the mechanism of this separation process, it depends on the difference of solubilities. Taking as
a model a system of three components:

F: original solid material containing S and c

S: solid
c: substance to extract
B: selective solvent of c

If B and S are not soluble in each other, mixing B with F will have a system with two phases and two
compositions per phase; That is to say there will be four composition variables plus pressure and
temperature. This gives us that for the determination of degrees of freedom we have three
components C (S, c, B) and two phases f (solid and liquid) that is to say that by the equation
 = C + 2 f we have 3 degrees of freedom, which can be pressure, temperature and a composition.
1

Solid- liquid extraction theory is based largely on material balances and the concept of an ideal stage.
Both algebraic and graphical methods are used. The more common graphic solution employs the
concept of a triangular diagram (see in annex 1) where the compositions of the three components,
solute (A), inert solid (B) and the solvent (S) are represented at constant temperature on the three
coordinates of a right angle triangle. The horizontal axis represents the locus of all possible mixtures
of solute (A) and inert solid (B) with zero weight fraction of the third component S, the solvent.
Concentration of component A are designated as xA and are plotted along this axis. Similarly, the
vertical axis represents the locus of all possible mixtures of solvent (S) and inert solid (B) with zero
weight fraction of component A, the solute. Concentrations of component S are designated as xS and
are plotted along this axis. The hypotenuse represents the locus of all possible mixtures of solvent
and solute with no weight fraction of the inert solid. Any point inside the diagram represents a mixture
of all the three components and the weight fraction of each components. The origin xA = 0 and xS = 0
represents the inert solid. The saturated solution of component A in the solvent, at the particular
temperature under consideration, is represented by point 2 on the diagram. The region above the line
represents the section of the diagram in which no undissolved A is present and is the region in which
most extraction are carried out. The region below this line represents the section of the diagram in
which the solids presents contain both components B and undissolved A and the solution present is a
saturated solution with the composition represented by point 2.2

In relation to our analysis, it is sought to determine the factors that influence the speed of extraction
for which it is important to know which factors limit the speed of extraction, so we consider the
following factors:

Particle size affects the rate of extraction in several ways. The smaller the area of contact
between the solid and liquid phase and therefore the higher extraction speed. It is also
preferable that the particle size is small, so that each particle needs the same time in the
extraction, just as the production of fine material must be avoided, since it can be housed in
the voids of the larger particles, which Produces an impediment on contact with the solvent
flow.
The solvent must be selective, with a viscosity sufficiently low for it to flow easily.
The temperature, in most cases the solubility of the component being extracted increases
directly with the temperature as the diffusion coefficient will increase with the temperature
generating higher extraction speed. In some cases the upper limit of the temperature is
considered by secondary processes depending on the components of the extraction, in this
case they are not evaluated.
Stirring of the fluid or solvent is important since it increases the diffusion of the swirl,
increasing the transfer of matter from the particles to the dissolution, the agitation avoids
sedimentation and causes the contact surfaces to be effectively used.3

3. EXPERIMENTAL

For the development of this practice, the procedure is divided into two parts. The first part was made
the calibration curves corresponding to pump 1, which was to be the one to be operated in the

1
(Patio Olivares, Introduccin a la ingeniera qumica: balances de masa y energa. Tomo I)

2
(Sambamurthy, 2007)
3
(Metcalfe Coulson, Richardson, & Backhurst, 1981)
development of the practice, it was decided to perform the calibration with the intention that the actual
flow may be related to the adjustment Of the rotating speed control of the equipment. To do this the
part of the discharge of the pump was connected to a volumetric vessel and filled for 1 minute, this
procedure was carried out at speeds of 2, 4, 6, 8 and 10. Also, in this part the The values of
conductivity with respect to a prepared concentration of sodium bicarbonate.

In the second part of the laboratory, runs are performed on the solid-liquid extraction equipment. In
total, three replicates of the procedure were performed, changing the pellets and the flow velocity of
5.7 and 9. In addition, the conductivity values were taken at different times in each of the runs. The
data obtained in these three processes are reported in Tables 1, 2 and 3.

4. RESULTS

4.1. THEORETICAL RESULTS

The proper operating conditions, variables and operational rates are not part in the mathematical
analysis of the problem are not going to be taken in count because we need to measure them first
experimentally to know how much the results variate depending on this variables and conditions.
Moreover, the optimal conditions are extensive, this means that they depend on the quantity of matter
that is going to be evaluated, also, we need an estimate of temperatures and conductivities that in this
moment we do not have.
This lets only the distribution coefficient, this variable is defined as the ratio of the quantity of the
adsorbate adsorbed per gram of solid to the amount of the adsorbate remaining in solution at
equilibrium4. The distribution coefficient equation found in the Environmental Protection Agency was
compared with other two documents and the mathematical expression remained equal as the first
one.
K d = Ai/Ci (1)
Equation 1 links Ai with Ci, being Ai the concentration of adsorbate on the solid at equilibrium (mol /g
or g/g) and Ci being total dissolved adsorbate concentration remaining in solution at equilibrium
/mol/mL or g/mL) therefore, the Kd units would be mL/g

There is another way to calculate the Kd, the difference is that this method is an empirical
approximation to determine the distribution coefficient without experimental data.
ln Kd = a + b(ln Biv) (2)
Equation 2 brings a way to determine the Kd by using two constants and the soil-to-plant
concentration ratio (Biv), b being always -0,5 and a value variating depending on the soil nature:
Sandy soil; a= 2,11
Loamy soil; a= 3,36
Clayey soil; a= 3,78
Organic soil a= 4,62
Depending on the soil nature, the potassium empirical Kd variates between 15-200 mL/g5

4.2. EXPERIMENTAL RESULTS

The results obtained in practice are presented below in tables 1 to 5.

Flow rate: 5

4
(EPA, 1999)
5
(EAD, n.d)
 Time (min) Conductivity (S)

0 1658

4 1013

8 613

12 419

16 295
Table 1. Time and conductivity values taken at a flow rate of 5.
Flow rate: 7

Time (min) Conductivity (S)

0 1757

4 863

8 407

12 258

16 195
Table 2. Time and conductivity values taken at a flow rate of 7.

Flow rate: 9

Time (min) Conductivity (S)

0 1898

4 684

8 302

12 214

16 177
Table 3. Time and conductivity values taken at a flow rate of 9.

Pump 1 calibration data

Speed set Volume recovered (mL)

2 63,5

4 113

6 163

8 216
 10 286
Table 4. Calibration values for Pump 1.

Conductometer calibration data

Conductivity (mS) Sodium Bicarbonate concentration (g/mL)

9,04 0,01

15,78 0,02

23,3 0,03

28,8 0,04

34,1 0,05
Table 5. Values of the calibration curve at different concentrations of sodium bicarbonate.

5. RESULTS ANALYSIS

For the analysis of the results, first the volume flow rate of the samples taken (Table 4) was
determined through equation 3 and from this it was possible to graph the volume flow rate according
to the speed adjustment of the equipment. These results are shown in Graph 1 to be able to know the
actual flow rate at which the equipment operates.

V olume collected (mL) 3.6

V olume f lowrate (litres/h) = T ime taken (seg)
(3)

Figure 1. Volume flowrate in function of speed set.

From the above graph it is possible to demonstrate the values of the volumetric flow rates that were
used in the laboratory. The speed set in the equipment of 5 is 8.55 L/h of volumetric flow rate, the
speed set number 7 is equal to 11.88 L/h and 9 is equal to 15.21 L/h. Graph 2 shows the
concentration-related calibration curve, which yields an equation of y = 631.4 x + 3.262 .
 Figure 2. Calibration curve for samples conductivity and salt concentration

From the equation obtained from the graph of conductivity as a function of the concentration, the
values of the concentrations of the solution extracted in the three different runs at a given time are
determined. These values are reported in the following table for each flow rate. In addition, the graph
of annex 2 seeks to know by an interpolation method the weight percent values of potassium
bicarbonate.
To calculate the distribution coefficient, first we measured the density of 500 mL of pellets that we
used in the practice, the result was a density of 0,87 g/mL, with this density we calculated the mass of
pellets with Equation 4 that relates mass and volume with density.
= m/v (4)
mass of pellets = 435 g
With this value and the sodium bicarbonate mass we obtained the variable Ai from Equation 1 and,
dividing this value in the concentration given by the measures we obtained the variable Ci

Flow rate: 5 Flow rate: 7

Time Conduct Concentr Kd (mL/g) Time Conduct Concentr Kd (mL/g)
(min) ivity ation (min) ivity ation
(S) (g/mL) (S) (g/mL)

0 1658 2,621 0,1462 0 1757 2,778 0,1379

4 1013 1,599 0,2394 4 863 1,362 0,2813

8 613 0,966 0,3966 8 407 0,639 0,6

12 419 0,658 0,5822 12 258 0,403 0,9506

16 295 0,462 0,8292 16 195 0,304 1,26

Flow rate: 9
Time (min) Conductivity (S) Concentration(g/mL) Kd (mL/g)

0 1898 3,001 0,1277

4 684 1,078 0,3554

8 302 0,473 0,81

12 214 0,334 1,147

 16 177 0,275 1,3931

Relate to this tables, we made some graphs in which we could see the behaviour of the distribution
coefficient along the samples.

Figure 3. Behaviour of distribution coefficient vs time

Taking in count the results given by the practice, the operation variables that are important for a
solid-liquid batch extraction are the concentration of solute in the solid matrix, the solvent flowrate
and temperature. There are other variables such as stirring speed and space time but this variables
are only found in continuous processes6 . This can be easily inferred from the results because at
different flow rates the conductivity measured at the same moment is different, and this was the only
variable that we changed during the practice, thus, it interacted with the operation.

The temperature was also a subject of study because looking at the literature, they said that the
temperature was important in a leaching process, at the moment of changing the systems
temperature we noticed that the thermocouple was not working because we changed the systems
temperature from 35 to 40 degrees in the control panel and there, it looked like it was changing but
physically, the solvent temperature was dramatically over 40C, so we took a sample and measured
the temperature and this was in 56C. We decided not to change the systems temperature because
the sensor was not working and the results could be wrong. The final important variable taken in count
for this process is the solute concentration inside the solid matrix because as higher the concentration
of solute is as more time we are going to need to dilute this solute into the solvent, this means more
time that is similar to more money, so as lower the concentration of solute is as cheaper the process
is going to be.

The operation temperature range of the solid-liquid extraction equipment in the laboratory is between
room temperature ~(19C) and (55C) that is the maximum temperature that can be reached by the
fluid with the maximum heater power. On the other hand, the operation flow rate range varies
between 0 L/h and 16,674 L/h, this values were taken from the calibration curve of the pumps that
relates speed set and flow rate in Figure 1.

6
(Mendes, Martins, 2003)
Calculating the distribution coefficient values (Kd) of the samples we can see that this value is higher
each time we took a sample, the reason for this behaviour is that each time, the concentration inside
the pellets its lower because the sodium bicarbonate is diluting in the solute (water in this case).
Moreover, analyzing Figure 3 it can be deducted that the higher the flow rate of solvent is entered to
the tower, more quickly the distribution coefficient is going to grow and thus the separation is going to
be. According to the EPA7 , kd values increase as flow rate does because transport phenomena
theory,when the flow rate enters to the container, at time 0 it starts to absorb solute from the pellets
and solutes that salt making that the concentration of the salt decreases inside them, when this
current enters faster and with more force, the separation process is better because of the turbulent
flow conditions, so the salt is more likely to be in the aqueous zone.

Due to the analysis of the calculated values obtained in this practice, it is considered important to
establish the conditions to be taken into account when using extractors. The design and optimization
of an extraction process entail the knowledge and the role of the technological parameters of the
process which are:

The preparation of solid material by size reduction, the solid size must be suitable (surface
area per unit volume) to make the solute more accessible to the solvent and to favor the
extraction, but not so fine as to cause packing of solids and impeding free flow of the solvent.
The selection of the solvent for extraction based on a number of characteristics like capacity,
selectivity, chemical inertness, thermophysical properties, flammability, cost and availability .
The selection of operating temperatures must be high to give higher solubility of solute in
solvents, but not so high as to cause solvent losses , extraction of undesirables constituents,
or damage of sensitive components.
The equipment depending on the mode of operations, the solid handled or the performing
arrangement (one state or multistage).8

6. CONCLUSIONS

As expected, the distribution coefficient is directly proportional to the flow rate, this condition is a
consequence of variables from transport phenomena theory and some others. On the other hand, the
literature says that the extraction is also affected by changes in the operation temperature because of
principles of solubility but this statement could not be tested because the system presented some
difficulties at the moment to change the operation temperature.The proper operation conditions are to
work at the lowest flow rate and at room temperature for the equipment located in the laboratory.

For an efficient process of solid-liquid extraction it is important to remember the parameters that are
involved as the correct selection of the size of the solid, to ensure the contact between solute and
solvent, also the temperature is an important value and although in this practice could not To
complete this analysis in detail, the literature allows us to know that this variable must be operated at
temperatures that allow solubility without reaching boiling points of any component with which to work.
Finally, it is important to select the solvent, since it must comply with the characteristics mentioned in
the analysis of results, according to the solute to be extracted.

7
(EPA,1999)
8
(Varzakas & Tzia , 2014)
REFERENCES

1. Patio Olivares, A. Introduccin a la ingeniera qumica: balances de masa y energa.

Tomo I. Ciudad de Mxico, Mxico: Universidad Iberoamericana.
2. Sambamurthy, K. (2007). Pharmaceutical Engineering. New Delhi, India: New Age
International.
3. Metcalfe Coulson, J., Richardson, J., & Backhurst, J. R. (1981). Ingeniera qumica:
Operaciones bsicas (3 edicin ed., Vol. II). Sevilla, Espaa: Reverte.
4. Mendes,F. Martins, A. (2003). A statistical approach to the experimental design of the
sulfuric acid leaching of gold-copper ore. So Paulo. Brazil. Universidade Federal de
Minas Gerais.
5. United States Environmental Protection Agency. (1999, August). Understanding
variation in partition coefficient, Kd, values. The Kd model, methods of measurement,
and applications of chemical reaction codes, Vol 1, Pag 63.
6. Armfield. (2010). Solid- Liquid extraction unit. Instruction manual.
7. Wankat, P. C. (2008). Ingeniera de procesos de separacin (2 edicin ed.). (R.
Fuerte Rivera, Ed.) Mexico: Pearson.
8. Varzakas , T., & Tzia , C. (Edits.). (2014). Food Engineering Handbook: Food
Process Engineering (illustrated ed.). CRC Perss.

ANNEX
1. Triangular diagram for solid- liquid extraction at constant temperature (Sambamurthy,
2007)
2. Graphs of concentration of potassium bicarbonate.

3. Calibration data

4. Experimental data