Hydrometallurgy Techniques

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Group No.: 5
Laboratory No.: 1,2,4,5 and 6

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Declaration

Except as indicated, this work being submitted is solely my/our own work.

Name ID Signature

(Brian) Ibrahim Nwiran 21698185

Hieber Enrique Rojas Bulla 21722796

Rais Fikry 21208199

Rahmadhani Triastomo 21276468

Due Date: 30th Oct 2023

Date Submitted: 30th Oct 2023

Office use only:

 Table of contents

Lab # Lab Name Page

1 Leaching of Chalcopyrite 2
2 CURRENT EFFICIENCY FOR ZINC ELECTRODEPOSITION 10
4 LEACHING OF COPPER IN AN AMMONIACAL SOLUTION 14
5 SOLVENT EXTRACTION OF COPPER 20
6 RESIDENCE TIME AND NON-IDEAL FLOW 29

1
 Experiment 1 – Leaching of Chalcopyrite

1. Introduction
1.1 Theory of chalcopyrite leaching
The sulphide minerals of copper such as chalcopyrite (CuFeS 2) are not readily
dissolved in dilute acid. Their solubility will increase in the presence of oxidizing
agents such as oxygen, ferric ions, and bacteria. However, acid medium such as sulfuric
acid lack selective properties in the leaching process. Hence, some gangue materials
also dissolved in the liquid medium, necessitating an expensive purification process [1].
Using an alkaline lixiviant seems to have many advantages given the known difficulties
with acidic leaching. Utilization of organic alkaline lixiviant (monosodium glutamate)
to selectively dissolved copper from electric arc furnace dust had been investigated,
with approximately 95% recovery of copper. The use of monosodium glutamate (MSG)
as a reagent in copper alkaline leaching has some advantages such as its wide
availability and biodegradability [2].
Leaching process is considered as a heterogeneous process which involves solid and
liquid phase. The kinetic of leaching process is essential in determining reactor types
and the size of the reactor. Rate of reaction and mean residence time required to
completely dissolve metal in a liquid medium were needed to measure kinetic
properties of leaching processes [3]. The leaching process frequently takes place in
three stages in many hydrometallurgical systems: (a) the mass transfer of reactants and
soluble product from bulk of liquid to the surface of solid; (b) the diffusion of reactant
and soluble product through the pore of solids; and (c) the chemical reaction of reactant
in the solid-liquid surface. The slowest step will be the rate-limiting step for a
particular set of experimental conditions [3].
One of the most reliable models to describe the kinetic of the leaching process is the
shrinking core model. This model states that during leaching, the reaction takes place in
the outer skin and then continuously happens in the deeper zone where an unreacted
core exists. The reacted core will form an ash layer that is assumed to be an inert layer
[4]. The Shrinking Core model covered three mechanisms of rate control during the
leaching process which are diffusion through liquid film control, diffusion through ash
product control, and chemical reaction control. Three types of rate controls covered in
the Shrinking Core model can be summarized in these following equations:
1) When diffusion of reactant A through the liquid boundary layer is rate limiting:

3bkg Cal t
X b= =K f t
ρb R

2) When diffusion of reactant A through the ash (reacted) layer is rate limiting:

2/ 3 6 b D e Cb t
⌊ 1−3(1−X b ) +2(1− X b) ⌋=K d t= 2
ρb R

3) When chemical reaction at the surface of the shrinking core is rate limiting:

2
 1/ 3 b K s Cb t
⌊ 1−( 1−X b ) ⌋ =K s t=
ρb R

1.2 Objective
The primary objective of this experiment is to become familiar with chemical
laboratory techniques and with the interpretation of kinetic leaching data.
2. Materials and methods
2.1 Materials
In this experiment, chalcopyrite (CuFeS2) was used as a solid specimen which was
pulverized to obtain -200μm in size. Chalcopyrite was assumed as the only copper
mineral in this specimen. Monosodium glutamate was used as the leaching agent, and
hydrochloric acid (HCl) as pH regulator. Merck brand analytical grade chemicals were
used, and deionized water was used in the preparation of analytical samples.
2.2 Methods
In the preparation of the leaching solution for each test, a 1L volume was achieved by
introducing 600ml of distilled H2O into the 1L volumetric flask. Prior to the addition of
the required quantity of Monosodium Glutamate, 5ml of concentrated HCl was
carefully incorporated. The required amount of monosodium glutamate was dissolved
in distilled water to achieve 0.5 M and 0.25 M reagent concentration. The pH solution
was evaluated within the range of 0.5 to 0.7 by adding concentrated HCl incrementally,
with comprehensive mixing during pH measurements to ensure consistent pH levels
across all solutions.

The solution was then transferred to the reaction flask, placed within a water bath, and
equipped with a thermometer and stirrer. While maintaining stirring, the solution was
gradually brought to the requisite temperature, with particular emphasis on maintaining
a steady temperature reading. In this experiment, the temperature varied between room
temperature and 520C.

Experiment Concentration Temp

C 0.5 M 520C

D 0.25 M 250C

Table 1 Experimental Design

In preparation for data collection, a record sheet was established for time and sample
number documentation, and a stopwatch was initialized. A precisely weighed 1-gram
sample of chalcopyrite was introduced into the reactor, and timing commenced
immediately. Periodically, the stirring rate was adjusted to prevent CuFeS 2 from
floating on the solution's surface. Sample extraction began with the removal of
approximately 6 to 7 ml of the solution using a 10ml pipette, which was then
transferred to a designated sample vial marked as "sample zero."

A total of twelve additional samples, each of the same size, were obtained at specified
elapsed time intervals of 2, 4, 6, 10, 15, 20, 30, 40, 50, 60, 70, and 80 minutes. To

3
 separate the solid CuFeS2 from the solution, these samples underwent filtration,
necessitating the use of a clean, dry 10mL pipette, filter paper, and a filter funnel.
3. Results and Discussions (between 3 and 6 pages)
3.1 Fraction of chalcopyrite converted.
The fraction of chalcopyrite converted during specific time was calculated using
equation below:
wt of Cu∈solution
X b= × 100 %
wt of Cu∈initial sample
Initial weight of Cu was calculated by assuming that the sample was pure chalcopyrite.
The weight percentage of Cu in Chalcopyrite was obtained by dividing atomic weight
of Cu and molecular weight of Chalcopyrite (CuFeS 2). The mass fraction of
chalcopyrite converted in this experiment were tabulated in Tables 3 and 4 below.

Wt sample 1 gram
% Cu: 34.626
Wt of Cu 0.34626 gram
346.26 mg
Volume: 1 litre
Table 2 Calculation of Cu weight percentage in the sample

Minutes Sample Cu Cu (mg) Converted

(52 C, 0.5M) (mg/L) Fraction (Xb)
0 C0 0.02 0.02 0.006%
2 C2 0.16 0.16 0.046%
4 C4 0.2 0.2 0.058%
6 C6 0.22 0.22 0.064%
10 C10 0.26 0.26 0.075%
15 C15 0.31 0.31 0.090%
20 C20 0.36 0.36 0.104%
30 C30 0.43 0.43 0.124%
40 C40 0.49 0.49 0.142%
50 C50 0.54 0.54 0.156%
60 C60 0.61 0.61 0.176%
70 C70 0.66 0.66 0.191%
80 C80 0.75 0.75 0.217%
300 C300 1.74 1.74 0.503%
Table 3 Mass conversion of Cu in experiment C (500C, 0.5M)

4
 Figure 1 Mass conversion of copper with variation of temperature

Minutes Sample Cu Cu Converted

(25 C, 0.25M) (mg/L) (mg) Fraction (Xb)
0 D0 0.2 0.2 0.058%
2 D2 0.12 0.12 0.035%
4 D4 0.21 0.21 0.061%
6 D6 0.13 0.13 0.038%
10 D10 0.15 0.15 0.043%
15 D15 0.16 0.16 0.046%
20 D20 0.18 0.18 0.052%
30 D30 0.23 0.23 0.066%
40 D40 0.3 0.3 0.087%
50 D50 0.23 0.23 0.066%
60 D60 0.37 0.37 0.107%
70 D70 0.36 0.36 0.104%
80 D80 0.27 0.27 0.078%
300 D300 0.62 0.62 0.179%
0
Table 4 Mass conversion of Cu in experiment D (25 C, 0.25M)

The results in figure 1 indicate that leaching in room temperature has a higher
conversion rate than 500C. After 300 minutes of leaching time, the amounts of copper
being leached were 0.503% and 0.179% for experiment C and experiment D,
respectively. The possible reason for these results is because experiment C were tested
using more concentrated reagent and higher temperature. Another study stated that the
increase in temperature strongly affects the percentage of copper dissolved in
monosodium glutamate (MSG) reagent. While variation in MSG concentrations had
less significant effects in percent copper extraction [2].

5
3.2 Leaching kinetics

To describe chalcopyrite leaching kinetics, two kinetic models were used to determine
the rate limiting process: diffusion through ash product layer or chemical reaction
process. The plotting results of experimental data to those kinetics models were listed
in Table 5.

Experiment Temperature Molar Coefficient of Correlation (R2)

Concentration
Ash Diffusion Chemical Reaction

C 520C 0.5 M 0.982 0.9631

D 250C 0.25 M 0.9409 0.8514

Table 5 Correlation coefficients for experimental data fitting using two kinetics models.

Based on the results tabulated in Table 5, diffusion through the product layer was
determined as a rate limiting process. The value of coefficient of correlation (R 2) of the
ash diffusion control model for both experiments was higher than the chemical reaction
control model. It means that the rate of reaction was determined by the rate of diffusion
of reagent through the product layer.

Figure 2 Fitting of chemical reaction control model in experiment C and D

6
 Figure 3 Fitting of ash diffusion control model in experiment C and D

3.3 Determination of activation energy

The determination of activation energy (Ea) for the leaching process was carried out
using the Arrhenius equation K = Ae (-Ea/RT), where K represents the rate constant through
the unreacted solid layer, A is a surface area constant, T is the leaching temperature (in
Kelvin), and R is the ideal gas constant (8.314 J/K.mol).

The value of K was determined as the slope of the rate limiting step model (ash
diffusion model). If the same step is the limiting mechanism in examined temperature,
then the value of K will be varied following linear regression trend. The value of K for
both different temperatures were estimated using mean square error (MSE) methods.
The results were listed in Table 6.

Experimen Linier Regression Equation Rate constant (K) MSE

t

C (500C) Y = (3x10-8) x – (3x10-7) 3x10-8 4.33x10-13

D (250C) Y = (3x10-9) x + (6x10-8) 3x10-9 1.02x10-14

Table 6 Rate constant calculation from ash diffusion control model

The value of Ea can be obtained by plotting ln K against (1/T), which yields a straight-
line equation with a slope, as demonstrated in Figure 4. From the slope of the curve in
Figure 4, the activation energy value for the leaching of Chalcopyrite in Monosodium
Glutamate solution was determined to be 60.72kJ.

7
 Figure 4 Plotting of Ln K vs 1/T

The kinetics of processes controlled by diffusion tend to exhibit low activation

energies, typically within the range of 4-13 kJ/mol, whereas processes controlled by
chemical reactions possess higher activation energies, exceeding 42 kJ/mol. Processes
are considered to be controlled both by diffusion and chemical reactions (mixed
controlled) when their activation energy falls within the intermediate range between
these two specified ranges [5]. Based on the results in Table 5, the leaching kinetic of
chalcopyrite using MSG was controlled by an ash diffusion mechanism. However, the
value of calculated activation energy was high (60.72 kJ). The possible reason for this
phenomenon was the possibility of a mixed control mechanism and the formation of
any constituent that hardly dissolves in the Monosodium Glutamate reagent.

3.4 Probable cause of deviation from idealized model

In the context of high values of fraction converted, it is commonly observed that the
reaction rate exhibits a tendency to plateau, and this phenomenon can be attributed to
several underlying factors. One prominent factor is the depletion of reactants as the
reaction progresses. As the reaction proceeds, the concentration of reactants diminishes,
resulting in a diminishing rate of reaction. At high levels of fraction converted, the
concentration of reactants reaches exceedingly low levels, contributing to the flattening
of the reaction rate curve. Furthermore, equilibrium limitations can significantly impact
reaction kinetics under such conditions. A reaction may approach equilibrium at high
levels of fraction converted, leading to a diminishing reaction rate. These dual factors,
namely reactant depletion and equilibrium limitations, play pivotal roles in elucidating
the observed flattening of reaction rates at elevated values of fraction converted.

To experimentally verify these hypotheses, one can conduct experiments with

prolonged time to clearly identify the deviation between experimental data and kinetic
models. Additionally, one can conduct experiments under different conditions, such as
varying the temperature or reagent concentration, to determine the effect of these
factors on the reaction rate and the extent of deviation from the idealized models.

8
3.5 Effect of larger particle size in limiting mechanism
As the particle size increases, the diffusion of reactants to the surface of the particle
becomes slower, leading to a decrease in the rate of reaction. Chemical reaction control
is independent of particle size. Based on the shrinking core model equation, the ash
diffusion control mechanism shows the longest time needed to achieve the same
fractional conversion. It equals the square of particle radii. Those the bigger particles
size will lead to longest distance for both reactant and product to diffuse and react with
the unreacted core [4].
3.6 Practical particle size limit
In practice, the optimum particle size for leaching is often determined through a
balance of diffusion limitation, energy consumption, reagent consumption, and solid-
liquid separation. Smaller particles typically have better mass transfer characteristics,
which means that leaching agents can penetrate and react with the material more
rapidly. However, extremely fine particles can suffer from reduced permeability,
leading to slower leaching rates and incomplete extraction. The energy required to
comminute (crush or grind) materials into smaller particles can increase significantly as
particles become finer. Extremely fine particles may require more leaching reagents per
unit of mass due to the increased surface area. After leaching, the solid-liquid
separation process becomes more challenging as particle size decreases. Extremely fine
particles can form sludges or suspensions that are difficult to clarify or filter. It is
essential to conduct thorough laboratory testing and modelling to identify the size range
that maximizes leaching efficiency while considering practical limitations. This may
involve trade-offs between faster kinetics associated with smaller particles and the
operational challenges they present.
3.7 Optimum particle size
One way to determine the optimum size for the leaching process is to conduct
experiments with different particle sizes and observe the leaching efficiency. For
example, in a study on copper recovery from waste printed circuit boards, the optimum
particle size was found to be 150 mesh according to the leaching efficiency [6]. The
smaller the particle size, it has a bigger surface area that leads to an increase in leaching
kinetic. However, the effect of particle size is also correlated with the precedent
processing stage. To get smaller particle size, grinding circuits need a higher energy
consumption per amount of material produced. Hence, there is a trade-off between
leaching recovery and operational cost for grinding circuits.
4. Conclusions
The fraction of chalcopyrite converted during the leaching process was calculated and
presented in Tables 3 and 4. It is evident that leaching at higher temperature (52°C)
exhibited a higher conversion rate compared to a room temperature (25°C). After 300
minutes of leaching, the conversion rates were 0.503% and 0.179% for experiments C
and D, respectively. This variation is attributed to differences in reagent concentration
and temperature. The linear regression analysis results indicate that the rate control of
the reaction is diffusion through the solid product layer, even though the value of
activation energy was 60.72kJ/mol that was probably caused by unreacted minerals.

9
10
 EXPERIMENT 2- CURRENT EFFICIENCY FOR ZINC
ELECTRODEPOSITION

1. Introduction.
1.1. Theory:
Electrode reactions are mainly redox reactions forced by a power source (electricity). A
net flow of charge travel into the electrode or out the electrode where reduction and
oxidation respectively take place. A change in the electrochemical potential occur when
the reaction happens, from an initial equilibrium Eeq to a new one Ereaction . this change
can be represented by the term polarisation potential or overpotential and given by
equation 1 below, and the net current that flows is the difference between the anodic i a
and the cathodic i c current as shown in equation 2:

η=Eeq −Ereaction (1)

i=i c −i a (2)

There are two types of polarisation potentials based on the cause of occurrence:

a- Activation polarisation: the reaction is chemical controlled and the change is due to
the activation energy for the electrode process.
b- Concentration polarisation: the reaction is transport controlled and the change is
due to a decrease in the concentration of reactant ions in the vicinity of the
electrode.

The relationship between the net current density j ( mA ) and the overpotential can be
2

given by the Tafel equation show below:

η=a−b ln j(3)
Where a and b are Tafel constants, unique values for each element redox reaction.

For the theory of the zinc electrodeposition, hydrogen overpotential on the surface of
the cathode can happen. Many factors can affect the hydrogen overpotential such as pH,
current density, and temperature. The current efficiency of electrodeposition has been
shown to be greatly affected by small concentrations of certain impurity ions in the acid
sulfate baths.

The presence of impurities on the cell can increase the hydrogen evolution by:

a- Acting as centres of low hydrogen overvoltage that permit discharge of hydrogen

to occur in preference to zinc electrodeposition.

b- Acting as galvanic couples with zinc, thus accelerating the dissolution of the zinc
electrodeposit with subsequent hydrogen evolution.

11
1.2. Objectives

a- Determining the current efficiency for the electrodeposition of zinc from a pure
zinc sulfate solution at the zinc cathode.

b- Studying the effect of various solution impurities on the current efficiency.

c- Determining the hydrogen overpotential at experimental conditions for each metal

(Copper and Tin) deposited.

2. Materials and Methods.

2.1. Material:

Equipment:
5ml burette, Ammeter, 250ml beaker, Stopwatch, lead anode, Electrical connecting
wire, 7 x zinc cathodes, Switch Voltmeter and Rheostat

Solutions:
Zinc sulfate solution (50g/L Zn and 1M H2SO4)
Cadmium chloride solution (0.1M)
Copper sulfate solution (0.1M)
Stannous chloride solution (0.1M)

2.2. Methods:

Current Efficiency:
A 200ml of the pure zinc sulfate solution was added to 250 ml beaker. Four zinc
cathodes were polished, washed with water and acetone, dried and weighed. The
dimension of each zinc electrode was measured to calculate the area and hence the
current required to give a current density of 400 A /m2.
The reaction was initiated by closing the circuit and inserting the cathode, and the
clock was started. Using the rheostat, the current density was adjusted to 400 A/m 2 and
maintained the current at the set value throughout the experiment. The cell voltage
should be about 3.5V but will vary according to solution resistance, temperature,
distance between electrodes, etc.
After 20 minutes the reaction was stopped. The electrodes were washed with water and
acetone and weighed again when dried.
Effect of impurities:
0.1M Copper and 0.1M Tin impurities are supplied. The same method has been used to
Determine the current efficiency for zinc sulfate solutions containing firstly 2mL then
5mL of one of these impurities using a fresh zinc cathode.

12
3. Results and Discussion.

The current efficiency was calculated using the following equation:

actual mass deposited

Efficiency= (4 )
theoretical ( Farad y ' s law )

For the Faraday’s law:

MAt
W= (5)
nF
Where:
W : weight deposited.
M: Molecular weight of the zinc element.
A: current (0.4 A ∈this experiment )
t: time (20 minutes = 1200 seconds)
n: number of electrons transferred.
F: Faraday’s constant 96485

For the Zinc:

−¿→Zn ¿

Z n2 +¿+2 e ¿

Then:
65.38∗0.4∗1200
W= =0.1626
2∗96485

The efficiency for the first sample of 0.1636g deposited is:

0.1636
≅1
0.1626

The efficiencies for the other five samples are shown in table below:

Concentration Zn Weight Before Zn Weight After Zn mass

Current
Impurities in the solution electrodeposition electrodeposition deposited
Efficiency
(M) (g) (g) (g)

Non 0 6.853 7.0166 0.1636 1.005974

Non 0 3.7008 3.8588 0.158 0.97154

2ml Sn 0.00099 9.9984 10.1451 0.1467 0.902057

5ml Sn 0.0024 7.9619 8.0907 0.1288 0.79199

2ml Cu 0.00099 7.5608 7.7198 0.159 0.977689

5ml Cu 0.0024 4.1465 4.3003 0.1538 0.945714

Table 1 Calculated Efficiencies for different impurities

13
 It can be noticed that the presence of impurities generally decreases the current
efficiency of the cell. The hydrogen gas coming out from the electrode was observed
and has increased as impurities presented in the cell. However, Copper didn’t have a
great impact on the efficiency dropping. The suggested reason is that for the efficiency
dropping to happen, the zinc should dissolve in into the solution, and at a certain
concentration the copper deposit would be enough to create a local galvanic cell.

The relation between the concentration of the impurities and the efficiency was also
studied. Figure 1 shows how does the concentration effects the efficiency.

Figure 1 Efficiency VS Concentrations of impurities

Increasing the concentration of the impurities has effect of the efficiency of the cell, the
direct proportion suggested that increasing the impurities ions interfere with the zinc
ions.

The hydrogen overpotential was calculated for the impurities Cu and Sn using equation
3 and the results are shown in table 2 below:

a b η

Zn 1.24 0.118 0.533007183

Sn 1.24 0.116 0.544990113

Cu 0.8 0.115 0.110981577

Table 2 Calculated Overpotential values.

4. Conclusion.

As Kerby and Ingraham suggested [7], the results show that the current efficiency is
affected by the concentration of impurities. The more concentrated the impurity ions

14
 are, the more drop the efficiency will have. They have classified the impurities to four
main classes, Tin is in class three, which has high hydrogen overvoltage and tend to
alter the crystalline structure of zinc deposit. Copper on the other hand is in class four,
which has low hydrogen potential and small effect on the cell efficiency.
EXPERIMENT 4 – LEACHING OF COPPER IN AN AMMONIACAL
SOLUTION

1. Introduction
1.1 Theory
Ammonia leaching has been widely used in hydrometallurgy for processing of
sulphide and oxide ores, concentrates or by-products, this solvent can be
effectively used for leaching of base metals (Copper, Niquel, Cobalt, Zinc) as well
as for precious metals (Gold, Silver). Additionally. in the case of materials
containing copper-iron and iron minerals (chalcopyrite, bornite, pyrite, pyrrhotite)
it could be beneficial because of its selectivity, which means that allows the
selection of the desired metals to be solubilized while undesired iron can be
precipitated, everything in just one operation. Beside this, it is considered a useful
leaching agent due to several factor such as low grade of toxicity, accessible cost,
and easy regeneration process from alkaline solution [8].

The experiment is going to be addressed with cooper and an ammonia reagent for
the leaching of copper, this base metal (copper) is soluble in an ammoniacal
solution according to the reaction:

−¿¿
2+¿+4 O H ¿
2 Cu+ xN H 3+O 2+2 H 2 O=2 Cu ( NH 3 ) x
2

The reaction is characterised as an electrochemical in nature.

1.2 Objectives
The aim of this experiment is examining how the reaction is influenced by
variations in the concentration of ammonia and adjustments in stirring speed and
temperature. The ammonium ion concentration will remain constant.
The lab for this group 5 is composed of developing the second analysis based on
effect of stirring speed on leaching rate.

2. Procedure
Effect of Stirring Speed on Leaching Rate Experiment
A copper disc with a diameter of 3.7 cm is going to be used in the experiment, it is
crucial to clean the copper coin by abrading and polishing one or both surfaces, for
this experiment is used a sandpaper and both sides were cleaned. Beside this, the

15
 copper coins were placed into two different leaching vessels where the
concentration of ammonia to study was 0.05 M and 0.01 M.

 Preparation of 800cm3 of a solution of approximately 0.01 and 0.05 M NH 3

containing 10g of ammonium sulphate.
 Prepare the copper discs and place those in the leaching vessels.
 Position the stirrer about 3cm above the disc and start it at about 30rpm.
 Add the solution and noting the time.
The experiment is addressed taking in consideration several factors. Firstly, the
samples are going to be taken every 10 min for 90 min with a total of 9 samples for
each concentration. Secondly, the stirring speed is going to be modified three times
from 30 rpm to 80 rpm finishing with 120 rpm. Finally, the sample are going to be
labelled with the relevant information and given to the lab staff to analyse the Cu
by AAS. Information provided in table 1.

Vassel Sample rpm Time (min)

0.01 30 10
0.01 30 20
0.01 30 30
0.01 80 40
1 0.01 80 50
0.01 80 60
0.01 120 70
0.01 120 80
0.01 120 90
0.05 30 10
0.05 30 20
0.05 30 30
0.05 80 40
2 0.05 80 50
0.05 80 60
0.05 120 70
0.05 120 80
0.05 120 90
Table 1 Theoretical settings for taking samples.

3. Calculation
Solution needed for each concentration of ammonia.
C1V1 = C2V2
- (0.05) x (800mL) = 1(V)
- 40 mL NH3
- (0.01) x (800mL) = 1(V)

16
- 8 mL NH3
Area of the copper coin.

Figure 1 Copper coin used in the experiment.

The diameter of the copper coin is 3.7 cm.

A = πr2
- A = 3.1416 x (1.85)2 = 10.75184

During the experiment was not possible to set the stirring speed to 30 rpm, the
stirring speed used is specified in the table 2.

Vassel Sample rpm

0.01 38.2
0.01 38.2
0.01 38.2
0.01 83.2
1 0.01 83.2
0.01 83.2
0.01 119
0.01 119
0.01 119
0.05 34.5
0.05 34.5
0.05 34.5
0.05 82.1
2 0.05 82.1
0.05 82.1
0.05 117
0.05 117
0.05 117
Table 2 Stirring speed adjusted for the experiment.

17
4. Results
To determine the leaching rate in g Cu/cm 2/second for each experiment it is
essential to know the results of the copper concentration that is shows in table 3.

Variables in consideration are:

Time = 600 sec (every 10 min each sample).
Surface Area = copper coin = 3.1416 x (1.85)2 = 10.75184 cm2
Quantity of substance leached (g) = Sample (mg/L)/ 1000
In order to have a good representation of the sample concentration the leaching
rate is going to be display in a ratio of 10^9 as the table 3 & 4 shows.

Vassel Sample RPM Time(min) Cu (mg/L) Leaching rate * 10^9

0.01 38.2 10 0.03 4.65036746539
0.01 38.2 20 0.11 17.05134737309
0.01 38.2 30 0.28 43.40342967695
0.01 83.2 40 0.4 62.00489953849
1 0.01 83.2 50 0.56 86.80685935389
0.01 83.2 60 0.76 117.80930912314
0.01 119 70 0.95 147.26163640392
0.01 119 80 1.19 184.46457612702
0.01 119 90 1.5 232.51837326935
Table 3 Experiment 0.01 concentration result

It is possible to notice in the figure 2 the concentration of copper that was leached.
It is notorious to evidence the increment of copper leached when the stirring rate
increased, with 38.2 rpm was a total of 43.4, 83.2 rpm was a total of 74.4 and 119
rpm was a total of 114.7 the leaching rate difference between the starting point and
ending point.

18
 Figure 2 Leaching Rate 0.01 Ammonia concentration.

Ti
m
Cu Leachi
Va Sa r e
(m ng
ss mpl p (
g/L Rate *
el e m m
) 10^9
in
)
2 3
0.0 4 1 0.0
5 . 0 3
5 4.7
3
0.0 4 2 0.0
5 . 0 7
5 10.9
3
0.0 4 3 0.0
5 . 0 8
5 12.4
8
0.0 2 4 0.4
5 . 0 3
1 66.7
8
0.0 2 5 0.5
5 . 0 5
1 85.3
0.0 8 6 0.6 99.2
5 2 0 4

19
 .
1
1
0.0 7 0.7
1
5 0 4
7 114.7
1
0.0 8 0.8
1
5 0 4
7 130.2
1
0.0 9 0.9
1
5 0 5
7 147.3
Table 4 Experiment 0.05 concentration result
As before, figure 4 shows the concentration of copper that was leached. It is
possible to see the increasing concentration of copper leached when the stirring
rate was settled with to high values such as 34.5 rpm was a total of 12.4, this result
is possibly wrong because it is not going with the trend, theoretically is around
18.6 according to the slop equation where m = 0.62, the 82.1 rpm was a total of
32.5 and 117 rpm was a total of 32.6 the leaching rate difference between the
starting point and ending point. Therefore, it is possible to highlight that apart from
34.5 rpm the trend of the graph was lineal and the stirring as a transport control is
being effective.

Figure 3 Leaching Rate 0.05 Ammonia concentration.

5. Conclusion
These linear results graphed suggests that increasing the stirring rate consistently
and proportionally accelerates the rate of transport of the leaching solution, which
consequently affects the amount of substance leached. Therefore, the stirring rate
has a significant impact on the leaching process under these conditions, indicating
transport control as a dominant factor.
20
21
 EXPERIMENT 5- SOLVENT EXTRACTION OF COPPER

1. Introduction
1.1 Theory of Solvent Extraction
One of the key options for producing copper from low-grade ore is the solvent
extraction process. Solvent extraction is a technique for selectively removing or
extracting a species from one liquid phase into another. This technique can be used to
separate valuable species (such as copper) from impurities. To minimise excessive
solvent loss, these two solutions must be insoluble and immiscible [9].
The solution from which the extraction is made in hydrometallurgical copper processes
is a dilute acid solution. In copper processing, sulphuric acid is usually used as dilution
[10]. Copper is recovered by mixing a copper sulphate solution with an immiscible
organic solution. In this process, copper ions will be transferred to the organic phase,
thus the organic phase is called "loaded organic". The barren aqueous phase, called
raffinate, is reused as lixiviant. Next, the loaded organic is stripped to separate the
copper ion from the organic phase to the copper solution aqueous phase. The extraction
and stripping process can also be explained by the reaction 1 below [11].

Extraction
[2 RH](org.) + [CuSO4](aq.) [R2Cu](org.) + (2H+SO42-](aq.) (1)
Stripping

RH is an extractant solution, typically using hydroxyphenyl oximes for copper

extraction. The extractant is not used in pure condition for economic reasons.
Therefore, it must be diluted in an affordable solution, usually kerosene [9].
The stripped organic, called "barren organic," is returned to the extraction step. The
copper solution will undergo an electrowinning technique to recover the copper.
Overall, the whole process of solvent extraction and electrowinning process can be
summarized in Figure 1.

Figure 1. Solvent extraction and electrowinning process cycle [9].

1.2 Objective
The main objective of this experiment is to familiarize with the solvent extraction
process on a laboratory scale and the data analysis.

22
2. Materials and methods
2.1 Materials
In this laboratory experiment, three different solutions were used as a feed solution.
The first solution, called solution A, is composed of 1 g/L Cu 2+, 3 g/L Fe 3+, 0.5 M
Na2SO4 adjusted to pH 2.2 with H2SO4. The second solution is solution B, which
consists of 8g/L Cu2+, 0.5M Na2SO4, and natural pH. The last solution is solution C
which contains 20g/l Cu2+, 150g/L H2SO4, 0.5M Na2SO4. An extractant solution is used
with 10% volume of the complexing agent in an organic solvent.
2.2 Methods
There are two main experiments: batch loading experiment and stripping loading
experiment.
2.2.1. Experiments with Batch Loading
30cm3 of aqueous feed solution A was added to five beaker glasses to mix it with
organic extractant with different volumes. 60 cm3 of organic extractant was added to the
first beaker, 30 cm3 to the second, and 15, 7.5, and 3.75 cm3 of organic extractant was
added to the rest of the beaker glass. All mixed solutions were stirred for 15 minutes
with a magnetic stirrer. The aqueous solution from each beaker was sampled after
stirring. The sample was used to determine the copper concentration of the aqueous
phase using Atomic Absorption Spectroscopy (AAS).

2.2.2. Experiments with Batch Stripping

200 cm3 extractant solution was mixed with 200 cm 3 solution B in 400 cm3 beaker
glass. The mixed solution was stirred for 15 minutes, and after the phases were
separated, the aqueous phase was sampled to identify the copper concentration. The
loaded extractant was used in the stripping experiment. It will be transferred to four
beaker glasses with 40 cm3 loaded extractant per glass. 40 cm3 of solution C was
added to the first glass, 10 cm 3 to the second, 5 cm3 to the third, and 2 cm 3 to the fourth.
All mixed solutions were stirred for 15 minutes. Aqueous solutions left in beaker
glasses were sampled after stirring to determine the copper concentration using AAS.

All experiments were done at room temperature (28oC). The result of the experiment
was analysed to construct an equilibrium loading isotherm and equilibrium stripping
isotherm. Additionally, McCabe-Thiele Diagrams were also applied to equilibrium
isotherm to determine the number of stages required to achieve a specified copper
separation between the organic and aqueous phases. An equilibrium loading isotherm
for copper is shown in figure 2. Drawing an operational line with slope A/O passing
through the point (xj,o) produces a McCabe-Thiele diagram for extraction, where xj is
the final aqueous solution concentration required. The figure is then completed by
drawing horizontal and vertical lines alternating between the operating and equilibrium
lines, starting with the first horizontal line drawn through (xo, y1). Each triangular step,
1, 2, symbolises a stage of extraction [12].

23
 Figure 2. McCabe-Thiele Diagrams for copper extraction (Dyer, 2023)

3. Results and Discussions

3.1 Equilibrium Loading Isotherm.
The pH and copper concentration aqueous phase or raffinate of the loading experiment
is determined in Table 2.

Table 2. Copper concentration in raffinate

The pH of raffinate decreases as copper concentrate decreases because the higher the
extracted copper to the organic phase, the higher the H+ ion will produced, which
follows reaction 1. To obtain the copper concentration in the organic phase, the mass
balance method is used by subtracting the copper mass in the feed A from the aqueous
phase. The calculation is shown below:
Determine the copper mass in the feed solution A:
Copper concentration in feed solution A = 1.133 g/L
Volume of solution A = 30 mL
Mass of copper in feed solution A = 1.133 g/L x 0.03 L = 0.0339 gram

24
Determine the copper mass in aqueous solution A:
Volume = 3.75 mL
Copper concentration (after accounting dilution factor) = 100 * 8.27 = 827 mg/L =
0.827 g/L
Copper mass in 3.75 mL solution A = 0.827 g/L* 0.00375 L = 0.02481 gram
Copper mass in that organic phase = 0.0339 gram – 0.02481 gram = 0.00918 gram
Therefore, copper concentrations in organic phase = 0.00918 gram / 0.00375 L = 2.448
g/L
The rest of calculation is done with same method, thus overall result can be shown in
Table 3. From this table, equilibrium loading isotherm can be constructed as illustrated
in Figure 3.

Table 3. Loading experiment result summary

12

10
Cu Concentration (g/L) organic

0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Cu Concentration (g/L) aqueous

Figure 3. Equilibrium loading isotherm diagram.

Results of this experiment show that the higher the volume of organic added to a
solution, the higher the copper concentration extracted from the aqueous solution.
99.5763 % of copper was extracted in 60 mL of organic extractant, while in 3.75 mL,
only 27% of copper was extracted. This result is happening because the larger volume
of organic extractant will contain a higher volume of extracted copper concentrate from
25
 the feed solution. Nevertheless, a higher volume of extractant will cost more for the
operation expenditure. Therefore, the optimum volume of extractant is needed to have a
high extraction value and low cost.
3.2 Equilibrium Stripping Isotherm
In the stripping experiment, copper concentration in the aqueous solution C, feed
solution C, feed solution B, and loaded solution B was identified by AAS, shown in
Table 4.

Table 4. Copper concentrations result from stripping experiments.

To obtain the copper concentration in the organic phase in the stripping experiment,
mass balance methods are used. The calculation will be shown below:
Determine the copper mass in feed solution B:
Volume = 200 mL
Copper mass = 1,840 mg/L x 0.2 L = 368 mg

Determine the copper mass in loaded solution B:

Volume = 200 mL
Copper mass = 185 mg/L x 0.2 L = 37 mg

Determine the copper concentration in loaded extractant:

Copper mass = copper mass in feed solution B – copper mass in loaded solution B
= 368 – 37 = 331 mg
Volume loaded extractant = 200 mL
Copper concentration = 331 mg / 200 mL = 1.655 mg/mL = 1.655 g/L

Determine the copper concentration in organic solution C at 40 mL:

26
Volume = 40 mL
Copper concentration = 22,548 mg/L / 1000 = 22.54 g/L
Copper mass = 22.54 g/L x 0.04 L = 0.90192 g
Initial copper mass = 20,900 mg/L x 0.04 L / 1000 = 0.836 g
Copper mass in organic phase = (1.655 g/L x 0.04 L) – (0.90192 – 0.836) = 0.00028 g
Volume organic phase = 40 mL
Copper concentration in organic phase = 0.00028 g / 0.04 L = 0.007 g/L
The rest of calculation is done with same method, thus overall result can be shown in
Table 5. From this table, an equilibrium stripping isotherm can be constructed, as
illustrated in Figure 4.

Table 5. Calculated data.

30

25
Cu Concentration (g/L) aqueous

20

15

10

0
0 0.5 1 1.5 2 2.5
Cu Concentration (g/L) organic

Figure 4. Equilibrium stripping isotherm

27
3.3. Determination of A/O Ratio Counter Current
To determine the A/O ratio required to reduce 1 g/L Cu 2+ feed to 0.04g/l in three stages,
assuming 0.02g/L Cu2+ in the organic feed (counter-current), McCabe – Thiele diagram
is applied as depicted in Figure 5. Inferred from Figure 6, the aqueous and organic
phases flow in opposite directions. This means that as the aqueous phase (often the feed
solution) flows in one direction, the organic phase flows in the opposite direction. This
mechanism provides maximum contact between the two phases, which enhances mass
transfer and extraction efficiency [13]. However, its design is more complex than the
crossflow system.
The slope of the operating line is determined to obtain three stages. Then, the A/O ratio
is a slope that can be determined by the gradient formula.
y 2− y 1 2.4−0.02
m= m= = 2.38
x 2−x 1 1−0

It is found that the slope or A/O ratio to obtain three stages is 2.38.
3

2.5

1
Cu Concentration (g/L) organic

1.5 2 A/O = 2.38

1

3 0.5

0
-0.3 0.2 0.7 1.2
Cu Concentration (g/L) aqueous

Figure 5. McCabe – Thiele diagram counter current, A/O = 2.38

Figure 6. Schematic of counter-current flow (Koch-Modular, 2020)

28
 Where A and B are feed solution, C is organic extractant, R is raffinate, and E is loaded
extractant.

3.4. Determination of Stages

To determine stages that would be required to reduce 1g/L Cu feed to 0.2g/L, assuming
0.1g/L Cu in the organic feed and A/O ratio of 0.5, the McCabe – Thiele diagram was
also constructed in Figure 6. From the graph, it can be concluded that the number of
stages that would be required is one stage.

2.5
Cu Concentration (g/L) organic

1.5

0.5
1 A/O = 0.5
0
-0.3 0.2 0.7 1.2
Cu Concentration (g/L) aqueous

Figure 6. McCabe – Thiele diagram counter current, A/O = 0.5

3.5. Determination of A/O in Cross Flow System

To determine the A/O ratio required to reduce 1 g/L Cu 2+ feed to 0.04 g/l in three
stages, assuming 0.02g/L Cu2+ in the organic feed with cross flow system, McCabe –
Thiele diagram is utilized as shown in Figure 8. In a crossflow system, the aqueous and
organic phases move in the same direction, parallel to each other, as seen in Figure 9.
Crossflow systems often have lower extraction efficiency because of the shorter contact
period between the phases than counter-current flow systems. This method stands out
for its simplicity and cheaper equipment costs than counter-current flow systems [13].
The slope of the operating line is determined to obtain three stages. Then, the A/O ratio
is a slope that can be determined by the gradient formula.

y 2− y 1 2.2−0
m=
x 2−x 1
m=
0.46−1
= -4.074

29
 3

2.5

Cu Concentration (g/L) organic

2

1.5

1 1 A/O = - 4.074
2
0.5

3
0
-0.3 0.2 0.7 1.2
Cu Concentration (g/L) aqueous

Figure 8. McCabe – Thiele diagram for cross flow system

Figure 9. Schematic of the crossflow system (Koch-Modular, 2020)

Where A and B are feed solutions, C is an organic extractant, R is raffinate, E is a

loaded extractant, and M is a composition of phase mixture.
4. Conclusions
The experimental results presented in this report provide insight into the behaviour of a
specific extractant system during the copper solvent extraction process. The equilibrium
loading isotherm, as depicted in Figure 3, reveals that the copper concentration in the
organic phase increases with the higher volume of organic extractant. Notably, the data
shows that 99.5763% of copper can be extracted when 60 ml of organic extractant is
used, while only 27% of copper is extracted with 3.75 ml. On the other hand, the
equilibrium stripping isotherm, illustrated in Figure 4, demonstrates the reverse process,
where copper is transferred from the organic phase back to the aqueous phase.
Moreover, the report explores the determination of A/O (aqueous-to-organic) ratios in
counter-current and crossflow systems, providing valuable insights for the design and
optimization of copper solvent extraction processes. To reduce 1 g/L Cu2+ feed to
0.04g/l in three stages, the A/O ratio value is 2.38 in the counter-current system, while
in the crossflow system, the A/O ratio value is -4.074. Additionally, the experiment
shows that reducing 1g/L Cu feed to 0.2g/L in an A/O ratio of 0.5, only needs one stage.
These findings contribute to a better understanding of the dynamics of copper solvent
extraction and will guide future efforts in developing efficient separation processes for
this valuable metal.

30
 EXPERIMENT 6- RESIDENCE TIME AND NON-IDEAL FLOW

1. Introduction
1.1. Theory:

Space time τ is the time required to process one reactor volume. In batch reactors, all
the fluid elements spend the same amount of time in the reactor, and if the density is
constant through the reaction, the space time will be the same as the mean residence
time.

τ =t=t
Same concept can be applied to the plug flow reactor where there is no density charge.
The residence time can be given by equation 1 below:
X Af
d XA
τ =t=C A 0 ∫ (1)
0
−r A

In the back-mix reactors, some of the fluid elements can pass through the reactor
quickly and others can remain in the reactor for long time. In this case the residence
time of the reactor is hard to be determined. However, residence time distribution RTD
can be produced. The mean residence time t can be equated to τ if the density in
constant.

V
τ =t= (2)
v0

There are two main types of stimulus-response or tracer techniques (step and pulse),
they can be used to determine the mixing characteristic of a non-ideal reactor. A
stimulus (tracer) is input to the vessel and the response is measured in the exit stream
over time. Usually, the tracer is a radioactive isotope or an inert chemical.

Consider an instantaneous injection of an inert chemical A into a CSTR.

Inert A

vo

Inert A

vo

31
32
 Rate that A exits the reactor:

dA N
=−C A v o =− A v o
dt V -ve indicates leaving reactor

Rearrange and integrate:

A t
vo
∫ dA =−∫ dt
A NA
o
0 V

v0
Ln N A - Ln N Ao=− t
V
NA
=e
( )
−v0 t
V
N Ao

Retention time is the average time a molecule of A spends in the reactor:

V
t=
ν0
(3)

∴
NA
=e
( − )
t
t

or
CA
=e
( − )
t
t

N Ao C Ao

The ratio of CA to CAo in the exit stream can then be calculated at any time t.
Note that CAo is the initial concentration in the reactor, not the concentration of the
tracer when it is being injected.

At t=t
CA −1
=e =0.368 C A =0.368 C A 0
CA 0

That means, 36.8% remains in the tank and 63.2% has exited the tank. The exist age
distribution can be represented by a graph using equation 3 as shown in figure 1 below:

33
 Figure 3 Relative concentration of A in the reactor as a function of mean time.
It can be noticed from the concentration of A in the CSTR, particles start to leave right
after the injection. This would cause a problem in surface contact processes like
leaching because the particles don’t have enough time to react with the solution.

The Erlang equation gives a representation of the shape of the distribution curve for
multiple CSTRs in series.

CA n
n
n−1 −n t
RTD= = t e r

C A 0 ( n−1 ) ! r
Where:
n: number of reactors in series.
t r: reduced time t /t .

The stimulus-response studies can be used to study the efficiency of the reactors. six
scenarios have been introduced by Levenspiel to diagnose the faulty flow and suggest
causes. Figure 2 shows these suggestions.

Figure 2 Misbehaving Mixed Flow Reactors

34
 1.2. Objective:

a. Studying the residence time for a single CSTR.

b. Investigating the possible problems resulted from the deviation of Ideal reactors.

2. Materials and Methods

2.1. Materials:
Equipment
2 continuously stirred tank reactors, Peristaltic pump, 2 x 100 mL measuring cylinders,
2x 1000 mL measuring cylinders, 50 mL injection syringe, 5 x 100 mL volumetric
flasks, 10 x 100mL beakers or sample vials, Water storage tank, pH meter and probe, 1
mL and 10 mL pipettes and filler
Chemicals
100 mL of 5 mol/L acetic acid.
Calibration standards for pH meter

2.2. Methods:
The whole experiment has been conducted using the tap water.
A 100 ml of 5 mol/L acetic acid was used as a tracer, 5 samples of different dilution
factors were prepared, and pH was measured for each to get a calibration curve as
follow:

Dilute a sample of the 5 mol/L solution by 100 (0.05 mol/L)

Measure the pH of the solution.

Dilute a sample of the 0.05 mol/L solution by 10 (0.005 mol/L)

Measure the pH of the solution.

Dilute a sample of the 0.005 mol/L solution by 10 (0.0005 mol/L)

Measure the pH of the solution.

Dilute a sample of the 0.0005 mol/L solution by 10 (0.00005 mol/L)

Measure the pH of the solution.

35
Single Reactor:

Using a single reactor, the volume of the reactor was measured and filled with tap water
by using a measuring cylinder. The Agitation has been started and pump power was
adjusted to 200 mL/min.
The exact volumetric flow rate has been measured to calculate the residence time using
equation 2. At time zero a 20 mL of 5 mol/L acetic acid was injected into the reactor at
the base of the reactor under the impellor.
A 10 ml of samples were collected at 0.1 times the mean residence time for one mean
residence time of the reactor. Then 0.5 times the mean residence time for a further two
mean residence times of the reactor. The pH was measured for each of the samples.
Multiple Reactors:
Two reactors in series were connected. The Agitator has started, and the pump was
adjusted to give a volumetric flow rate of about 400 mL/min.
The exact volumetric flow rate was measured, and the mean residence time was
calculated using the equation 2. At time zero a 20 mL of 5 mol/L acetic acid was
injected into the first reactor at the base of the reactor under the impellor.
Samples of about 10 mL were collected at 0.1 times the mean residence time for one
mean residence time of the reactors. Then 0.5 times the mean residence time for a
further two mean residence times of the reactors. The pH was measured for each of the
samples.

36
3. Results and Discussion.

● Prework
1. Single CSTR plotting using equation below with an assumption t=1.

CA ( −t )
=e t
C Ao
1.2

0.8
CA/CA0

0.6
Theroretical (t*10)
0.4

0.2

0
0 0.5 1 1.5 2 2.5 3 3.5
t (0.1min)

Figure 3 Mass Conversion vs Mean Residence Time for Single CSTR

2. Plotting of residence time distribution with two reactors in series
CA n
n
n−1 −n t
RTD= = tr e r

C Ao (n−1)!

0.8
0.7
0.6
0.5
CA/CA0

0.4
0.3
0.2
0.1
0
0 0.5 1 1.5 2 2.5 3 3.5
Time (minutes)

Figure 4 CSTR with two reactors in series

37
 3. Plotting of CSTR with single, two, five, and ten reactors in series.

CA n
n
n−1 −n t
RTD= = t e r

C Ao (n−1)! r

1.4

1.2 CSTR 2 in Series

CSTR 5 in Series
1
CSTR 10 in Series

0.8 Single CSTR

CA/CA0

0.6

0.4

0.2

0
0 0.5 1 1.5 2 2.5 3 3.5 4
Mean Residence Time
Figure 5 Plotting of Mean residence time vs CA/CA0 in various CSTR.

 Experimental Results
The concentration of tracer (acetic acid) is measured in periodic times. The plotting of the ratio
of tracer concentration at specific time and initial tracer concentration versus mean residence
time is compared with the theoretical line for both single CSTR and Two Reactor in Series. The
results are depicted in Figure 6 and 7, respectively. The experimental results of single reactor
and two reactor is reasonably good flow compared to theoretical results based on the Figure 1
illustration for single reactor and Figure 8 for two reactors. Despite the good flow results, it still
has deviation to theoretical results.

Deviation between experimental line and theoretical line of single CSTR is probably caused by
imperfect mixing that can result in tracer concentration gradient within the reactor [4]. To
provide homogeneous reaction conditions and high conversion rates, single CSTR rely on
efficient reactant mixing. Imperfect mixing can result in concentration gradients, incomplete
reactions, and overall reactor misbehaviour. In some conditions, temperature and pressure
gradients in single reactor can alter reaction rate and selectivity. These gradients can be
caused by insufficient mixing, heat transmission limits, or other circumstances, resulting in the
reactor misbehaving [14]. Another reason for imperfect mixing is the speed of the stirrer
factor. The stirrer speed must be set to the optimum value to achieve the best mixing results.
Suppose the stirrer speed is not in optimum value. In that case, the contact between the acetic
acid and the water will not be in perfect condition, thus reducing the conversion rate and
resulting in deviation results [4] [15] .

38
 Deviation in two reactor results is also caused by imperfect conditions and parameters,
resulting in imperfect mixing between acetic acid and water and misbehaving in two reactor
results. The imperfect condition is like the single reactor condition, which is a non-optimum
temperature, pressure, and stirring speed, which leads to deviation results between
experimental and theoretical results. Additionally, In the two-reactors experiment, the
presence of dead zone or stagnant fluid regions in the reactor and pipe is more significant than
in a single reactor [4]. This dead zone can affect the conversion rate performance and lead to
deviation.

1.2

1
Experiment
0.8
Theoritical
CA/CA0

0.6

0.4

0.2

0
0 0.5 1 1.5 2 2.5 3 3.5
Mean Residence Time

Figure 6 Comparison between experimental and theoretical single CSTR curve

0.8

0.7

0.6

0.5 Theoretical

Experimental
CA/CA0

0.4

0.3

0.2

0.1

0
0 0.5 1 1.5 2 2.5 3 3.5
Time (min)

Figure 7 Comparison between experimental and theoretical two reactors in series

39
 Figure 8. Misbehaving in plug flow reactor for two reactor experimental results [4].

4. Conclusion.

In conclusion, the experiment describes a study that focused on measuring the

concentration of acetic acid tracer at regular intervals and comparing the results with
theoretical expectations within the context of both single Continuous Stirred-Tank
Reactor (CSTR) and two CSTRs in series. The experimental findings, presented
graphically in Figure 4 and 5, generally exhibited a reasonable alignment with
theoretical projections in Figures 6 and 7. However, deviations were observed, which
were primarily attributed to imperfect mixing conditions within the reactor systems. In
single CSTR setups, variables such as temperature and pressure gradients and stirrer
speed were identified as influential factors affecting reaction rates and selectivity.
Furthermore, in the two-reactor configuration, the presence of dead zones or stagnant
fluid regions exacerbated the observed deviations. The insights gained from this study
underscore the significance of addressing issues related to mixing and reactor
conditions to improve the accuracy of chemical processes. These findings contribute
valuable knowledge regarding the complex dynamics of CSTR systems and offer
guidance for future process optimization endeavours.

40
 References

[1] J. E. E. O. G. O. B.C. Tanda, “The kinetics of chalcopyrite leaching in alkaline glycine/glycinate solutions,”
Minerals Engineering, vol. 135, pp. 118-128, 2019.

[2] E. A. C. N. F. A. M. M. H. A. S. B. F. &. M. Prasetyo, “Monosodium Glutamate as Selective Lixiviant for

Alkaline Leaching of Zinc and Copper from Electric Arc Furnace Dust,” MDPI, vol. 644, no. 10, 2020.

[3] M. E. W. Hong Yong Sohn, Rate processes of extractive metallurgy, New York: Plenum Press, 1979.

[4] O. Levenspiel, “Chemical Reaction Engineering.,” John Wiley & Sons., 1999.

[5] T. Havlik, Hydrometallurgy principles and application.., England: Cambridge International Science
Publishing Limited, 2008.

[6] J. W. X. W. Y. W. Y. &. G. F. Hao, “Optimizing the Leaching Parameters and Studying the Kinetics of Copper
Recovery from Waste Printed Circuit Boards,” ACS Omega, vol. 7, pp. 3689-3699, 2022.

[7] R. a. I. T. KERBY, “Effect of Impurities on the Current Efficiency of Zinc Electrodeposition,” Dept. Energy,
Mines and Resources, Mines Branch,, Ottawa, 1971.

[8] W. J. CHMIELEWSKI T., “ AMMONIA PRESSURE LEACHING FOR LUBIN,” Physicochemical Problems of
Mineral Processing, pp. 5-20, 2009.

[9] V. P. K. &. D. N. A. M. S. Prasad, “Development of SX-EW Process for Copper Recovery,” Mineral Processing
and Extractive Metallurgy Review, vol. 8, pp. 1-4,95-118, 1992.

[10] T. C. Katarzyna Rotuska, “GROWING ROLE OF SOLVENT EXTRACTION IN COPPER ORES PROCESSING,”
Physicochemical Problems of Mineral Processing, vol. 42, pp. 29-36, 2008.

[11] G. A. Kordosky, “Copper solvent extraction: The state of the art,” Journal of Metals, vol. 44, pp. 40-45,
1992.

[12] B. T. B. A. L. D. Hugo Guerra, “Nanofiltration for treatment of Western Australian bore water for mineral
processing operations: A pilot scale study,” Journal of Water Process Engineering, vol. 52, 2023.

[13] K. Modular, “Designing Liquid-Liquid Extraction Columns,” 2022.

[14] F. G. L. v. H. J. v. E. D. S. &. B. J. H. (. .. ,. 3. van der Klis, “From batch to continuous: Au-catalysed oxidation
of d-galacturonic acid in a packed bed plug flow reactor under alkaline conditions,” Reaction Chemistry &
Engineering, vol. 3, no. 4, pp. 540-549, 2018.

[15] R. H. L. &. P. C. A. (. Marinho, “Effect of Stirring Speed on Conversion and Time to Particle Stabilization of
Poly (Vinyl Chloride) Produced by Suspension Polymerization Process at the Beginning of Reaction,” .
Brazilian Journal of Chemical, vol. 35, no. 2, pp. 631-640, 2018.

41