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TABLE OF CONTENT

CONTENTS PAGE

Title Page…………………………………………………………………………………………………………………………………... 1

Table of content………………………………………………………………………………………………………………………… 2

Abstract……………………………………………………………………………………………………………………………………… 3

Introduction………………………………………………………………………………………………………………………………… 4

Theory…………………………………………………………………………………………………………………………………………. 5-11

Description of Apparatus……………………………………………………………………………………………………………… 12-13

Procedure……………………………………………………………………………………………………………………………………… 14

Result and Calculation……………………………………………………………………………………………………………………. 15-19

Discussion………………………………………………………………………………………………………………………………………. 20

Conclusion……………………………………………………………………………………………………………………………………… 21

References……………………………………………………………………………………………………………………………………… 22

Appendix………………………………………………………………………………………………………………………………………… 23

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ABSTRACT

This experiment involves a continuous stirred tank reactor (CSTR) in series. The reactor system consists
of an agitated three glass reactor vessel connected in series. The concentration is kept uniform for each
reactor and it is observed from the conductivity reading that there is change in concentration as fluids
move from one reactor to the other reactor. The experiment is conducted to study and thoroughly
investigate the behaviour of continuous stirred tank reactors in series, also the effect on the progress of
chemical reactions carried out in such system.

2 liters of 0.1 M of potassium chloride solution was made and used to fill one of the reagent feed vessels
and the three reactors is filled with water to the standpipe level following the procedure further and
calculation was done and the residence time of each of the three reactors was found to be
1322.1 s for reactor 1 ,1483.75 s for reactor 2∧1280.69 s for reactor 3 with the average residence
time of the reactor system to be 1362.18s.

Conductivity versus time graph was plotted for each reactor and a single graph for the three reactors,
this can be found on the results and calculation page for analysis.

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INTRODUCTION

The design and operation of a chemical reactors are essential criteria to the success of an industrial
operation. A reactor is an operating unit where raw materials undergo a chemical change to form a
desired product. The stirred tank reactor in the form of either a single tank, or more often a series of
tanks, particularly suitable for liquid phases reactions and widely used in chemical industry, i.e.
pharmaceutical for medium and large scale of production. It can form a unit in a continuous process,
yielding consistent product quality, easily to control automatically and low man power requirement.

A continuous flow reactor, the feed is feed continuously to the reactor and discharge from it
continuously. There are three types of continuous flow reactor they are the plug flow reactor, the
dispersed plug flow reactor and completely mixed or continuously stirred tank reactors (CSTRs). The
continuous stirred tank reactor (CSTR), also known as vat- or backmix reactor, mixed flow reactor (MFR),
or a continuous-flow stirred -tank reactor (SFSTR), is common model for a chemical reactor in chemical
engineering and environmental engineering. CSTR consist of a stirred tank that has a feed stream and
discharge stream. Frequently, several CSTRs in series are operating to improve their conversion and
performance.

Complete mixing in a CSTR reactor produce the tracer concentration throughout the reactor to be the
same. Meaning, in an ideal CSTR, at any travel time, the concentration down the reactor is identical to
the composition within the CSTR as mixing degree in CSTR is a crucial factor and it is assumed that the
fluid in the reactor is perfectly mixed that is the contents are uniform to give a high degree yield. But an
ideal mixing in practice, to obtain a sufficient mixing the liquid should not be too viscous. If the mixing is
inadequate, there will be a bulk streaming between the inlet, and the composition of the reactor
contents will not be uniform. If the liquid is too viscous, dispersion will occur and this will affect the
mixing extent.

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THEORY

A chemical reactor is an enclosed volume in which a chemical reaction takes place. In chemical


engineering, it is generally understood to be a process vessel used to carry out a chemical
reaction, which is one of the classic unit operations in chemical process analysis. Chemical engineers
design reactors for optimization and maximize net present value for a given reaction.
The most common basic types of chemical reactors are tanks (where the reactants mix in the whole
volume) and pipes or tubes (for laminar flow reactors and plug flow reactors) Both types can be used as
continuous reactors or batch reactors, and either may accommodate one or more solids (reagents,
catalysts, or inert materials), but the reagents and products are typically fluids (liquids or gases).
Reactors in continuous processes are typically run at steady-state, whereas reactors in batch processes
are necessarily operated in a transient state. When a reactor is brought into operation, either for the
first time or after a shutdown, it is in a transient state, and key process variables change with
time. There are three idealized models used to estimate the most important process variables of
different chemical reactors:

1. Batch reactor model,


2. Continuous stirred-tank reactor model (CSTR), and
3. Plug flow reactor model (PFR).

Many real-world reactors can be modeled as a combination of these basic types

Key process variables include:

1. Residence time (τ, lower case Greek tau)


2. Volume (V)
3. Temperature (T)
4. Pressure (P)
5. Concentrations of chemical species (C1, C2, C3, ... Cn)
6. Heat transfer coefficients (h, U)

Chemical reactions occurring in a reactor may be exothermic, meaning giving off heat, or endothermic,
meaning absorbing heat. A tank reactor may have a cooling or heating jacket or cooling or heating coils
(tubes) wrapped around the outside of its vessel wall to cool down or heat up the contents, while
tubular reactors can be designed like heat exchangers if the reaction is strongly exothermic, or like
furnaces if the reaction is strongly endothermic.

TYPES

Batch reactor
The simplest type of reactor is a batch reactor. Materials are loaded into a batch reactor, and the
reaction proceeds with time. A batch reactor does not reach a steady state, and control of temperature,
pressure and volume are often necessary. Many batch reactors therefore have ports for sensors and
material input and output. Batch reactors are typically used in small scale production and reactions with
biological materials, such as in brewing, pulping, and production of enzymes.

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PFR (plug flow reactor)
In a PFR, sometimes called continuous tubular reactor (CTR), one or more fluid reagents are pumped
through a pipe or tube. The chemical reaction proceeds as the reagents travel through the PFR. In this
type of reactor, the changing reaction rate creates a gradient with respect to distance
traversed; at the inlet to the PFR the rate is plug flow reactor model
very high, but as the concentrations of the reagents decrease and the concentration of the product(s)
increases the reaction rate slows.
Some important aspects of the PFR:
1. The idealized PFR model assumes no axial mixing: any element of fluid traveling through the reactor
doesn't mix with fluid upstream or downstream from it, as implied by the term "plug flow".
2. Reagents may be introduced into the PFR at locations in the reactor other than the inlet. In this way,
a higher efficiency may be obtained, or the size and cost of the PFR may be reduced.
A PFR has a higher theoretical efficiency than a CSTR of the same volume. That is, given the same space-
time (or residence time), a reaction will proceed to a higher percentage completion in a PFR than in a
CSTR. This is not always true for reversible reactions.

CSTR (Continuous Stirred-Tank Reactor)


In a CSTR, one or more fluid reagents are introduced into a tank reactor which is
typically stirred with an impeller to ensure proper mixing of the reagents while the
reactor effluent is removed. Dividing the volume of the tank by the average volumetric flow rate
through the tank gives the space time, or the time required to process one reactor volume of fluid. Using
chemical kinetics, the reaction's expected percent completion can be calculated.

Some important aspects of the CSTR:


1. At steady-state, the mass flow rate in must equal the mass flow rate out, otherwise the tank will
overflow or go empty (transient state).
2. While the reactor is in a transient state the model equation must be derived from the differential
mass and energy balances.
3. The reaction proceeds at the reaction rate associated with the final (output) concentration, since the
concentration is assumed to be homogenous throughout the reactor.
4. Often, it is economically beneficial to operate several CSTRs in series. This allows, for example, the
first CSTR to operate at a higher reagent concentration and therefore a higher reaction rate. In these
cases, the sizes of the reactors may be varied in order to minimize the total capital investment
required to implement the process.
5. It can be demonstrated that an infinite number of infinitely small CSTRs operating in series would be
equivalent to a PFR.

The behavior of a CSTR is often approximated or modeled by that of a Continuous Ideally Stirred-Tank
Reactor (CISTR). All calculations performed with CISTRs assume perfect mixing. If the residence time is 5-
10 times the mixing time, this approximation is considered valid for engineering purposes. The CISTR
model is often used to simplify engineering calculations and can be used to describe research reactors.
In practice it can only be approached, particularly in industrial size reactors in which the mixing time
may be very large.

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Ideal CSTR

Fig1: Diagram showing the setup of a continuous stirred tank reactor

Modeling
A continuous fluid flow containing nonconservative chemical reactant A enters
an ideal CSTR of volume V.

Fig 2: Cross-sectional diagram of a CSTR.

Assumptions:
1. perfect or ideal mixing
dNA
2. steady state, ( =0 ) where NA is the number of moles of species A
dt
3. closed boundaries
4. constant fluid density (valid for most liquids; valid for gases only if there is no net change in the
number of moles or drastic temperature change)
5. nth-order reaction (r = kCAn), where k is the reaction rate constant, CA is the concentration of
species A, and n is the order of the reaction
6. isothermal conditions, or constant temperature (k is constant)
7. single, irreversible reaction (νA = −1)
8. All reactant A is converted to products via chemical reaction
9. NA = CAV

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Integral mass balance on number of moles N A specie A in a reactor of volume V:

1. [Net accumulation of A] = [A in]-[A out]+[net generation of A]


dNA
2. =F Ao - FA + VvArA
dt

Where,
 FAo is the molar flow rate inlet of species A
 FA is the molar flow rate outlet of species A
 vA is the stoichiometric coefficient
 rA is the reaction rate

Applying the assumptions of steady state and νA = −1, Equation 2 simplifies to:
3. 0=FAo – FA –VrA
The molar flow rates of species A can then be rewritten in terms of the concentration of A and the fluid
flow rate (Q):
4. 0=QCAo – QCA – VrA
Equation 4 can then be rearranged to isolate rA and simplified:
Q
5. rA = ¿Ao –CA)
V
1
6. rA = ¿Ao –CA)
τ
where,
Q
 τ is the theoretical residence time (τ = )
V
 CAo is the inlet concentration of species A
 CA is the reactor/outlet concentration of species A

Residence time is the total amount of time a discrete quantity of reagent spends inside the reactor. For
an ideal reactor, the theoretical residence time, is always equal to the reactor volume divided by the
fluid flow rate. Depending on the order of the reaction, the reaction rate, rA, is generally dependent on
the concentration of species A in the reactor and the rate constant. A key assumption when modeling a
CSTR is that any reactant in the fluid is perfectly (i.e. uniformly) mixed in the reactor, implying that the
concentration within the reactor is the same in the outlet stream. The rate constant can be determined
using a known empirical reaction rate that is adjusted for temperature using the Arrhenius temperature
dependence. Generally, as the temperature increases so does the rate at which the reaction occurs.
Equation 6 can be solved by integration after substituting the proper rate expression. The table below
summarizes the outlet concentration of species A for an ideal CSTR. The values of the outlet
concentration and residence time are major design criteria in the design of CSTRs for industrial
applications.

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The Residence Time Distribution Concept

The residence time of a fluid parcel is the total time that the parcel has spent inside a control
volume (e.g.: a chemical reactor, a lake, a human body). The residence time of a set of parcels is
quantified in terms of the frequency distribution of the residence time in the set, which is known
as residence time distribution (RTD), or in terms of its average, known as mean residence time.

Residence time plays an important role in chemistry and especially in environmental


science and pharmacology. Under the name lead time or waiting time it plays a central role respectively
in supply chain management and queuing theory, where the material that flows is usually discrete
instead of continuous.

Simply put, “the time it takes a molecule to pass through a reactor is called its residence time”. For non-
ideal reactors, different elements of fluid entering the reactor would have different lengths of time to
pass through the vessel.

An ideal CSTR
An ideal CSTR will exhibit well-defined flow behavior that can be characterized by the

Exit age distribution E(t) and cumulative age


distribution F(t) functions for an ideal CSTR.

reactor's residence time distribution or exit age distribution. Not all fluid particles will spend the same
amount of time within the reactor. The exit age distribution (E(t)) defines the probability
that a given fluid particle will spend time t in the reactor. Similarly, the cumulative age distribution (F(t))
gives the probability that a given fluid particle has an exit age less than time t. One of the key takeaways
from the exit age distribution is that a very small number of fluid particles will never exit the CSTR.
Depending on the application of the reactor, this may either be an asset or a drawback.

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Non-ideal CSTR

Exit age distribution E(t) and cumulative age


distribution F(t) functions for a CSTR with dead space.

While the ideal CSTR model is useful for predicting the fate of constituents during a chemical or
biological process, CSTRs rarely exhibit ideal behavior in reality. More commonly, the reactor hydraulics
do not behave ideally or the system conditions do not obey the initial assumptions. Perfect mixing is a
theoretical concept that is not achievable in practice. For engineering purposes, however, if the
residence time is 5-10 times the mixing time, the perfect mixing assumption generally holds true.
Non-ideal hydraulic behavior is commonly classified by either dead space or short circuiting.
These phenomena occur when some fluid spends less time in the reactor than the theoretical residence
time. The presence of corners or baffles in a reactor often results in some dead space where the fluid is
poorly mixed. Similarly, a jet of fluid in the reactor can cause short circuiting, in which a portion of the
flow exits the reactor much quicker than the bulk fluid. If dead space or short-circuiting occur in a CSTR,
the relevant chemical or biological reactions may not finish before the fluid exits the reactor. Any
deviation from ideal flow will result in a residence time distribution different from the ideal distribution,
as seen at right.

Stirred Tank Reactors in Series

Stirred tanks in series are, as the name says, continuous stirred tank reactors connected in series. They
enable a higher conversion than a single stirred tank reactor. Stirred tanks in series enable flexible
process control as the temperature and retention time can be set separately for each individual reactor.
This took advantage of surface area in continuous three-stage operation, two pumps of the supply unit
deliver the reactants into the first reactor. A stirrer ensures a homogeneous mixture and thus increases

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the direct contact of the reactants. The product is formed by reaction of the reactants. The mixture of
product and unconverted reactants leaves the reactor through an overflow and is then delivered into
two further identical reactors one after the other. The intermediate delivery occurs via 2 further
peristaltic pumps of the supply unit. After the third reactor the transport occurs in a tank of the supply
unit.
The retention time of the reactants in the reactor is adjusted via the speed of the pumps on the supply
unit.

Fig 3: diagram of a stirred tank in series

Applications

CSTRs facilitate rapid dilution of reagents through mixing. Therefore, for non-zero order reactions, the
low concentration of reagent in the reactor means a CSTR will be less efficient at removing the reagent
compared to a PFR with the same residence time. Therefore, CSTRs are typically larger than PFRs, which
may be a challenge in applications where space is limited. However, one of the added benefits of
dilution in CSTRs is the ability to neutralize shocks to the system. As opposed to PFRs, the performance
of CSTRs is less susceptible to changes in the influent composition, which makes it ideal for a variety of
industrial applications.

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DESCRIPTION OF APPARATUS

Fig 4: Stirred Tank Reactors in Series – CEP-MKII

Fig 4 shows the Armfield CEP-MKII Stirred Tank Reactors in Series Unit is designed to follow the
dynamics of the perfectly mixed multistage process.

Dynamic behaviour can be studied as can multi stage chemical reaction.

Bench mounted and self-contained, the unit requires only to be connected to a single-phase electrical
supply for operation.

Fig 5: Propeller Agitator

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There are three reactor vessels connected in series, each containing a propeller agitator driven by a
variable speed electric motor as show below in fig 5.

Two reagent vessels and two variable speed feed pumps feed reagents into the first reactor in line.

For certain experiments the feed can be connected to the third reactor and a dead time coil, also
positioned on the vacuum formed plinth.

Each reactor and the exit port of the dead time coil are fitted with conductivity probes for monitoring
the process.

Conductivity is displayed on a digital meter on the console through a selector switch.

Fig 6: A stop watch

A stopwatch is a handheld timepiece designed to measure the amount of time that elapses between its
activation and deactivation.

The stop watch was use to take timing for interval of 5mins during the experiment.

2litres of 0.5M of potassium chloride was prepared and used as the tracer.

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PROCEDURE

1. 2 liters of 0.1 M of potassium chloride solution was made and used to fill one of the reagent feed
vessels.
2. The other feed was filled with demineralized water.
3. The water is poured to each of the reactors until they are full to the stand pipe overflow levels. This
saves time.
4. the Stirred Tank Reactors is turned on and the conductivity at reactor 1, 2 and 3 is noted.
5. The water pump is switched on and the conductivity readings is collected for every 5mins for each
reactor at a period of 30mins.

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RESULT AND CALCULATIONS

Time Reactor 1 Reactor 2 Reactor 3 Exit


(min) (mS) (mS) (mS) (mS)
0 0.04 0.09 0.11 0.00
5 1.52 0.19 0.11 0.00
10 0.57 0.13 0.00 0.00
15 4.46 0.18 0.13 0.00
20 5.49 1.82 0.27 0.00
25 6.40 2.57 0.37 0.00
30 7.18 3.33 0.46 0.00
Table 1: Experimental Values for the conductivities of reactors in series

Residence Time of The Three Reactors in Series

The formula for calculating the retention time of a reactor is given as:

∫ tCdt ∑ tᵢCᵢΔtᵢ V
0 ᵢ
ṫ= ∞ = = v (s)
∑ CᵢΔtᵢ
∫ Cdt ᵢ
0

∆ti =Constant

Where:

ṫ= Mean of CPulse curve.

Cᵢ=Output concentration.

Δt =Change in time

V= Volume of the reactor.

ѵ= volumetric flow rate.

∆ti =Constant

V=1.05975L=0.00105975m3

M=0.1M

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Calculation for Reactor 1 mean of CPulse Curve;

tᵢ tᵢ Cᵢ tᵢ Cᵢ
-3
min (S) (*10 ) s (*10-3) s2
0 0 0.04 0
5 300 1.52 456
10 600 0.57 342
15 900 4.46 4014
20 1200 5.49 6588
25 1500 6.40 9600
30 1800 7.18 12924
∑ ¿25.66 ∑ ¿33924
i i
Table 2

From the table the value of residence time can be calculated as thus;

∑ tᵢCᵢ 33924

ṫ= = = 1322.1s
∑ Cᵢ 25.66

0.00105975 m³
ѵ= = 8.016ϵ −7 m³s¯¹
1322.1 s
Thus, the volumetric flow rate for Reactor 1= 8.016ϵ −7 m³s¯¹

8 Conductivity vs Time
7 7.18

6 6.4

5 5.49
𝑪ᵢ (*10-3) s

4 4.46

1.52
1
0.57
0
0.04
0 200 400 600 800 1000 1200 1400 1600 1800 2000
𝑡ᵢ (S)

Graph 1: Reactor 1

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Calculation for Reactor 2 mean of CPulse Curve;

tᵢ tᵢ Cᵢ tᵢ Cᵢ
-3
min (S) (*10 ) s (*10-3) s2
0 0 0.09 0
5 300 0.19 57
10 600 0.13 78
15 900 0.18 162
20 1200 1.82 2184
25 1500 2.57 3855
30 1800 3.33 5994
∑ ¿8.31 ∑ ¿12330
i i
Table 3

From the table the value of residence time can be calculated as thus;

∑ tᵢCᵢ 12330

ṫ= = = 1483.75s
∑ Cᵢ 8.31

0.00105975 m³
ѵ= = 7.142ϵ −7 m³s¯¹
1483.75 s
Thus, the volumetric flow rate for Reactor 2 = 7.142ϵ −7 m³s¯¹

8 Conductivity vs Time
7.18
7
6.4
6
5.49

5
4.46
𝑪ᵢ (*10-3) s

2 1.52

1 0.57
0.04
0
0 200 400 600 800 1000 1200 1400 1600 1800 2000
𝑡ᵢ (S)

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Graph 2: Reactor 2

Calculation for Reactor 3 mean of CPulse Curve;

tᵢ tᵢ Cᵢ tᵢ Cᵢ
-3
min (S) (*10 ) s (*10-3) s2
0 0 0.11 0
5 300 0.11 33
10 600 0.00 0
15 900 0.13 117
20 1200 0.27 324
25 1500 0.37 555
30 1800 0.46 828
∑ ¿1.45 ∑ ¿1857
i i
Table 4

From the table the value of residence time can be calculated as thus;

∑ tᵢCᵢ 1857

ṫ= = = 1280.69s
∑ Cᵢ 1.45

0.00105975 m³
ѵ= = 8.27ϵ −7 m³s¯¹
1280.69 s
Thus, the volumetric flow rate for Reactor 3 = 8.27ϵ −7 m³s¯¹

8 Conductivity vs Time
7.18
7
6.4
6
5.49

5
4.46
𝑪ᵢ (*10-3) s

2 1.52

1 0.57
0.04
0
0 200 400 600 800 1000 1200 1400 1600 1800 2000
𝑡ᵢ (S)

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Graph 3: Reactor 3

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Conductivity vs Time
8

5
𝑪ᵢ (*10-3) s

0
0 200 400 600 800 1000 1200 1400 1600 1800 2000

𝑡ᵢ (S)
Reactor 1 Reactor 2

Graph 4: Reactor 1,2 & 3

Average Residence Time

= (sum of residence time of Reactor 1, Reactor 2 and Reactor 3)/ 3

ṫ 1+ ṫ 2+ṫ 3
=
3
1322.1 s+1483.75 s +1280.69 s
= 3
=1362.18s

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DISCUSSION

The experimental values of conductivity of 0.1M of potassium chloride, and the time of reaction, its that
observed that the conductivity increases with time (5 minutes) for the three reactors. Within space 30
minutes, the conductivity of reactor 1 increases from 0.04mS to 7.18mS but looking clearly there was a
drop-in conductivity from 5minutes to 10minutes which is also observed by the reactor 2 and reactor 3.
the conductivity of reactor 2 increases also from 0.09mS to 3.33mS and reactor 3, 0.11mS to 0.46mS
with and exit/output conductivity of zero mS what this simply means is that from reactor 1 to reactor 3
as the conductivity decreases the reactant to product yield there is an increase in the quality percent
yield. From table 2, the mean residence time of reactor 1 was calculated to be 1322.1s, and with a
volumetric flow rate of 8.016ϵ −7 m³s¯¹. For reactor 2 (table 3) the mean residence time was calculated
to be 1483.755s and a volumetric flow rate of 7.142ϵ −7 m³s¯¹. For reactor 3 (table 4) the mean
residence time was calculated to be 1280.69s and a volumetric flow rate of 8.27ϵ −7 m³s¯¹. From the
results above it can be deduced that with the decrease in conductivity of the system come with a
decrease in the residence time also meaning the percentage yield increases meaning output with a high
quality. Studying the graph 4 carefully, it can be deduced that the mean residence time is inversely
proportional to the flow rate.

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CONCLUSION

From the graphs plotted it can be observed that the step-charge input affected the concentration at the
reactors. If we compare the graphs with theoretic graphs, it is almost the same (due to error
encountered).

It was concluded that actual reactors show non-ideal behavior even if efforts are made to approach
ideality in reactors.

This experiment is feasible in determining the residence time distribution account for non-ideality and
help in calculation for exit conversion.

In conclusion, behaviour of continuous stirred tank reactors in series was thoroughly investigated
including their behaviour its effect on the progress of chemical reactions carried out in such system,
hence the aim of the experiment was a success.

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REFERENCES

1. Smith J M (1981) “Chemical reaction Engineering kinectics” 3 rd edition McGraw Hill Inc., USA
2. LevespieL, O. (1999) “Chemical reaction Engineering” 3 rd edition John Wiley & sons, Inc.
Singapore. Pp 257
3. McCabe W.L Smith J.C and Harriot p (2001) unit operations of chemical engineering 6 th
edition.
4. Armfield Engineering teaching and research Equipment.
5. Coulson Richardson J.F 9(2004); Chemical engineering .

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APPENDIX

The retention time of a reactor is given as:


0

∫ tCᵢdt ∑ tᵢCᵢΔtᵢ V
0 ᵢ
ṫ= 0 = = (s)
∑ CᵢΔtᵢ v
∫ Cdt ᵢ
0

ṫ= residence time

Cᵢ=Conductivity of the reactor

Δt =Change in time

V= Volume of the reactor

V = volumetric flow rate

Volume of a cylinder = πr²h

Where:

π= pie taken as 3.142

r = radius

h = height

v = volumetric flow rate.

V = volume of reactor.

Ci = conductivity of reactor.

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