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# UNIVERSITI TEKNOLOGI MARA MALAYSIA FACULTY OF CHEMICAL ENGINEERING PROCESS ENGINEERING LABORATORY II NAME STUDENT ID EXPERIMENT : AIMULLAH BIN

## RAZAK : 2007269622 : CONTINUOUS STIRRED TANK REACTOR (CSTR)

DATE PERFORMED : 18TH JANUARY 2008 PROG/CODE NO 1 2 3 4 5 6 7 8 9 10 11 12 13 Title Summary Introduction Objectives Theory Procedures Apparatus Results Calculation Discussion Conclusion Recommendation References Appendices TOTAL : Bachelor of Engineering (Hons.) in Process Engineering/EH221 Allocated Marks % 5 5 5 5 3 5 20 10 20 10 5 5 2 100 Marks %

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## Cik Radziah TABLE OF CONTENT

CONTENTS SUMMARY INTRODUCTION OBJECTIVES THEORY PROCEDURES APPARATUS RESULTS CALCULATIONS DISCUSSIONS CONCLUSIONS RECOMMENDATIONS REFERENCES APPENDICES

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SUMMARY In chemical engineering, chemical reactors are vessels designed to contain chemical reactions. The reactor is the equipment in which empirical information is obtained can be divided into two types, the batch and flow reactors. The batch reactor is simply a container to hold the contents while they react. The flow reactor is used primarily in the study of the kinetics of heterogeneous reactions. In this case of study, the continuous stirred tank reactor is carried out in order to determine the order of the saponification reaction and also to determine the reaction rate constant, k. According to the theory, the saponification process can be categorized as the second order reaction. A plot of the experimental data should be a straight line in which its slope is the rate constant of the reaction. The deviation of graph is due to the lateness addition of sample into HCl that will quench the reaction between sodium hydroxide and ethyl acetate. The deviation of graph between minute 0 to minute 1 is also due to the titration process in which the pink color that needs to obtain is not as light as needed. Also, the error when taking the buret readings can be lead to the deviation when plotting both the graph of ln CA versus time and ln CB/CA versus time.. The objectives of study are not successfully achieved.

INTRODUCTION Every industrial chemical process is designed to produce economically a desired product from a variety of starting materials through a succession of treatment steps. The raw materials undergo a number of physical treatment steps to put them in the form in which they can be reacted chemically. They then pass through the reactor. The products of the reaction must then undergo further physical treatment like separations, purification, etc for the final desired product to be obtained. In chemical engineering, chemical reactors are vessels designed to contain chemical reactions. The design of a chemical reactor deals with multiple aspects of chemical engineering. Chemical engineers design reactors to maximize the net present value for the given reaction. Designers ensure that the reaction proceeds with the highest efficiency towards the desired output product, producing the highest yield of product while requiring the least amount of money to purchase and operate. Reactor design uses information, knowledge and experience from a variety of areas such as thermodynamics, chemical kinetics, fluid mechanics, heat transfer, mass transfer and economics. Chemical reaction engineering is the synthesis of all these factors with the aim of properly designing a chemical reactor. The reactor is the equipment in which empirical information is obtained can be divided into two types, the batch and flow reactors. The batch reactor is simply a container to hold the contents while they react. The flow reactor is used primarily in the study of the kinetics of heterogeneous reactions. OBJECTIVES The purposes of this Continuous Stirred Tank Reactor experiment are: To determine the order of saponification reaction To determine the reaction rate constant, k by plotting the graph

THEORY The continuous stirred-tank reactor (CSTR), also known as vat- or backmix reactor is a common ideal reactor type in chemical engineering. A CSTR often refers to a model is used to estimate the key unit operation variables when using a continuous agitated-tank reactor to reach a specified output. A stirred tank reactor (STR) may be operated either as a batch reactor or as a steady-state flow reactor (better known as Continuous Stirred tank Reactor {CSTR}). The key or main feature of this reactor is that mixing is complete so that properties such as temperature and concentration of the reaction mixture are uniform in all parts of the vessels. Material balance of a general chemical reaction is described below: The conservation principle requires that the mass of species A in an element of reactor volume V obeys the following statement: [ Rate of A into ] [ Rate of A out of ] + [ Rate of A produced ] = [ Rate of A ] volume element volume element within volume element accumulated within volume element

Batch Stirred Tank Reactor (BSTR) In batch reactions, there are no feed of exits streams and therefore the general equation can be simplified into: [Rate of A produced in volume element] [Rate of A accumulated in volume element] The rate of reaction of component A is defined as: -rA = 1 V dNA dt = [moles of A appear by reaction] / [unit volume] [unit time]
by reaction

By this definition, if A is a reaction product, the rate is positive; whereas if it is a reactant which is consumed, the rate is negative. (- rA) V = NAO dXA dt t = NAO dXA (-rA)V

Steady State Mixed Flow Reactor The general material balance for this reactor is: Input of A (moles/time) = FAO (1-XAO) = FAO Output of A (moles/time) = FA = FAO ((1-XA) Dissapearance of A by reaction (moles/time) = (-rA) V FAO XA = (-rA ) V V = = XA = XA FAO CAO -rA -rA

= 1 = V = VCAO = CAO XA
S Vo FAO -rA

PROCEDURE Experiment: Batch Reactor Experiment Reactant Preparation Procedure 1. 0.05 M NaOH and 0.05 M Ethyl Acetate solutions is prepared in two separate 20 liter feed tanks. 2. The concentration of 0.1 M NaOH solution is to be confirmed by titrating a small amount of it with 0.1 M HCl using phenolphthalein as indicator. The concentration of ethyl acetate solution is evaluated by the following manner. First, 0.1 M NaOH solution is added to a sample of the feed solution such that the 0.1 M NaOH solution is in excess to ensure all of the ethyl acetate has reacted. This mixture is let to be reacting overnight. On the following day, the amount of unreacted NaOH is determined by direct titration with standard 0.1 M HCl. The ethyl acetate real concentration is then recorded. 3. 1 liter of quenching solution of 0.25 M HCl and 1 liter of 0.1 M NaOH is prepared for back titration. Batch Reaction Procedure 1. The overflow tube in the reactor is adjusted to give a desired working volume (2.5L). The pump P1 is switched on and 1.25L of the 0.1M ethyl acetate is pumped from the feed tank into the reactor. The pump P1 is stopped. 2. The pump P2 is switched on and 1.25L of the 0.05 M NaOH is pumped into the reactor. The pump P2 is stopped when 2.5L volume is reached. The stirrer is switched on and the speed is set to be 180 rpm. Immediately, the timing of the reaction is recorded. 3. 10mL of 0.25 M HCl is quickly measured in a flask 4. After 1 minute of reaction, the valve V7 is opened. 50mL sample is then collected and added immediately to the 10mL of 0.25 M HCl prepared in step 3 and let to be mixed. The HCl will quench the reaction between ethyl acetate and sodium hydroxide. 5. The mixture is then titrated with 0.1 M NaOH to evaluate the amount of unreacted HCl. 6. Steps 3 to 5 is repeated for reaction times 5,10,15,20 and 25 minutes

## APPARATUS Chemicals HCL, NaOH, Ethyl Acetate and phenolphthalein.

Equipment Description: (a) Reactor The reactor consists of a glass vessel with top and bottom plate made of stainless steel. The reactor comes with a coiling coil, a 1.0kW heater, a temperature sensor, stirrer system, an overflow tube and a gas sparging unit. (b) Feed Inlet System (Liquid Reactions) For each liquid reactant, a 20 L feed tank, a pump, a needle valve and a flow meter are provided. Each reactant is pumped from the feed tank to the appropriate inlet port at the top plate (c) Gas Inlet System (Gas-Liquid Reactions:Optional) Gas from gas cylinder flows through a needle valve, a flow meter and a gas sparger before reacting with the liquid inside the reactor. (d) Product/Waste Tank A 50L rectangular tank made of stainless steel is provided for collecting the product or waste before being discharged. (e) Control Panel The control panel consists of all the necessary electrical components for controlling the operations of the unit. Components mounted on the panel door are all labeled for convenience. The control panel also houses the necessary modules for data acquisition system (f) Data Acquisition System (Optional) The Data Acquisition System consists of a personal computer, ADC modules and instrumentations for measuring the process parameters. A flow meter with 0 to 5 VDC output signal is supplied for each feed stream. A temperature sensor and temperature

transmitter with 4 to 20 mA output signal is provided to measure the reaction temperature. A pH sensor with controller are provided for monitoring the changes in pH while the reaction is taking place. All analog signals from the sensors are converted by the ADC modules into digital signal before being sent to the personal computer for display and manipulation.

## Figure 1: Continuous Stirred Tank Reactor Equipment

RESULTS Feed Concentration Standard Solution Concentration of NaOH (CNaOH) = 0.05 mol/L Concentration of ethyl acetate (CEA) = 0.1 mol/L Concentration of HCl (CHCl,std) = 0.25 mol/L Volume of HCl (VHCl) = 10 mL = 0.01 L Sample
Time (min)
Volume of titrating NaOH (mL) Volume of quenching HCl unreacter with NaOH in Sample (mL) Volume of HCl Reacted with NaOH in Sample (mL) Mole of HCl Reacted with NaOH in Sample (mol) (x10-4) Mole of NaOH unreacted in Sample (mol) (x10-4) Concentration of NaOH unreacted with Ethyl Acetate (mol/L) (X10-2) Steady State Fraction Conversion of NaOH Concentration of NaOH reacted with Ethyl Acetate (mol/L) (X10 ) Mole of NaOH reacted with Ethyl Acetate in Sample(mol) (X10-3) Concentration of Ethyl Acetate reacted with NaOH (mol/L) (X10 ) Concentration of Ethyl Acetate unreacted (mol/L) (X10-2)
-2 -2

## Concentration of NaOH (CNaOH) = 0.1 mol/L Volume of Sample (VS) = 50 mL = 0.05 L

1 13.4 5.36 4.64 11.6 11.6 2.32 0.53 6 2.68 1.34 2.68 7.32 5 9.4 3.76 6.24 15.6 15.6 3.12 0.37 6 1.88 0.94 1.88 8.12 10 7.3 2.92 7.08 17.7 17.7 3.54 0.29 2 1.46 0.73 1.46 8.54 15 6.7 2.68 7.32 18.3 18.3 3.66 0.26 8 1.34 0.67 1.34 8.66 20 3.7 1.48 8.52 21.3 21.3 4.26 0.14 8 0.74 0.37 0.74 9.26 25 2.5 1.00 9.00 22.5 22.5 4.50 0.10 0.50 0.25 0.50 9.50

SAMPLE OF CALCULATIONS (A) Sample: t = 1 min (B) Volume of titrating NaOH (mL) = 13.4 mL = 0.0134L

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(C) Volume of quenching HCl Unreacted = C NaOH,std x (B) with NaOH in Sample (mL) C HCl, std = 0.1 mol / L x 13.4 mL 0.25 mol/L = 5.36 mL (D) Volume of HCl Reacted with NaOH = VHCl (C) in sample (mL) = 10 mL 5.36 mL = 4.64 mL = 0.00464L (E) Mole of HCl Reacted with NaOH in = C HCl, std x (D) sample (mol) = 0.25 mol/L x 0.00464 L = 11.6 x 10-4 mol (F) Mole of NaOH unreacted in Sample = (E) (mol) = 11.6 x 10-4 mol (G) Concentration of NaOH unreacted = (E) with Ethyl Acetate (mol/L) VS = 11.6 x 10-4 mol 0.05 L = 0.0232 mol/L (H) Steady State Fraction Conversion = 1 CA of NaOH (XA) CAO = 1 - 0.0232 mol/L 0.05 mol/L = 0.536 (I) Concentration of NaOH reacted = CNaOH,O (G) with Ethyl Acetate (mol/L) = 0.05 mol/L - 0.0232 mol/L = 0.0268 mol/L (J) Mole of NaOH reacted with = (I) x VS Ethyl Acetate in Sample(mol) = 0.0268 mol/L x 0.05 L = 1.34 x 10-3 mol (K) Concentration of Ethyl Acetate = (J)

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## Vs = 1.34 x 10-3 mol 0.05 L = 0.0268 mol/L

(L) Concentration of Ethyl Acetate = CEA,O (K) unreacted (mol/L) = 0.1 mol/L 0.0268 mol/L = 0.0732 mol/L

DISCUSSION The continuous stirred tank reactor study is carried out experimentally in order to determine the order of saponification reaction and also to determine the reaction rate constant, k. The saponification process is the hydrolysis of an ester under basic

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conditions to form an alcohol and the salt of a carboxylic acid .For example in this case of study, CH3COOC2H5 + NaOH CH3COONa + C2H5OH From the theory, the saponification process is known to be the first order reaction in which, when the graph of ln CA versus time (min) is plotted, it will shows the straight line which the slope is in negative value and is equal to the rate constant of the process. The experimental data is summarized as below: Time (min) CA ln CA 1 0.0232 -3.764 5 0.0312 -3.467 10 0.0354 -3.341 15 0.0366 -3.308 20 0.0426 -3.156 25 0.0450 -3.101

## Figure 2: Graph ln CA versus time (min) (based on experimental data)

From Figure 2 above, the slope of the graph in which is known as the rate constant of the process can be calculated as below: k = -3.308 (-3.764) 15-1 k = 0.0326 min-1

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The graph above shows the straight line but the rate constant was in a positive value. According to the theory, the graph for the first order of saponification process needs to be a straight line and positive value of slope which is the rate constant of the reaction. Therefore, the graph above is altered so that the reaction between minute 0 to minute 1 is not taken as consideration because of the minor error. The theory also state that the saponification process is known to be the second order reaction in which, when the graph of ln CB/CA versus time (min) is plotted, it will shows the straight line which the slope is in positive value and is equal to the rate constant of the process. The experimental data is summarized as below: Time (min) CA CB ln CB/CA 1 0.0232 0.0732 1.149 5 0.0312 0.0812 0.956 10 0.0354 0.0854 0.881 15 0.0366 0.0866 0.861 20 0.0426 0.0926 0.776 25 0.0450 0.0950 0.747

Figure 2: Graph ln CB/CA versus time (min) (based on experimental data) From Figure 3 above, the slope of the graph in which is known as the rate constant of the process can be calculated as below: (0.1 - 0.05)k = 0.776 0.956 14

20-5 k = -0.24 min-1 The graph above shows the straight line but the rate constant was in a negative value. According to the theory, the graph for the second order of saponification process needs to be a straight line and negative value of slope which is the rate constant of the reaction. Therefore, the graph above is altered so that the reaction between minute 0 to minute 1 is not taken as consideration because of the minor error. Also the result that we get does not satisfy the theory due to human error during the experiment was conducted.

CONCLUSION The continuous stirred tank reactor (CSTR) study is carried out experimentally using the continuous stirred tank reactor equipment. The first objective of this study is to determine the order of saponification reaction. The second objective is to determine the rate constant of the reaction which can be calculated from both the slope of the graph of ln CA versus time (min) and ln CB/CA versus time (min). Based on the result that we obtain, the order of saponification reaction cannot be determined. Further more; the rate of reaction that we calculate in the discussion part cannot be used due to the error in collecting data from the experiment. The deviation of graph in Figure 2 and Figure 3 is due to the lateness addition of sample into HCl that will quench the reaction between sodium hydroxide and ethyl acetate. The deviation of graph between minute 0 to minute 1 is due to the titration process in which the pink color that needs to obtain is not as light as needed.

## RECOMMENDATION Here are some recommendations regarding to this study:

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The eyes should be meniscus to get the accurate readings in order to avoid parallax error. The titration process should be done slowly in order to get the first point in which the light pink of sample is obtained. The sample must be quickly added into HCl to avoid any experimental error due to the lateness addition of HCl. Glove and goggle should be wearing when dealing with the chemicals such as hydrochloric acid, sodium hydroxide etc. When taking the buret readings, white paper should be used in order to reduce parallax error.

REFERENCES 1. Schmidt, Lanny D. (1998). The Engineering of Chemical Reactions. New York: Oxford University Press. 2. Kenneth A. Connors Chemical Kinetics, the study of reaction rates in solution, 1991, VCH Publishers. 3. http://www.chem.arizona.edu/~salzmanr/480a/480ants/chemkine.html. 4. Isaacs, N.S., "Physical Organic Chemistry, 2nd edition, Section 2.8.3, Adison Wesley Longman, Harlow UK, 1995.

APPENDICES

A batch stirred tank reactor is the simplest type of reactor. It is composed of a reactor and a mixer such as a stirrer, a turbine wing or a propeller. The batch stirred tank reactor 16

is illustrated below:

This reactor is useful for substrate solutions of high viscosity and for immobilized enzymes with relatively low activity. However, a problem that arises is that an immobilized enzyme tends to decompose upon physical stirring. The batch system is generally suitable for the production of rather small amounts of chemicals. A continuous stirred tank reactor is shown below:

The continuous stirred tank reactor is more efficient than a batch stirred tank reactor but the equipment is slightly more complicated

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## Type of Reactor Continuously Stirred Tank Reactor (CSTR)

Characteristics Run at steady state with continuous flow of reactants and products; the feed assumes a uniform composition throughout the reactor, exit stream has the same composition as in the tank

## Kinds of Phases Present 1. Liquid phase 2. Gas-liquid rxns 3. Solid-liquid rxns

Usage 1. When agitation is required 2. Series configurations for different concentration streams

Advantages 1. Continuous operation 2. Good temperature control 3. Easily adapts to two phase runs 4. Good control 5. Simplicity of construction 6 Low operating (labor) cost 7. Easy to clean

Disadvantages 1. Lowest conversion per unit volume 2. By-passing and channeling possible with poor agitation

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## General Mole Balance Equation

Assumptions 1) Steady state therefore 2) Well mixed therefore rA is the same throughout the reactor

## Rearranging the generation

In terms of conversion

Reactor Sizing Given rA as a function of conversion, rA = f(X), one can size any type of reactor. The volume of a CSTR can be represented as the shaded areas in the Levenspiel Plot shown below:

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Reactors in Series Given rA as a function of conversion, , rA = f(X), one can also design any sequence of reactors in series provided there are no side streams by defining the overall conversion at any point.

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## Mole Balance on Reactor 2

Given rA = f(X) the Levenspiel Plot can be used to find the reactor volume

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