Batch Distillation of Water-Methanol System

Batch distillation of methanol-water system and modeling
and simulation of distillation column using ARTIFICIAL

NEURAL NETWORK and ChemCAD
Satadru Chakrabarty, Sayantan Roy Choudhury, Tapas Saha

DEPARTMENT OF CHEMICAL ENGINEERING
NATIONAL INSTITUTE OF TECHNOLOGY

AGARTALA-799055, INDIA
MAY - 2013
BATCH DISTILLATION OF METHANOL-WATER SYSTEM

AND MODELING AND SIMULATION OF DISTILLATION
COLUMN USING ARTIFICIAL NEURAL NETWORK AND
CHEMCAD
Report submitted to
National Institute of Technology, Agartala
For the award of the degree
Of
Bachelor of Technology
By
Satadru Chakrabarty (09UCH013)
Sayantan Roy Choudhury (09UCH014)
Tapas Saha (09UCH016)
Supervisor
Mr. Bibhab Kumar Lodh
Assistant Proffessor Chemical Engg Department
Chemical Engineering Department

National Institute of Technology, Agartala
May- 2013
2013 Satadru Chakrabarty, Sayantan Roy Choudhury, Tapas Saha. All rights reserved
ii
Dedicated:
To all the teachers of the department

of chemical engineering, who have
inspired us to make this project
successfully
iii
APPROVAL SHEET
This thesis/dissertation/report entitled Batch distillation of methanol-water system and

modeling and simulation of distillation column using ARTIFICIAL NEURAL
NETWORK and ChemCAD by Sayantan Roy Choudhury, Satadru Chakrabarty and
Tapas Saha is approved for the degree of ____________ (Degree details).
Examiners
________________________
________________________
________________________
________________________
________________________
________________________
________________________
________________________
________________________
Supervisor (s)
________________________
Chairman
________________________
Date: ____________
Place: ____________
iv
DECLARATION
We declare that this written submission represents my ideas in my own words and where
others' ideas or words have been included, I have adequately cited and referenced the original
sources. We also declare that we have adhered to all principles of academic honesty and
integrity and have not misrepresented or fabricated or falsified any idea/data/fact/source in
our submission. We understand that any violation of the above will be cause for disciplinary
action by the Institute and can also evoke penal action from the sources which have thus not
been properly cited or from whom proper permission has not been taken when needed.
_________________________________
(Signature)
________________________________
(Name of the student)
_________________________________
(Roll No.)
Date: __________
CERTIFICATE
This is certified that the work contained in the project titled Batch distillation of methanolwater system and modeling and simulation of distillation column using ARTIFICIAL
NEURAL NETWORK and ChemCAD, by Satadru Chakrabarty, Sayantan Roy
Choudhury, Tapas Saha has been carried out under my/our supervision and that this work
has not been submitted elsewhere for a degree
Signature of Supervisor(s)
Name(s)
Department(s)
N.I.T. Agartala
May, 2013
vi
PREFACE
Technology is any technique, instrument or device that makes human life on this planet
easier. This gives us immense pleasure to be working on a project that deals with a very
important phenomena or unit operation of the industry. This project Batch distillation of
methanol-water system and simulation of working of distillation column using
ARTIFICIAL NEURAL NETWORK and ChemCAD is a humble step in trying to
understand and design a fully operational batch distillation column, with the help of software.
The mixture chosen for the simulation is basically methanol- water mixture, which is a
very common mixture found in industries and is usually separated by a distillation column.
In this project there would be wide scale use of Artificial Neural Network (ANN), basically
for the purpose of data prediction and data validation.
Finally the simulation and design of the distillation column would be completed using
ChemCAD, with the data acquired from the initial experiments and data prediction from
ANN.
Hope this humble effort would manage to earn the appreciation of all the readers.
Satadru Chakrabarty
Sayantan Roy Choudhury
Tapas Saha
vii
ACKNOWLEDGEMENT
We would like to express my sincerest gratitude to our Director Prof. Dr. P.K.Bose, who has
been kind enough to provide us with the infrastructural facilities that we have in our labs.
Then we would like to give our sincere regards to Mrs. Soma Nag (H.O.D, Dept. of
Chemical Engg.), without whose help and support this project would not have been possible.
Next we would like to give regards to our project guide Mr. Bibhab Kumar Lodh
(Asst. professor, dept. of chemical engg.) who has been so patient with us, and always giving
his advice for the betterment of the project and correcting our errors whenever necessary.
We are also grateful to all the teachers of the dept. of chemical engg. for their
valuable advice and insights. We are also grateful to each and every person who has helped
us in the project with their valuable supports and advices.
viii
LIST OF FIGURES:
Fig. 1.1: basic layout of a distillation column
Fig. 1.2.1: a typical packed distillation column
Fig. 1.2.2 :The basic distillation column
Fig. 1.3.1: Typical Process flow diagram in ChemCAD
11
Fig. 1.4.1: the data is entered in this sheet
13
Fig. 1.4.2: the neural network between the inputs and outputs
14
Fig. 1.4.3: the error graph showing the range of errors in the A.N.N prediction
15
Fig. 3.1.1:schematic representation of the multicomponent Batch

Distillation Process
22
Fig. 4.3.1: the calibration curve attained from the calibration data at 28C
30
Fig 4.4.1 : the laboratory packed bed distillation column
31
Fig. 5.4.1: flowsheet of batch distillation as displayed by ChemCAD
37
Fig. 5.5.1(a) : distillation column specification (general model)
39
Fig. 5.5.1(b): distillation column specification (heat and material balance)
40
Fig. 6.1: this figure shows the softwares data entry sheet
43
Fig. 6.2: the internal network of ANN, correlating the output and
input parameters
44
Fig 6.3: the importance given to the different inputs
Fig. 6.3: the error graph, showing the target error, maximum,
45
minimum and average error values
45
Fig 7.1: T-x-y graph of MeOH-H2O system
59
Fig 7.2: x-y graph
60
Fig 7.3: liquid heat capacity curve
61
Fig 7.4: : liquid heat capacity curve
63
ix
Fig 7.5: Temperature vs. vapour thermal conductivity graphs
64
Fig 7.6: Temperature vs. liquid thermal conductivity graphs
65
Fig 7.7: composite curve
71
LIST OF TABLES
Table 1.1: CRC 44th ed. lists azeotropes for acetic acid/water and
acetone/water,
Table 4.3.1: calibration curve data for different mole fraction.
29
Table 4.5.1: daily experiment log
33
Table 6.1: A.N.N prediction result
46
Table 7.1: experiment vs. ChemCAD
47
Table 7.2: experiment vs. ANN
72
Table 7.3: experiment vs. ANN vs. ChemCAD
73
LIST OF SYMBOLS AND ABBREVIATIONS
MB =liquid holdup in still pot (kmol)

MD =liquid holdup in reflux drum (kmol)
Mn =liquid holdup in the nth tray (kmol)
nT =total number of trays
QR =Heat input to the still pot (kJ/min)
R=Reflux flow rate (kmol/min)
RS =steady state value of R, (kmol/min)
VB =vapor boil-up rate (kmol/min)
Vn=vapor flow rate of vapor leaving nth tray (kmol/min)
VnT =vapor flow rate of vapor leaving top tray (kmol/min)
D=distillate flow rate (kmol/min)
Ln=liquid flow rate of liquid leaving the nth tray (kmol/min)
xB,i=composition of component i in the still
xD,i=composition of component i in the Distillate
xn,i=composition of component i in Liquid stream leaving the nth tray
r,i=rate of reaction of component (kmol/lit.min)
=volume of catalyst (lit)
k1, k2 =rate constants
K1, K2= GMC controller tuning parameters
vb =volume of reboiler (lit)
vd=volume of reflux drum (lit)
v=volume of tray (lit)
RF=multiplication factor (RF=1 for reactive section, RF=0 for non-reactive section)
Him=stoichiometric coefficient of i the component of m the reaction.
1, 2, 3=estimator tuning parameters.
Radii=rate of reaction of component i in distillate.
Rabbi= rate of reaction of component i in bottom.
Roni = rate of reaction of component i in nth tray.
xi
ABSTRACT
This project Batch distillation of methanol-water system and simulation of working of
distillation column using ARTIFICIAL NEURAL NETWORK and ChemCAD , is an
intensive study to check the chances, whether ARTIFICIAL NEURAL NETWORK can be
used in the prediction of distillation column output.
This is a relatively different field, for which A.N,N could be used. So this project tries to
answer this question by experimental analysis carried out on a packed bed distillation
column.
Hope that this project is fruitful and further work is done in the future on this topic.
xii
CONTENTS
Title Page
Dedication
ii
Certificate of Approval
iii
Declaration
iv
Certificate
Preface
vi
Acknowledgements
vii
List of Figures
viii
List of Tables
ix
List of Symbols and Abbreviations
Abstract
xi
Contents
xii
Chapter 1 Introduction
1.1 Methanol Water system
1.2 Distillation
1.3 ChemCAD
10
1.4 A.N.N
13
Chapter 2 Literature Review
17
2.1 Batch Distillation
17
2.2 A.N.N
18
2.3 ChemCAD
19
Chapter 3 Modelling of the distillation column
21
3.1 Process Description
21
3.2 Modeling Equations
23
Chapter 4 Experimental distillation of MeOH- H2O system
27
4.1 Introduction
27
4.2 Theory
28
4.3 Calibration Curve
29
xiii
4.4 Description of Apparatus
31
4.5 Experimental Observation
33
Chapter 5 ChemCAD simulation
34
5.1 Overview of the Batch Distillation Process
34
5.2 Creating a New Simulation
35
5.3 Drawing the Flowsheet
35
5.4 Selecting Engineering Units
35
5.5 Selecting Components
37
5.6 Run the simulation.
39
5.7 Review the results and print as needed
40
Chapter 6 Artificial Neural Network
43
6.1 Data entry and training
43
6.2 Data prediction and further learning
44
6.3 Error analysis
45
6.4 Procedure
46
6.5 Prediction results
46
Chapter 7 Results and Discussions
47
7.1 Comparison between experimental result and ChemCAD results 47

7.2 ChemCAD generated results
48
7.3 Comparison between experimental result and A.N.N results
70
Chapter 8 Conclusions and Future Scope of Study
73
Chapter 9 References
75
APPENDIX
77
xiv
LITERATURE REVIEW
CHAPTER 2
LITERATURE REVIEW
2.1 Batch distillation
Batch Distillation is a separation process based on relative volatilities of the components in the
system to be separated. A multi-component batch distillation model deals with a system having
more than two components, but this does not preclude it being used for a binary system. Batch
distillation is actually a semi batch process where the system is charged once in one cycle time
by a fresh feed at the beginning of a batch, while the products can be continually withdrawn
from the system and other fresh feed or slop recycles can be introduced to the system during
the cycle time. The essential temporal features of the cycle time are the charging period, the
start-up period, the topping and feeding period.
Due to its flexibility, simple operation, and low capital costs, batch distillation has established
itself as a standard unit operation for the separation of small amounts of liquid mixtures. This
unit operation has therefore been extensively studied.
Minimum energy demand
Distillation is an energy-intensive separation process, since heat has to be supplied to the
system in order to create the second phase required for separation. Both during the design and
operation phases, the energy required by the process plays a fundamental role. The minimum
energy required for a given separation task is that needed by a distillation column having an
infinite number of stages. This is therefore a theoretical minimum, which can be used during
the design phase as a pre-selection tool to restrict the choice among the available batch
distillation processes.
17
LITERATURE REVIEW
On the other hand, during operation, the minimum energy demand can be used as a measure
of how far the process is from its thermodynamics optimal, and how wide the optimization
margins of the process are. The most popular method for the calculation of the minimum
energy demand is the one published by Underwood [1948]. This is an iterative method, which,
under the assumption of constant molar overflow, allows the calculation of the minimum reflux
ratio for ideal mixtures. Offers et al. [1995] describe a direct method to calculate the minimum
reflux ratio for a given separation both for ideal and real systems. This method is applicable to
multi-component batch distillation operated with constant product composition. The
calculation of the minimum reflux and reboil ratios is repeated for every concentration in the
still. The stills concentration can be determined via Rayleighs equation, as described in
Stichlmair and Fair [1998]. This calculation requires only the knowledge of the relative
volatilities of the mixture in the still.
Modeling and simulating distillation columns is not a new enterprise. All of the models
described in literature either contain algebraic loops or simplifying assumptions that render the
model ill-equipped for dynamic simulations. The structure and the equations that represent a
tray distillation column are explored using bond graphs. Bond graphs model the power flow in
a system, an inherently instructive way to view complex systems. Results of this study by
Braden Alan Brooks[1993] reveal several ways of eliminating the algebraic loops and
producing a dynamic model. The bond graph model can be expanded by introducing other
elements including chemical reactions and thermal interaction with other columns.
The design for a new packed distillation column for consideration as a new experiment for the
University
Of
Florida
Department
Of
Chemical
Engineering
Unit
Operations
Laboratory[2011] was created to demonstrate the separation of water and isopropanol (i-Pr)
and to evaluate a parallel applied multi-correlation approach to creating a high accuracy
process model based on correlations with known margins of error.
Only few rigorous models for distillation columns start-up are available in literature and
generally required a lot of parameters related to tray or pack geometry. On an industrial
viewpoint, such a complexity penalizes the achievement of a fast and reliable estimate of startup periods. In S. Elguea, L. Prata, M. Cabassuda,, J.M. Le Lanna, J. Cezeracb, two simple
mathematical models are proposed for the simulation of the dynamic behavior during start-up
18
LITERATURE REVIEW
operations from an empty cold state. These mathematical models are based on a rigorous trayby-tray description of the column described by conservation laws, liquidvapour equilibrium
relationships and equations representative of hydrodynamics.
2.2 Artificial Neural Network

Because the pattern of the relationships between the independent (input) factors and the
dependent (output) factor in our model will be learned from the data by the Artificial Neural
Network (ANN) algorithm, the selection of input to the neural networks is an important
decision. It is crucial to select factors that fully capture the domain of feed and product relation
in the distillation process. In this session we focuses on a literature review of the factors to
provide an understanding of how they affect the successful data prediction from limited known
factors. Also, as our resources to study the effectiveness of A.N.N in distillation process is
somewhat limited; therefore, instead of adopting a micro approach to understand the specific
effects of a few factors, we use a macro approach that examines a broad variety of factors in
an effort to capture the complexities of the process. This macro approach is warranted because
we are trying to subsume the intricacies of the process into our model to improve the accuracy
of its predictions (Calantone, di Benedetto, and Bojanic 1988) [6]. Furthermore, all the
measures were IJCSI International Journal of Computer Science Issues, Vol. 9, Issue 2, No 2,
March 2012 ISSN (Online): 1694-0814 www.IJCSI.org 114
Copyright (c) 2012 International Journal of Computer Science Issues. All Rights Reserved.
Well-validated and accepted measures in the new product literature (see Song and Parry 1997
[7]). In choosing the input for our models, we rely on the resource-based theory of the firm
(Wernerfelt 1984, Barney 1991; Conner 1991) [8]-[10]. Resource-based theory provides a
unique insight into the situation that faces managers who make project selection and resource
allocation decisions. This theory is relatively new in relation to industrial organization theory.
Traditional industrial organization theory posits that a firm's strategy and ultimately its ability
to create and sustain a competitive advantage are dependent on environmental factors.
Resource-based theory takes a different position by viewing firm resources as heterogeneous
and immobile. Thus, each firm has a limited, heterogeneous endowment of resources, and its
task is to combine the endowment to form capabilities which are the basis for creating a unique,
valuable market offering that is not easily imitated or substituted. The central tenant of
19
LITERATURE REVIEW
resource-based theory is that this offering is the mechanism for creating a sustainable
competitive advantage for the firm. A review of literature in the study of factors influence the
successful product innovation has shown numerous factors which can be grouped into three
main factors: (1) the firms innovation capability, (2) the firms new product development
capability, (3) the external competitive environment.
2.3 ChemCAD
The software CHEMCAD 6.1.3 is a very important tool for this study of packed bed
distillation column and its simulation based on laboratory experiments. The main parts of this
software include the setting up of the units, thermodynamic parameters, setting up of the
process flowsheet. The problems and techniques of ChemCAD have been used from the Help
menu of the software.
More detailed information about the software has been got from the website
http://www.chemstations.com/
More information about the working of ChemCAD is available at,

http://www.chemstations.com/Why_ChemCAD/
Detailed demos of the software are available at http://www.chemstations.com/.
20
MODELLING OF THE DISTILLATION COLUMN
CHAPTER 3

3.1.
Process Description
In batch distillation, a liquid mixture is charged into a vessel and heat is added to produce
vapor that is fed into a rectifying column. The liquid mixture can be a fresh feed and also with
any recycled slop cuts. During the initial startup period, the column operates under total reflux
condition in which vapor from the top of the column is condensed and returned to the column.
The operation of batch distillation described here corresponds to a ternary system. During the
column operation under total reflux condition, the concentration of the lightest component
buildup on the upper trays in the column and the concentrations of the intermediate component
and heaviest component decreases in the top of the column but increases in the still pot. When
the concentration of the lightest component in the distillate reaches its specified purity level,
then the distillate product withdrawal is begun. During the withdrawal of the first product,
there is a composition front located in the lower part of the column that separates the lightest
and intermediate components. This front moves up the column as light product is removed.
When this front nears the top of the column, the distillate stream is diverted to another tank as
the 1rst slop cut. When the concentration of the intermediate component in the distillate reaches
its speci1ed purity level, the distillate is diverted to another tank in which second product is
21
collected. When the purity of the material in this tank drops to the speci1ed purity level, the
distillate stream is diverted into another tank, and the second slop cut is collected until the
average composition of the material remaining in the still pot and on the trays in the column
meets the purity speci1cation of the heavy product.
In order to represent realistic operation of actual batch distillation column, a rigorous nonlinear
model that considers simultaneous effect of heat and mass transfer operations and fluid flow
on the plates is needed. Such batch distillation model is derived from first principles involving
dynamic material and component, and algebraic energy equations supported by vaporliquid
equilibrium and physical properties. The multicomponent batch distillation dynamics
simulator has major computation functions like vapor flow, liquid flow and tray holdup
calculations, enthalpy calculations, average molecular weight and density calculations, and
vaporliquid equilibrium calculations.
As assumed, the production phase the reflux drum holdup is kept constant employing
Proportional
controller.
Fig. 3.1.1. Schematic representation of the multicomponent Batch Distillation Process
22
The operation of batch distillation described here corresponds to a ternary system of

cyclohexanetoluenechlorobenzene. Among these constituent feed components, cyclohexane
is the lightest component, toluene is the intermediate component, and chlorobenzene is the
heaviest component. The model structure of the ternary distillation.
3.2.
Modeling Equations
Material balance, component balance and enthalpy balance equations can be written
accordingly,
The change in the heat energy for a very small amount of time can be considered negligible
i.e. the change is very less. So d(M Hl)/dt is very small, d(M Hl)/dt = 0; on rearrangement, we
get
23
24
25
26
EXPERIMENTAL DISTILLATION OF MeOH-H2O SYSTEM
CHAPTER 4
EXPERIMENTAL DISTILLATION OF
MEOH- H2O SYSTEM
4.1
Introduction
Batch Distillation is often preferred to continuous distillation in cases where relatively small
quantities of material are to be handled at irregularly scheduled periods. The simplest case of
batch distillation is one in which the material to be separated is charged to a heated kettle fitted
with a total condenser and product receiver. The material is distilled without reflux until a
definite quantity of one of the components of the mixture has been recovered or until a definite
change in composition of the still contents has been effected.
In all types of batch distillation, a quantity of feed is charged to a still pot, or kettle, and heat
is applied to it. The vapor which is usually passed through a fractionating column is then
condensed giving the overhead product while a less volatile residue remains in the kettle at the
end of the distillation. Continuous distillation is a steady state process because once
equilibrium has been attained, conditions at any given point remains constant whereas batch
distillation is an unsteady state process the concentration of the more volatile component
27
decreasing continually so that the temperature and composition of the mixture at a point in the
system must alter as the distillation proceeds. 4
4.2
Theory
Batch distillation with only a single still does not give a good separation unless the relative
volatility is very high. To obtain product with a narrow composition range, a rectifying batch
still is used that consists of a reboiler, a rectifying column, a condenser, some means of splitting
of a portion of condensed vapor or distillate as reflux and the receiver. The operation of a batch
still and column can be analysed using the same operating line equation as for the rectifying
section of the continuous distillation.
Yn+1= + n++XD
(4.1)
For the binary system:

y2= 1- y1x2= 1- x1
Since the slope of the operating line is R/(R+1), the slope increases as the reflux increases,
until when reflux is infinite. Under total reflux slope is 1. The operating line then coincides
with the diagonal. The number of plate is minimum at the total reflux. Minimum number of
plates required can be calculated from the terminal concentration of xb and xd based on the
relative volatility of the components , which is defined in terms of equilibrium concentrations:
( / )
(4.2)
(/ )
An ideal mixture follows Raoults law and the relative volatility is the ratio of vapor pressure.
Thus:
p1 = P1x1
28
p2 = P2x2
y1 = p1/P
(3.3)
y2 = p2/P
Therefore = P1/P2
(3.4)
The final ratio does not change much over the range of temperature encountered in a typical
column, so the relative volatility is taken as constant.
4.3
Calibration Curve
Prepare a calibration curve for Me OH- Water by plotting RI as a function of mole fraction Me
OH at the current room temperature 28C. Prepare different mixtures of Me OH + Water by
volume and measure the RI of each mixture. Convert your volume fractions and plot mole
fraction Me OH vs. RI on a simple graph.
Mole% Me OH
R.I. at 25C
1.332
10
1.335
20
1.339
30
1.341
40
1.342
50
1.34
60
1.337
70
1.334
80
1.331
90
1.329
100
1.324
Table 4.3.1: calibration curve data for different mole fraction

29
1.344
1.342
1.34
1.338
refractive index
1.336
1.334
ri
1.332
Poly. (ri)
1.33
1.328
1.326
1.324
1.322
0
20
40
60
80
100
120
molefractuion
Fig.4.3.1: the calibration curve attained from the calibration data at 28C
The calibration curve follows the following curve fitting equation:

y = -4 + 8e-11x5 2e-09x4 3e-07x3 + 1e-05x2 + 0.000x + 1.332
(4.5)
The above equation has been developed using MS-Excel
So, if we know the refractive index, it becomes easy to find the required mole fraction, using
this equation.
4.4
Description Of Apparatus
The column is made of stainless steel material packed with borosilicate glass rasching rings.
An electrically heated reboiler is installed at the bottom of the column. The bottom product is
collected in the tank. The vapours form the top of column are condensed in the shell and tube
30
Fig 4.4.1 : the laboratory packed bed distillation column
type condenser by circulating cooling water, supplied by laboratory overhead tank. The
condensate is divided into reflux and distillate by automatic reflux divider and R/D ratio can
be varied. Reflux is fed back to the column and distillate is received in a receiving tank. The
complete column is insulated for minimizing the heat loss.
31
4.4.1 Utilities
1. 50 l of methanol
2. Electricity Supply: single phase, 220V AC, 6KW with earth connection.
3 Water supply: 2LPM at 5m head
4 Floor drain required
5 Required chemicals
6 Refractometer for analysis.
4.4.2 Experimental Procedure

1. Connect the cooling water supply to setup.
2. Fill the reboiler with Methanol-water solution. The total amount of solution should
not be less than 15lts. The composition of should be in range of 15-25% of methanol
by volume.
3. Set a process temperature for the process using the digital temperature controller. The
temperature should be in range of 85-95C
4. Start the heaters and cooling supply.
5. Adjust the cooling water flow rate to a moderate value.
6. Set the cyclic timer for total reflux.
7. Wait for 25-30 min for the system to achieve steady state.
8. Now take the samples from the bottom and distillate stream.
9. Cool down the samples to room temperature and measure RI
10. Now adjust the cyclic timer to a desired reflux ratio and wait for 5min
11. Now take out the samples from both distillate and bottom product.
12. Cool down the samples and measure RI.
13. The experiment can be repeated with different set point temperatures and reflux
ratios.
32
4.5
DAY
S
EXPERIMENT OBSERVATIONS
MeOH
IN
WATE
R IN
TEMP.
REFLUX
RATIO
0.4
0.6
95
0.7
0.1
0.5
0.5
90
0.75
0.15
0.3
0.7
104
2.33333
0.6
0.4
0.3
0.7
105
1.5
0.65
0.5
0.6
0.4
103
0.66667
0.58
0.4
0.8
0.2
104
2.33333
0.75
0.65
0.2
0.8
106
0.4285714
2
0.75
0.4
0.9
0.1
105
0.56
0.1
0.85
0.15
107.1
0.72
0.65
10
0.55
0.45
107
1.5
0.7
0.65
Table 4.1: daily experiment log
33
MeOH
TOP
MeOH
BOTTOM
34
SIMULATION IN CHEMCAD
CHAPTER 5
5.1
Overview of the Batch Distillation Process
The process of building the flowsheet and simulating the batch distillation involves
the following steps:
o Create a new simulation.
o Select engineering units.
o Draw the flowsheet.
o Select the components.
o Select thermodynamic options.
o Specify pot charge.
o Specify the distillation column.
o Define operating steps.
o Run the simulation.
o Review the results and print as needed.
35
5.2
Creating a New Simulation
Start by creating a new simulation and giving it a name.

To do this, launch CHEMCAD and then Select File >Save to open the Save As
dialog box. Navigate to the directory where you want to store the simulation (try
MySimulations, located under My Documents) and give your simulation a name,
leaving the type as CHEMCAD 6 (*.cc6). Then click Save to create the file and return to the
main CHEMCAD window.
5.3
Selecting Engineering Units
Select Format >Engineering Units to open the Engineering Unit Selection dialog
box.
The English units option is the default and is currently highlighted. To change
the engineering units system, you would click the Alt SI, SI, or Metric button; you
could then change any of the individual units as well. For our project we will be using the S.I.
unit. So we will select it.
5.4
Drawing the Flowsheet
Creating a flowsheet is a matter of placing UnitOp icons

on the screen, connecting them with streams, and then adding various graphical
objects to enhance the drawing.
36
37
5.5
Selecting Components
Now you need to identify the components to be used in this simulation. Start by
selecting Thermophysical >Select Components.
For this example, youll choose components from the standard CHEMCAD
database. In the Select Components dialog box, find and add each needed
component.
From the available component section select the following components:

a) Methanol
b) Water
Then add the components to the selected components section.
Press ok
5.5.1 Thermodynamic Options

As soon as we have finished component selection, the Thermodynamics Wizard
appears. This tool can suggest thermodynamics options to use with this simulation.
Here we keep all the other constraints unchanged, just the global K option is changed to
Peng-Robinson
5.5.1.1
Specifying Pot Charge
Now that we have thermodynamics and components defined for this simulation
and we have a batch column in the flowsheet, we can define the pot charge for the column.
We will specify the pot charge according to the following rules:
The Temp (C), Pressure (psia), Vapor Fraction, and Enthalpy (MMBtu/h) fields
are the thermodynamic properties of the charge.
38
We specify the temperature, pressure, total flow and mole fraction of methanol and
water entering into the system. And press on the FLASH button. This will automatically
calculate the enthalpy.
In this case the mole fraction is kept 0.5 for both.
5.5.3
Specify the distillation column.
We will specify the distillation column details according to our condition. There the only
fixed constraint will be the number of stages which we will take as 3. The other
constraints like pressure etc will be fixed after we have the initial conditions from the
experimental setup.
Fig 5.5.1(a) : distillation column specification (general model)
39
Fig 5.5.1(b): : distillation column specification (heat and material balance)
5.5.4
Defining the Operating Steps
When you have completed the initial column specification, the Batch Operation
Parameters dialog box appears.
Here we will set the reflux ratio for the process. During our simulation we will take up
different values of reflux ratio and simulate the column operation.
5.6
Run the simulation.
In this step we run the simulation for the column that we have designed. To run the
simulation, click the Run All toolbar button. If there are errors that will be shown. So steps
would be taken to correct those accordingly.
40
5.7
Review the results and print as needed
Once the simulation is complete, we can review the results interactively before
Printing a hard copy. The commands needed to do this are located in the Report and Plot
menus.
From this menu we can get all the required outputs.
Which has been displayed in chapter 7 (results and discussion), section 7.2.
41
42
ARTIFICIAL NEURAL NETWORK
CHAPTER 6

The software that we are going to use for this project is known as justNN. This is a freeware
and very effective ANN software.
The process of using the software is described as under:
6.1.1 DATA ENTRY AND TRAINING:
First of all tables are created in the software and the input and output rows are designated.
Then the data (got from experiments) are fed into the system. Then the system is trained to
understand and find a correlation between the input and output.
Fig 6.1: the data entry and prediction sheet generated in ChemCAD
43
6.1.2 DATA PREDICTION AND FURTHER LEARNING:

In this step we insert a query row and for different conditions of input, the ANN gives
us suitable outputs. The ANN is then made to learn the new values that we have
predicted. It must be kept in mind that the error range changes with every new stage of
data prediction and learning. The software validates whether the given input in sync
with the correlations that it had created and based on that gives the output.
Fig 6.2: the internal network of ANN, correlating the output and input parameters
44
6.1.3 INPUT IMPORTANCE
Fig 6.3: the importance given to the different inputs
6.1.3 ERROR ANALYSIS:

The error analysis function of the software allows us to check the amount of error that
has occurred during the data prediction and further validation. The software allows us
to set a certain range of error so that the predicted output falls within that range of
approximation. After the learning process is complete, the software gives us a graph
which shows us the amount of error that is present in the prediction. It must be noted
that with increments in the number of prediction and validation, the amount of
average error is reduced.
Fig 6.3 : the error graph, showing the target error, maximum, minimum and average
error values
45
6.4
6.5
PROCEDURE
The input and output rows are defined in the software in the data entry page.
The input and output data, from the experiment, are entered in their respective rows.
Then the software is made to learn these values. After series of iterations, the
software creates a correlation between the input and output.
Now query rows are inserted in the table.
The input variables are inserted and the software predicts the output.
Then the values predicted are learnt.
The last two steps are repeated till we have the required amount of data for our
simulation.
Then the data is recorded up in a spreadsheet.
PREDICTION RESULTS:
DAYS MeOH WATER TEMP.

IN
IN
REFLUX MeOH
RATIO
TOP
MeOH
BOTTOM
95
0.7
0.1
0.5
90
0.75
0.15
0.3
0.7
104
2.33333
0.7499
0.5122
0.3
0.7
105
1.5
0.7499
0.4805
0.6
0.4
103
0.66667
0.7499
0.5173
0.8
0.2
104
2.33333
0.7373
0.501
0.2
0.8
106
0.4285714
0.75
0.4
0.9
0.1
105
0.56
0.1
0.85
0.15
107.1
0.72
0.65
10
0.55
0.45
107
1.5
0.7498
0.5922
0.4
0.5
0.6
Table 6.1: A.N.N prediction result

46
RESULTS AND DISCUSSIONS
CHAPTER 7

7.1
Comparison between experimental result and ChemCAD results:

EXPERIMENT
ChemCAD
MeOH TOP
MeOH TOP
MeOH BOTTOM
MeOH BOTTOM
0.7
0.1
0.366693
0.0301
0.75
0.15
0.6067237
0.07327176
0.6
0.4
0.65
0.5
0.5395392
0.011748
0.58
0.4
0.7081614
0.02940297
0.75
0.65
0.9921251
0.03692383
0.75
0.4
Could not converge
Could not converge
0.72
0.65
Could not converge
Could not converge
0.7
0.65
Could not converge
Could not converge
Could not converge
Table 7.1: experiment vs. ChemCAD

47
Could not converge
7.2
ChemCAD generated results
The ChemCAD data/calculation for the following sample:

day
10
MeOH in
0.55
Water in
0.45
temperature
107
Reflux ratio
1.5
CHEMCAD 6.1.3
Page 1
Job Name: srsctsbldist
Date: 05/14/2013
Time: 12:53:57
FLOWSHEET SUMMARY
Equipment
1
2
3
Label
Stream Numbers
TOWR
MIXE
HTXR
4
2
3
-5
1
-4
-6
-3
Stream Connections
Stream
Equipment
Equipment
From
Stream
To
Equipment
From
To
2
3
3
1
Stream
From
To
1
2
2
2
3
4
5
6
1
1
Calculation mode : Sequential

Flash algorithm : Normal
Equipment Calculation Sequence
2
3
1
No recycle loops in the flowsheet.
CHEMCAD 6.1.3
Page 2
Overall Mass Balance
Methanol
Date: 05/14/2013
lbmol/h
Input
0.000
Output
0.000
48
Time: 12:53:57
lb/h
Input
0.000
Output
0.000
Water
0.000
0.000
0.000
0.000
Total
0.000
0.000
0.001
0.001
CHEMCAD 6.1.3
Page 3
Date: 05/14/2013
Time: 12:53:57
COMPONENTS
1
2
ID #
117
62
Name
Methanol
Water
Formula
CH4O
H2O
THERMODYNAMICS
K-value model
Enthalpy model
Liquid density
:
:
UNIFAC
No correction for vapor fugacity
Latent Heat
Library
Std vapor rate reference temperature is 0 C.

Atmospheric pressure is
1.0332 kg/cm2.
CHEMCAD 6.1.3
Page 4
EQUIPMENT SUMMARIES
Date: 05/14/2013
Time: 12:53:57
Towr Rigorous Distillation Summary

Equip. No.
Name
No. of stages
1st feed stage
Condenser mode
Condenser spec.
Cond. comp i
Reboiler mode
Reboiler spec.
Reboiler comp i
Initial flag
Calc cond duty
(MMBtu/h)
Calc rebr duty
(MMBtu/h)
Est. Dist. rate
(lbmol/h)
Est. Reflux rate
(lbmol/h)
Est. T top C
1
8
8
1
1.5000
1
3
93.4000
1
6
-8.2924e-007
6.7044e-007
1.0679e-005
1.6019e-005
63.8918
49
Est. T bottom C
Est. T 2 C
Column type
No of sections
Calc Reflux ratio
Calc Reflux mole
(lbmol/h)
Calc Reflux mass lb/h
93.4000
63.9418
1
1
1.5000
2.9996e-005
0.0008
Mixer Summary
Equip. No.
Name
Output Pressure
(kg/cm2-G)
2
0.0500
Heat Exchanger Summary

Equip. No.
Name
1st Stream dp kg/cm2
1st Stream T Out C
Calc Ht Duty MMBtu/h
LMTD Corr Factor
1st Stream Pout
(kg/cm2-G)
3
0.0750
93.4000
3.6360e-007
1.0000
-0.0250
CHEMCAD 6.1.3
Page 5
STREAM PROPERTIES
Stream
Date: 05/14/2013
1 Methanol+wat properties:
Overall
Solid
Temperature deg C
32.000
Pressure kg/cm2-G
0.000
Vapor fraction
0.000E+000
Critical T deg C
280.67
Critical P kg/cm2-G
105.47
Std sp. gr. * wtr = 1
0.854
Std sp. gr. * air = 1
0.888
Deg API
34.14
Enthalpy MMBtu/h
-1.115E-006
0.000E+000
Molar flow lbmol/h
0.000
0.000
Time: 12:53:57
Vapor
Liquid
0.000E+000
-1.115E-006
0.000
0.000
50
Mass flow lb/h

0.000
0.000
Avg. mol. wt.
25.730
0.000
Actual dens lb/ft3
52.386
0.000
Actual vol
ft3/hr
0.000
0.000
Std liq vol ft3/hr
0.000
0.000
Std vapor
scfh
0.004
0.000
Cp Btu/lbmol-F
0.000
Z factor
Viscosity cP
Thermal cond. Btu/hr-ft-F
Surface tension dyne/cm
0.000
0.000
0.000
25.730
0.000
52.386
0.000
0.000
0.000
0.000
0.000
0.004
0.000
18.938
0.000
0.00000
0.0000
1.616E-003
0.6104
0.1543
30.7655
Component mole fractions

Methanol
0.5500
0.0000
0.5500
Water
0.4500
0.0000
0.4500
0.0000
0.0000
CHEMCAD 6.1.3
Page 6
STREAM PROPERTIES
Stream
Date: 05/14/2013
2 Water+methan properties:
Overall
Solid
Temperature deg C
32.000
Pressure kg/cm2-G
0.000
Vapor fraction
0.000E+000
Critical T deg C
280.67
Critical P kg/cm2-G
105.47
0.854
0.888
Deg API
34.14
Enthalpy MMBtu/h
-1.115E-006
0.000E+000
Molar flow lbmol/h
0.000
0.000
Mass flow lb/h
0.000
0.000
Avg. mol. wt.
25.730
0.000
Actual dens lb/ft3
52.386
0.000
Time: 12:53:57
Vapor
Liquid
0.000E+000
-1.115E-006
0.000
0.000
0.000
0.000
0.000
25.730
0.000
52.386
51
Actual vol
ft3/hr
0.000
Std liq vol ft3/hr
0.000
Std vapor
scfh
0.000
Cp Btu/lbmol-F
0.000
Z factor
Viscosity cP
0.000
0.000
0.000
0.000
0.000
0.000
0.004
0.000
0.004
0.000
18.938
0.000
0.00000
0.0000
1.616E-003
0.6104
0.1543
30.7655

Methanol
0.5500
0.0000
0.5500
Water
0.4500
0.0000
0.4500
0.0000
0.0000
CHEMCAD 6.1.3
Page 7
STREAM PROPERTIES
Date: 05/14/2013
Stream
properties:
Overall
Solid
Temperature deg C
32.000
Pressure kg/cm2-G
0.050
Vapor fraction
0.000E+000
Critical T deg C
280.67
Critical P kg/cm2-G
105.47
0.854
0.888
Deg API
34.14
Enthalpy MMBtu/h
-2.231E-006
0.000E+000
Molar flow lbmol/h
0.000
0.000
Mass flow lb/h
0.001
0.000
Avg. mol. wt.
25.730
0.000
Actual dens lb/ft3
52.386
0.000
Actual vol
ft3/hr
0.000
0.000
Std liq vol ft3/hr
0.000
0.000
Std vapor
scfh
0.007
0.000
Time: 12:53:57
Vapor
Liquid
0.000E+000
-2.231E-006
0.000
0.000
0.000
0.001
0.000
25.730
0.000
52.386
0.000
0.000
0.000
0.000
0.000
0.007
52
Cp Btu/lbmol-F
0.000
Z factor
Viscosity cP
0.000
18.934
0.000
0.00000
0.0000
1.694E-003
0.6104
0.1543
30.7655

Methanol
0.5500
0.0000
0.5500
Water
0.4500
0.0000
0.4500
0.0000
0.0000
CHEMCAD 6.1.3
Page 8
STREAM PROPERTIES
Stream
Date: 05/14/2013
4 Methanol+wat properties:
Overall
Solid
Temperature deg C
93.400
Pressure kg/cm2-G
-0.025
Vapor fraction
1.000E+000
Critical T deg C
280.67
Critical P kg/cm2-G
105.47
0.854
0.888
Deg API
34.14
Enthalpy MMBtu/h
-1.867E-006
0.000E+000
Molar flow lbmol/h
0.000
0.000
Mass flow lb/h
0.001
0.000
Avg. mol. wt.
25.730
0.000
Actual dens lb/ft3
0.053
0.000
Actual vol
ft3/hr
0.010
0.000
Std liq vol ft3/hr
0.000
0.000
Std vapor
scfh
0.007
0.000
Cp Btu/lbmol-F
0.000
Z factor
Viscosity cP
Time: 12:53:57
Vapor
Liquid
-1.867E-006
0.000E+000
0.000
0.000
0.001
0.000
25.730
0.000
0.053
0.000
0.010
0.000
0.000
0.000
0.007
0.000
10.095
0.000
0.989
0.01206
0.0131
0.000E+000
0.0000
0.0000
0.0000
53

Methanol
0.5500
0.5500
0.0000
Water
0.4500
0.4500
0.0000
0.0000
0.0000
CHEMCAD 6.1.3
Page 9
STREAM PROPERTIES
Date: 05/14/2013
Stream
properties:
Overall
Solid
Temperature deg C
71.497
Pressure kg/cm2-G
-0.025
Vapor fraction
0.000E+000
Critical T deg C
280.66
Critical P kg/cm2-G
105.46
0.854
0.888
Deg API
34.14
Enthalpy MMBtu/h
-2.203E-006
0.000E+000
Molar flow lbmol/h
0.000
0.000
Mass flow lb/h
0.001
0.000
Avg. mol. wt.
25.731
0.000
Actual dens lb/ft3
50.127
0.000
Actual vol
ft3/hr
0.000
0.000
Std liq vol ft3/hr
0.000
0.000
Std vapor
scfh
0.007
0.000
Cp Btu/lbmol-F
0.000
Z factor
Viscosity cP
Time: 12:53:57
Vapor
Liquid
0.000E+000
-2.203E-006
0.000
0.000
0.000
0.001
0.000
25.731
0.000
50.127
0.000
0.000
0.000
0.000
0.000
0.007
0.000
20.233
0.000
0.00000
0.0000
1.462E-003
0.3565
0.1493
26.2743
0.0000
0.5501

Methanol
0.5501
0.0000
54
Water
0.4499
0.0000
0.4499
0.0000
CHEMCAD 6.1.3
Page 10
STREAM PROPERTIES
Date: 05/14/2013
Stream
properties:
Overall
Solid
Temperature deg C
93.407
Pressure kg/cm2-G
-0.025
Vapor fraction
0.000E+000
Critical T deg C
365.22
Critical P kg/cm2-G
208.86
0.984
0.640
Deg API
12.26
Enthalpy MMBtu/h
-3.267E-010
0.000E+000
Molar flow lbmol/h
0.000
0.000
Mass flow lb/h
0.000
0.000
Avg. mol. wt.
18.534
0.000
Actual dens lb/ft3
58.803
0.000
Actual vol
ft3/hr
0.000
0.000
Std liq vol ft3/hr
0.000
0.000
Std vapor
scfh
0.000
0.000
Cp Btu/lbmol-F
0.000
Z factor
Viscosity cP
Time: 12:53:57
Vapor
Liquid
0.000E+000
-3.267E-010
0.000
0.000
0.000
0.000
0.000
18.534
0.000
58.803
0.000
0.000
0.000
0.000
0.000
0.000
0.000
18.322
0.000
0.00000
0.0000
8.549E-004
0.3012
0.3522
54.4451

Methanol
0.0370
0.0000
0.0370
Water
0.9630
0.0000
0.9630
0.0000
0.0000
CHEMCAD 6.1.3
Page 11
55

FLOW SUMMARIES
Date: 05/14/2013
Stream No.
1
4
Stream Name
Methanol+wat
Methanol+wat
Temp C
32.0000
93.4000
Pres kg/cm2-G
0.0000
0.0250
Enth MMBtu/h
-1.1154E-006
1.8671E-006
Vapor mole fraction
0.00000
1.0000
Total lbmol/h
0.0000
0.0000
Flowrates in lbmol/h
Methanol
0.0000
0.0000
Water
0.0000
0.0000
Stream No.
5
Stream Name
Temp C
71.4974
Pres kg/cm2-G
-0.0250
Enth MMBtu/h
-2.2026E-006
Vapor mole fraction
0.00000
Total lbmol/h
0.0000
Flowrates in lbmol/h
Methanol
0.0000
Water
0.0000
Time: 12:53:57
2
Water+methan
32.0000
32.0001
0.0000
0.0500
-1.1154E-006
-2.2307E-006
0.00000
0.00000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
6
93.4072
-0.0250
-3.2673E-010
0.00000
0.0000
0.0000
0.0000
CHEMCAD 6.1.3
Page 12
DISTILLATION PROFILE
Unit type : TOWR
Temp
Duties
Stg
C
MMBtu/h
1
71.5
8.292E-007
2
82.4
3
90.1
4
92.2
5
92.9
Pres
Date: 05/14/2013
Unit name:
Eqp #
*
Net Flows
*
Liquid
Vapor
kg/cm2-G lbmol/h
-0.02
0.00
-0.02
-0.02
-0.02
-0.02
0.00
0.00
0.00
0.00
lbmol/h
Time: 12:53:57
1
Feeds
Product
lbmol/h
lbmol/h
0.00 -
0.00
0.00
0.00
0.00
56
6
93.2
7
91.7
8
93.4
6.704E-007
-0.02
-0.02
-0.02
0.00
0.00
Mole Reflux ratio
0.00
0.00
0.00
0.00
0.00
1.500
Total liquid entering stage
8 at
93.407 C,
0.000 lbmol/h.
7.2.1 ChemCAD GENERATED GRAPHS AND RESULTS

7.2.1.1
TPXY GRAPH OF MeOH- H2O SYSTEM
CHEMCAD 6.1.3
1
Page
Date: 05/14/2013
Time: 13:26:07
XY data for Methanol / Water

K value model: UNIF
T Deg C
Phi2
120.161
1.000
112.308
1.000
107.285
1.000
103.744
1.000
101.065
1.000
98.925
1.000
97.138
1.000
95.595
1.000
94.224
1.000
92.980
1.000
91.830
1.000
90.752
1.000
89.732
1.000
P kg/cm2-G
Mole Fractions
X1
Y1
Gamma1
Gamma2
1.000
0.00000
0.00000
2.296
1.000
1.000
1.000
0.05000
0.26083
2.027
1.003
1.000
1.000
0.10000
0.40333
1.819
1.012
1.000
1.000
0.15000
0.49456
1.656
1.025
1.000
1.000
0.20000
0.55956
1.527
1.043
1.000
1.000
0.25000
0.60962
1.424
1.064
1.000
1.000
0.30000
0.65051
1.340
1.089
1.000
1.000
0.35000
0.68549
1.272
1.116
1.000
1.000
0.40000
0.71649
1.216
1.147
1.000
1.000
0.45000
0.74475
1.170
1.179
1.000
1.000
0.50000
0.77108
1.132
1.214
1.000
1.000
0.55000
0.79606
1.101
1.252
1.000
1.000
0.60000
0.82006
1.076
1.292
1.000
57
Phi1
88.758
1.000
87.821
1.000
86.916
1.000
86.037
1.000
85.182
1.000
84.347
1.000
83.530
1.000
82.730
1.000
1.000
0.65000
0.84339
1.055
1.333
1.000
1.000
0.70000
0.86623
1.039
1.377
1.000
1.000
0.75000
0.88876
1.026
1.423
1.000
1.000
0.80000
0.91110
1.016
1.471
1.000
1.000
0.85000
0.93332
1.009
1.521
1.000
1.000
0.90000
0.95551
1.004
1.573
1.000
1.000
0.95000
0.97772
1.001
1.627
1.000
1.000
1.00000
1.00000
1.000
1.682
1.000
58
fig 7.1: T-x-y graph of MeOH-H2O system
59
fig 7.2: x-y graph
7.2.1.2
Temperature vs. Liquid heat capacity graphs

Stream 5
Temperature C
28.000
32.158
36.316
40.474
44.632
48.789
52.947
57.105
Date: 05/14/2013
Time: 13:11:00
Pressure =-0.025 kg/cm2-G

Liquid Heat Capacity
Btu/lbmol-F
1.88302e+001
1.89384e+001
1.90552e+001
1.91755e+001
1.93002e+001
1.94291e+001
1.95666e+001
1.97076e+001
60
61.263
65.421
69.579
73.737
77.895
82.053
86.211
90.368
94.526
98.684
102.842
107.000
1.98530e+001
1.99983e+001
2.01600e+001
2.03183e+001
2.04843e+001
2.06581e+001
2.08406e+001
2.10160e+001
2.12063e+001
2.13973e+001
2.15926e+001
2.17880e+001
Fig 7.3: liquid heat capacity curve
61
7.2.1.3
Temperature vs. vapour heat capacity graphs
CHEMCAD 6.1.3
Stream 5
Pressure =
Temperature C
28.000
32.158
36.316
40.474
44.632
48.789
52.947
57.105
61.263
65.421
69.579
73.737
77.895
82.053
86.211
90.368
94.526
98.684
102.842
107.000
Date: 05/14/2013
-0.025 kg/cm2-G
Vapor Heat Capacity
Btu/lbmol-F
9.41930e+000
9.45749e+000
9.49649e+000
9.53626e+000
9.57677e+000
9.61798e+000
9.65985e+000
9.70235e+000
9.74545e+000
9.78910e+000
9.83328e+000
9.87794e+000
9.92306e+000
9.96860e+000
1.00145e+001
1.00608e+001
1.01075e+001
1.01544e+001
1.02016e+001
1.02491e+001
62
Time: 14:05:29
Fig 7.4: : liquid heat capacity curve
7.2.1.3
Temperature vs. vapour thermal conductivity graphs
CHEMCAD 6.1.3
1
Stream 5
Pressure =
Temperature C
28.000
32.158
36.316
40.474
44.632
48.789
52.947
57.105
61.263
65.421
69.579
73.737
77.895
82.053
86.211
90.368
94.526
98.684
102.842
107.000
Page
Date: 05/14/2013
Time: 13:13:44
-0.025 kg/cm2-G
Vapor Thermal Conductivity
Btu/hr-ft-F
1.00217e-002
1.01995e-002
1.03803e-002
1.05640e-002
1.07507e-002
1.09402e-002
1.11326e-002
1.13276e-002
1.15254e-002
1.17258e-002
1.19288e-002
1.21344e-002
1.23426e-002
1.25533e-002
1.27665e-002
1.29822e-002
1.32003e-002
1.34208e-002
1.36437e-002
1.38690e-002
63
Fig 7.5: Temperature vs. vapour thermal conductivity graphs
7.2.1.4
Temperature vs. liquid thermal conductivity graphs
CHEMCAD 6.1.3
Stream 5 Pressure =
Temperature C
28.000
32.158
36.316
40.474
44.632
48.789
52.947
57.105
61.263
65.421
69.579
73.737
77.895
82.053
86.211
90.368
94.526
98.684
102.842
107.000
Date: 05/14/2013 Time: 13:22:30

-0.025 kg/cm2-G
Liquid Thermal Conductivity
Btu/hr-ft-F
1.54744e-001
1.54317e-001
1.53870e-001
1.53403e-001
1.52916e-001
1.52409e-001
1.51883e-001
1.51339e-001
1.50777e-001
1.50196e-001
1.49597e-001
1.48981e-001
1.48347e-001
1.47695e-001
1.47026e-001
1.46341e-001
1.45638e-001
1.44918e-001
1.44181e-001
1.43427e-001
64
Fig 7.5: Temperature vs. liquid thermal conductivity graphs
7.2.1.5
Composite Curve
CHEMCAD 6.1.3
1
Page
Date: 05/14/2013
Time: 13:20:45
Column 1 Condenser
NP
1
2
3
4
5
6
7
8
9
10
11
Temp
C
82.4
81.3
80.2
79.1
78.0
76.9
75.8
74.8
73.7
72.6
71.5
Pres
Del H
kg/cm2-G MMBtu/h
-0.0 8.29E-007
-0.0 7.65E-007
-0.0 7.04E-007
-0.0 6.42E-007
-0.0 5.79E-007
-0.0 5.13E-007
-0.0 4.41E-007
-0.0 3.59E-007
-0.0 2.63E-007
-0.0 1.47E-007
-0.0 3.25E-010
Vapor
lb/h
0
0
0
0
0
0
0
0
0
0
0
Liquid
lb/h
0
0
0
0
0
0
0
0
0
0
0
Vap mole
frac.
1.0000
0.9271
0.8562
0.7853
0.7120
0.6337
0.5469
0.4475
0.3296
0.1849
0.0006
Vap mass
frac.
1.0000
0.9410
0.8818
0.8202
0.7538
0.6797
0.5943
0.4925
0.3673
0.2086
0.0007
Vapor
Liquid
Vap mole
Vap mass
Column 1 Reboiler
NP
Temp
Pres
Del H
65
1
2
3
4
5
6
7
8
9
10
11
C
86.5
87.2
87.9
88.6
89.3
89.9
90.6
91.3
92.0
92.7
93.4
kg/cm2-G MMBtu/h
-0.0 9.54E-013
-0.0 4.06E-008
-0.0 8.37E-008
-0.0 1.30E-007
-0.0 1.80E-007
-0.0 2.36E-007
-0.0 2.99E-007
-0.0 3.70E-007
-0.0 4.53E-007
-0.0 5.51E-007
-0.0 6.70E-007
lb/h
0
0
0
0
0
0
0
0
0
0
0
lb/h
0
0
0
0
0
0
0
0
0
0
0
frac.
0.3463
0.3862
0.4283
0.4736
0.5227
0.5770
0.6379
0.7074
0.7880
0.8837
0.9998
frac.
0.3961
0.4367
0.4786
0.5226
0.5696
0.6205
0.6768
0.7400
0.8125
0.8975
0.9998
Pres
Del H
kg/cm2-G MMBtu/h
0.1
0.000
0.0 4.21E-009
0.0 8.45E-009
0.0 1.27E-008
0.0 1.71E-008
0.0 2.14E-008
0.0 2.59E-008
-0.0 1.60E-007
-0.0 3.22E-007
-0.0 3.61E-007
-0.0 3.64E-007
Vapor
lb/h
0
0
0
0
0
0
0
0
0
0
0
Liquid
lb/h
0
0
0
0
0
0
0
0
0
0
0
Vap mole
frac.
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.4119
0.8916
1.0000
1.0000
Vap mass
frac.
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.0000
0.4551
0.9117
1.0000
1.0000
Stream 3
NP
1
2
3
4
5
6
7
8
9
10
11
Temp
C
32.0
38.1
44.3
50.4
56.6
62.7
68.8
75.0
81.1
87.3
93.4
Hot Composite
Temp C
71.497
71.606
71.715
71.823
CHEMCAD 6.1.3
2
DH MMBtu/h
0.000e+000
1.647e-008
3.216e-008
4.755e-008
Page

71.932
72.041
72.150
72.258
72.367
72.476
72.584
72.693
72.802
72.911
73.019
73.128
73.237
73.345
73.454
Date: 05/14/2013
6.263e-008
7.741e-008
9.190e-008
1.061e-007
1.200e-007
1.335e-007
1.466e-007
1.591e-007
1.715e-007
1.836e-007
1.955e-007
2.073e-007
2.188e-007
2.301e-007
2.412e-007
66
Time: 13:20:45
73.563
73.671
73.780
73.889
73.998
74.106
74.215
74.324
74.432
74.541
74.650
74.759
74.867
74.976
75.085
75.193
75.302
75.411
75.519
75.628
75.737
75.846
75.954
76.063
76.172
76.280
76.389
76.498
76.607
76.715
76.824
76.933
77.041
77.150
77.259
77.367
77.476
77.585
77.694
77.802
77.911
CHEMCAD 6.1.3
3
2.521e-007
2.629e-007
2.732e-007
2.833e-007
2.932e-007
3.030e-007
3.127e-007
3.222e-007
3.316e-007
3.408e-007
3.499e-007
3.589e-007
3.674e-007
3.759e-007
3.844e-007
3.927e-007
4.009e-007
4.091e-007
4.171e-007
4.251e-007
4.329e-007
4.407e-007
4.482e-007
4.557e-007
4.631e-007
4.704e-007
4.777e-007
4.849e-007
4.921e-007
4.992e-007
5.062e-007
5.132e-007
5.200e-007
5.267e-007
5.334e-007
5.401e-007
5.468e-007
5.534e-007
5.599e-007
5.665e-007
5.730e-007
Page

78.020
78.128
78.237
78.346
78.454
78.563
78.672
78.781
78.889
78.998
Date: 05/14/2013
5.795e-007
5.858e-007
5.921e-007
5.984e-007
6.047e-007
6.110e-007
6.173e-007
6.235e-007
6.298e-007
6.360e-007
67
Time: 13:20:45
79.107
79.215
79.324
79.433
79.542
79.650
79.759
79.868
79.976
80.085
80.194
80.302
80.411
80.520
80.629
80.737
80.846
80.955
81.063
81.172
81.281
81.390
81.498
81.607
81.716
81.824
81.933
82.042
82.150
82.259
82.368
Cold Composite
Temp C
32.000
32.614
33.228
33.842
34.456
35.070
35.685
36.299
36.913
37.527
38.141
38.755
CHEMCAD 6.1.3
4
6.422e-007
6.483e-007
6.544e-007
6.605e-007
6.667e-007
6.728e-007
6.789e-007
6.851e-007
6.912e-007
6.974e-007
7.035e-007
7.096e-007
7.157e-007
7.218e-007
7.279e-007
7.341e-007
7.403e-007
7.465e-007
7.527e-007
7.590e-007
7.653e-007
7.716e-007
7.779e-007
7.842e-007
7.906e-007
7.970e-007
8.034e-007
8.098e-007
8.163e-007
8.227e-007
8.292e-007
DH MMBtu/h
0.000e+000
4.189e-010
8.382e-010
1.258e-009
1.678e-009
2.099e-009
2.519e-009
2.941e-009
3.362e-009
3.784e-009
4.207e-009
4.629e-009
Page

39.369
39.983
40.597
41.211
41.825
Date: 05/14/2013
5.052e-009
5.476e-009
5.900e-009
6.324e-009
6.749e-009
68
Time: 13:20:45
42.439
43.053
43.667
44.282
44.896
45.510
46.124
46.738
47.352
47.966
48.580
49.194
49.808
50.422
51.036
51.650
52.264
52.879
53.493
54.107
54.721
55.335
55.949
56.563
57.177
57.791
58.405
59.019
59.633
60.247
60.861
61.476
62.090
62.704
63.318
63.932
64.546
65.160
65.774
66.388
67.002
67.616
68.230
68.844
69.458
70.073
70.687
71.301
71.915
72.529
73.143
CHEMCAD 6.1.3
5
7.174e-009
7.599e-009
8.025e-009
8.452e-009
8.878e-009
9.306e-009
9.733e-009
1.016e-008
1.059e-008
1.102e-008
1.145e-008
1.188e-008
1.231e-008
1.274e-008
1.317e-008
1.360e-008
1.403e-008
1.447e-008
1.490e-008
1.533e-008
1.577e-008
1.620e-008
1.663e-008
1.707e-008
1.751e-008
1.794e-008
1.838e-008
1.881e-008
1.925e-008
1.969e-008
2.013e-008
2.057e-008
2.101e-008
2.145e-008
2.189e-008
2.233e-008
2.278e-008
2.322e-008
2.366e-008
2.410e-008
2.455e-008
2.499e-008
2.543e-008
2.596e-008
3.815e-008
5.061e-008
6.334e-008
7.635e-008
8.963e-008
1.032e-007
1.170e-007
Page
Date: 05/14/2013
69
Time: 13:20:45
73.757
74.371
74.985
75.599
76.213
76.827
77.441
78.055
78.670
79.284
79.898
80.512
81.126
81.740
82.354
82.968
83.582
84.196
84.810
85.424
86.038
86.652
87.267
87.881
88.495
89.109
89.723
90.337
90.951
91.565
92.179
92.793
93.407
1.311e-007
1.455e-007
1.602e-007
1.764e-007
1.925e-007
2.087e-007
2.249e-007
2.410e-007
2.572e-007
2.734e-007
2.895e-007
3.057e-007
3.218e-007
3.257e-007
3.297e-007
3.337e-007
3.376e-007
3.416e-007
3.455e-007
3.495e-007
3.535e-007
3.669e-007
4.072e-007
4.459e-007
4.870e-007
5.314e-007
5.796e-007
6.326e-007
6.921e-007
7.593e-007
8.361e-007
9.266e-007
1.034e-006
70
Fig 7.6: composite curve
7.2.2
Discussion:
We can see that there is lots of errors in the ChemCAD simulation results. It is
because of the fact that ChemCAD works for ideal situations, since we do not
have those ideal situations in our current lab, so for many conditions we get
these error messages.
From the comparison study we see that the results do not match and there is
huge amount of difference. This problem arises, because our equipments are
not module to serve the purpose of high accuracy distillation operations
71
7.3
Comparison between experimental result and A.N.N results:
EXPERIMENT
ANN
MeOH TOP
MeOH BOTTOM
MeOH TOP
MeOH BOTTOM
0.7
0.1
0.75
0.2897
0.75
0.15
0.75
0.15
0.6
0.4
0.7499
0.5151
0.65
0.5
0.7499
0.4805
0.58
0.4
0.7499
0.5173
0.75
0.65
0.7373
0.501
0.75
0.4
0.75
0.4
0.56
0.1
0.56
0.1
0.72
0.65
0.72
0.65
0.7
0.65
0.7498
0.5922
Table 7.2: experiment vs. ANN
7.3.1
Discussions:
We see that A.N.N results are quite similar to the experimental results. Here we were
limited by the equipment in the implementation of the many other controlling factors.
But in real life industrial situation, where we will have the liberty of finding many other
factors, the use of A.N.N, would be good.
The accuracy of A.N.N depends on the number of input factors. The differences in our
results with the A.N.N values is due to the lack of chances to monitor controlling
factors.
72
73
74
CONCLUSION AND FUTURE SCOPE OF STUDY
CHAPTER 8
CONCLUSIONS AND FUTURE SCOPE OF STUDY
In the past A.N.N has never been used to study and predict the outcome of the products from the
distillation column. This has been a first attempt to do so. And the results from the A.N.N
predictions are really promising.
With only four changeable factors, namely methanol in, water in, temperature and reflux ratio,
we have seen that the results from the prediction are quite close to the experimental results.
So it can be hoped that, in the future, if these studies are conducted on real life industrial scale
columns, then A.N.N might be really successful.
As for the case of the ChemCad software simulation. We have used it to actually see the
variations that our equipments suffer from that of the original data. So there is a lot of scope for
the upcoming students to investigate the sectors where the laboratory equipments are falling
short of the real/ industrial distillation columns.
73
REFERENCES
CHAPTER 9
REFERENCES:
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Principles and Practice (Illustrated ed.). Oxford: Blackwell Scientific Publications.
pp. 141143. ISBN 978-0-632-02017-1.
2. ^ a b Forbes, Robert James (1970). A short history of the art of distillation: from the
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China. Routledge. pp. 147148. ISBN 978-1-134-27542-7. "The earliest possible period
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distillation of spirits for drinking in China is during the Jin and Southern Song dynasties"
5. ^ Sarton, George (1975). Introduction to the history of science. R. E. Krieger Pub. Co.
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6. ^ Holmyard, Eric John (1990). Alchemy. Courier Dover Publications. p. 53. ISBN 0-48626298-7.
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8. ^ Industrial Engineering Chemistry (1936) page 677
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20. ^ Laurence M. Harwood, Christopher J. Moody (13 June 1989). Experimental organic
chemistry: Principles and Practice (of) (Illustrated ed.). Wiley, Blackwell.
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25. ^ Energy Institute website page
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commercial packed towers, Moore, F., Rukovena, F., Chemical Plants & Processing,
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Engineering and Processing 45 (11): 1011. doi:10.1016/j.cep.2006.05.003.
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Kunesh, John G.; Lahm, Lawrence; Yanagi, Takashi (1987). "Commercial scale
experiments that provide insight on packed tower distributors". Industrial & Engineering
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Symposium on Artificial Neural Networks. Elsevier.doi:10.1016/j.neucom.2004.07.002.

Retrieved 2011-12-30.
5. ^ Wu, J., Chen, E. (May 2009). "A Novel Nonparametric Regression Ensemble for
Rainfall Forecasting Using Particle Swarm Optimization Technique Coupled with
Artificial Neural Network". In Wang, H., Shen, Y., Huang, T., Zeng, Z.. 6th International
Symposium on Neural Networks, ISNN 2009. Springer.doi:10.1007/978-3-642-015137_6. ISBN 978-3-642-01215-0. Retrieved 2012-01-01.
6. ^ Roman M. Balabin, Ekaterina I. Lomakina (2009). "Neural network approach to
quantum-chemistry data: Accurate prediction of density functional theory energies". J.
Chem. Phys. 131 (7): 074104. doi:10.1063/1.3206326. PMID 19708729
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APPENDIX
1. MODELLING EQUATIONS
23
2. CALIBRATION CURVE
29
30
3. CURVE FITTING EQUATION
30
4. DAILY EXPERIMENT LOG
33
5. PREDICTION RESULT
46
6. COMPARISON BETWEEN EXPERIMENTAL RESULT

AND CHEMCAD RESULTS
47
7. ChemCAD GENERATED RESULTS
48
8. TPXY GRAPH OF MeOH- H2O SYSTEM
57
9. TEMPERATURE VS. LIQUID HEAT CAPACITY GRAPHS
60
10. TEMPERATURE VS. VAPOUR HEAT CAPACITY GRAPHS
62
11. TEMPERATURE VS. VAPOUR THERMAL CONDUCTIVITY GRAPHS
63
12. TEMPERATURE VS. LIQUID THERMAL CONDUCTIVITY GRAPHS
64
13. COMPOSITE CURVE
65
14. COMPARISON BETWEEN EXPERIMENTAL RESULT

AND A.N.N RESULTS
72

Batch Distillation of Water-Methanol System

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Batch Distillation of Water-Methanol System

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Batch distillation of methanol-water system and modeling

and simulation of distillation column using ARTIFICIAL

Satadru Chakrabarty, Sayantan Roy Choudhury, Tapas Saha

NATIONAL INSTITUTE OF TECHNOLOGY

BATCH DISTILLATION OF METHANOL-WATER SYSTEM

Chemical Engineering Department

To all the teachers of the department

This thesis/dissertation/report entitled Batch distillation of methanol-water system and

Fig. 1.1: basic layout of a distillation column

Fig. 1.2.1: a typical packed distillation column

Fig. 1.2.2 :The basic distillation column

Fig. 1.3.1: Typical Process flow diagram in ChemCAD

Fig. 1.4.1: the data is entered in this sheet

Fig. 3.1.1:schematic representation of the multicomponent Batch

Fig 4.4.1 : the laboratory packed bed distillation column

Fig. 5.4.1: flowsheet of batch distillation as displayed by ChemCAD

Fig. 5.5.1(a) : distillation column specification (general model)

Fig. 5.5.1(b): distillation column specification (heat and material balance)

Fig 6.3: the importance given to the different inputs

minimum and average error values

Fig 7.1: T-x-y graph of MeOH-H2O system

Fig 7.2: x-y graph

Fig 7.3: liquid heat capacity curve

Fig 7.4: : liquid heat capacity curve

Fig 7.5: Temperature vs. vapour thermal conductivity graphs

Fig 7.6: Temperature vs. liquid thermal conductivity graphs

Fig 7.7: composite curve

Table 4.3.1: calibration curve data for different mole fraction.

Table 4.5.1: daily experiment log

Table 6.1: A.N.N prediction result

Table 7.1: experiment vs. ChemCAD

Table 7.2: experiment vs. ANN

Table 7.3: experiment vs. ANN vs. ChemCAD

LIST OF SYMBOLS AND ABBREVIATIONS

MB =liquid holdup in still pot (kmol)

List of Symbols and Abbreviations

1.1 Methanol Water system

Chapter 2 Literature Review

2.1 Batch Distillation

Chapter 3 Modelling of the distillation column

3.1 Process Description

3.2 Modeling Equations

Chapter 4 Experimental distillation of MeOH- H2O system

4.3 Calibration Curve

4.4 Description of Apparatus

4.5 Experimental Observation

Chapter 5 ChemCAD simulation

5.1 Overview of the Batch Distillation Process

5.2 Creating a New Simulation

5.3 Drawing the Flowsheet

5.4 Selecting Engineering Units

5.5 Selecting Components

5.6 Run the simulation.

5.7 Review the results and print as needed

Chapter 6 Artificial Neural Network

6.1 Data entry and training

6.2 Data prediction and further learning

6.3 Error analysis

6.5 Prediction results

Chapter 7 Results and Discussions

7.1 Comparison between experimental result and ChemCAD results 47

7.3 Comparison between experimental result and A.N.N results

Chapter 8 Conclusions and Future Scope of Study

2.2 Artificial Neural Network