The Production of Acetylsalicylic Acid Project

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The Production of Acetylsalicylic acid Project
Summary
When considering the design of a crystallizer, there are a number of things to consider. Solubility of the
components in the solution, the supersaturation and the growth of the components are crucial in the
overall design of the crystallizer. During the design of the crystallizer, it is important to identify the
activities such as the growth of the crystals. The growth of the crystals only occurs at the supersaturated
state. The growth is usually started with the nuclear formation and the gradual growth hence follows. In
order to make a proper design of the crystallizer for the Acetylsalicylic acid, the crystal growth rate
should be determined in the laboratory. This is where the residence time is determined. The rate of the
crystal growth is also determined in the process which also corresponds to the time spent in the in the
crystallizer.
The most important parameter to consider in the crystallizer control design is the supersaturation. The
parameter is responsible is responsible for the scaling of the heat transfer areas. It is also responsible for
the nucleation process and the CSD. When the natural cooling is considered in cooling slurry in the
crystallizer, the level of supersaturation is rapidly increased thus slurry reaches metastable state in the
early stage of crystallization. Basically the resulting crystals formed are finer and of poor quality.
When seeding a controlled cooling is applied, the desired crystal size is then obtained. In this case the
cooling rate is under control therefore a metastable state is maintained throughout the process of
nucleation.
Hazards and operations analysis is a result of the theory that the problems in the operations failure is
mainly caused by the failure of the process design and the inability of the system to cope with the
challenges during the operations. Basically these problems can be identified from the control system of
the Piping and the instrumentation diagram. In exploration of the problems that might have been caused
by the faults in the design or any other problem developed during the processing of the materials can be
obtained mainly from the human analysis of the process.
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The P&ID is an important diagram during the design and when applied in the field. Basically the
diagram is essential in showing the piping system and the control of the plant and in specific the
Crystallizer. Some of the major components in the P&ID of the crystallizer are basically the design
specifications as the installation of the instrumental and control, the flow of the process, various
components of the machine which are important in the process of accomplishing the requirement for the
processing.
Table of Contents
Summary 2
INTRODUCTION 6
1.0 Project Brief 6
1.1 Project Objectives 6
1.2 Project Plan 8
1.3 Technical Objectives 8
1.4 Personal Objectives 9
1.5 Techniques to Accomplish the Objectives 10
2 CRYSTALLIZER DESIGN 10
Design of a batch crystallizer 11
Chemical engineering design 12
Retention time 12
Heat transfer area 13
Vaporization surface 14
Elements of a batch crystallizer 14
Pipe diameter 14
Wall thickness 15
Stirrer size 15
Diameter 16
Height 16
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Baffle height and width 17
Power 18
Design Parameters 19
Calculation of volume 19
Calculation of baffle width 20
Calculation of baffle height 20
Calculation of wall thickness 20
Design 23
Mass and energy balance in the crystallizer 23
Energy balance around the crystallizer: 23
Q for Crystallizer Inlet: 24
Acetic acid (by product): 25
Acetic anhydride: 25
Sulphuric acid catalyst: 26
Q for Crystalliser outlet: 27
Energy balance 28
Mechanical design 32
Design Consideration 32
Habits of the crystals 32
Defects in the crystals 33
Characteristics of the particles formed 33
Mixing in the crystallizer 35
Simulation of the fluid mechanics in the crystallizer 36
Mechanism Models 38
Scale up 39
Summary 39
HAZOP (Hazards and Operations Analysis) 40
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HAZOP process 42
Piping and Instrumentation Diagram (P&ID) 44
47
Control and instrumentation 48
Control diagram 48
Batch crystallizer control and instrumentation 48
Introduction 48
Control 49
Operating at Maximum control 50
Control and Instrumentation 51
Feedback controllers 52
Economic Appraisal of Process 52
References 58
APPENDIXES 62
A.Cost Index for some equipment. 62
B. General characteristics for various equipment types(Coulson 2011). 64
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INTRODUCTION
1.0 Project Brief
This individual design project entails the development of a process to produce 5000 tonnes of
acetylsalicylic acid (Aspirin) per year. The plant will be located in the UK. The feedstock to the plant are;
solid salicylic acid, acetic anhydride and sulphuric acid which act as a catalyst. The process main
equipments include the feedstock storage tanks, reactor, filter, crystalliser, slurry tank, centrifuge,
distillation column, washer, drier and Grinder. The individual assignment was to design and develop the
crystalliser. The crystallisation process is a batch process with the main inputs being Aspirin, acetic acid,
acetic anhydride and sulphuric acid. These inputs appear as solids at the end of the crystallisation
process.
1.1 Project Objectives
The general objective of this project is to design a manufacturing facility that has a capacity of producing
5000 tonnes of aspirin per year. The main objective of the individual project is to design and evaluate the
performance of the crystalliser in the aforementioned manufacturing facility.
In the design and evaluation of the crystalliser for the manufacturing facility, the following main factors
need to be taken into consideration;
»
Evaluation of the crystallisation process
First I will study the crystallisation process and the factors that affect the process
»
Evaluation of the different crystallisation units used in conventional manufacturing facilities.
Next, I will study the different crystallisation units that are currently available in the market. A detailed
study of these crystallisation units, their capacity, limits and demerits will be done. This will be done
through a thorough literature review of the existing crystallisation technologies and equipment required.
»
Selection of the best crystallisation facility: After a detailed examination of the existing technology, I will
select the best crystalliser to use. The selection of the crystalliser will be based on costs, its efficiency,
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resulting quality of the product and compatibility with other processes in the manufacturing line.
»
Evaluation of the chemical engineering design of the crystalliser: After selecting the crystalliser, a detailed
description of the crystalliser will be done. The different equipments and the chemical changes that
occur in this process will be elaborated. The design methodology of the crystalliser is described in
detail. A datasheet with all the design data and specification will then be prepared. A concept
drawing of the crystalliser will then be drawn.
»
Design of the control and instrumentation systems for the crystalliser: The control and instrumentation of
the crystalliser will then be described. All the systems, instruments functions as well as the control
strategy will be elaborated.
»
Design and drafting of the piping and instrumentation diagram for the crystalliser: This will be a design of all
the piping, equipments and instrumentation diagram for the crystalliser. A legend of all the symbols
used will then be drawn.
»
Conduct a hazard and operable study (HAZOP) for the crystalliser: The hazard and operability study of one
of the major line in the acetylsalicylic acid manufacturing process will be done. This part will be done
as a group activity.
»
Perform an economic evaluation of the whole process: An estimate of the overall capital cost and operation
and maintenance cost for the whole acetylsalicylic acid manufacturing plant will be carried out.
»
Prepare a project report for the selected process: A detailed report will then be prepared
»
Reference all the work properly
1.2 Project Plan
In order to archive the set objectives, the researcher prepared a Gna chart detailing all activities and
time schedule they will take. This enabled the researcher perform all activities comprehensively and in
time. The Gna chart is a ached at appendices section.
1.3 Technical Objectives
The main technical objectives are;
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»
To evaluate the aspirin manufacturing process
»
To develop a project plan and draw a gnat chart
»
To evaluate the different crystalliser units
»
To design and draw the crystalliser unit
»
To calculate the mass balance for the crystalliser
»
To calculate the energy balance for the crystalliser
»
To design the control and instrumentation system for the crystalliser
»
To design and draft the piping and instrumentation diagram for the crystalliser
1.4 Personal Objectives
»
Research: for the design to be appropriate, a detailed research of the manufacturing process is
necessary. The researcher will conduct a detailed research which involves extensive reading of
academic journals, books, company catalogue and other materials.
»
Organisation: conducting this research against a fixed timeline require a lot of organisation and time
scheduling. During this research, I will ensure that I adhere strictly to the gna chart.
»
Enhance knowledge and skills: During the course of the research, design and drawing, I will gain an in
depth understanding of this process as well as a general understanding of the chemical engineering
processes. My expertise in the field of chemical engineering will be greatly improved.
»
Presentation: After the final design, an oral presentation and a report will be wri en. My skills in
writing and presenting the finding must be improved in order to succeed.
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Enhance computer skills: this project requires that I use several computer programs for different
functions. for the project to be successful, I must understand how to use the flowing programs
»
Microsoft word: this program will be used for writing the final report
»
Microsoft excel: this program will be used to perform all computations and for drawing graphs and for
drawing the gnat chart.
»
Microsoft Visio: for drawing PFDs
»
Microsoft outlook: for communication with group members
»
Microsoft project;
»
Internet explorer: for searching materials
1.5 Techniques to Accomplish the Objectives
In order to archive the set objectives, the researcher will;
»
Ensure that the timeline set in the gannt are strictly adhered to
»
Conduct extensive literature review on aspirin manufacturing process
»
Engage in teamwork and group discussions
»
Consult with the course instructor regularly
Ensure that am well versed with the IT knowledge and software packages to be used
2 CRYSTALLIZER DESIGN
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When considering the design of a crystallizer, there are a number of things to consider. Solubility of the
components in the solution, the supersaturation and the growth of the components are crucial in the
overall design of the crystallizer. During the design of the crystallizer, it is important to identify the
activities such as the growth of the crystals. The growth of the crystals only occurs at the supersaturated
state(Crundwell 2008). The growth is usually started with the nuclear formation and the gradual growth
hence follows. In order to make a proper design of the crystallizer for the Acetylsalicylic acid, the crystal
growth rate should be determined in the laboratory. This is where the residence time is
determined(Letcher 2004). The rate of the crystal growth is also determined in the process which also
corresponds to the time spent in the in the crystallizer. For the batch process, crystallization can be
speeded up by seeding. The overall crystals weight can be estimated by the McCabe Delta-Law where
the original crystals grow to the same size(Seliger Khraisheh, & Jawahir 2011). Therefore the overall size
can quote in terms of the size increment which can be denoted by ∆L(Silla 2003).
Determination of the number of crystals formed per a batch, or per unit volume can be calculated from
the rate of nucleation and the degree of supersaturation. ∆Xo
Where the ∆Xo can be determined by
∆Xo=X-Xs
Design of a batch crystallizer
In the design of a batch crystallizer, it is important to put in mind the importance of correctly placing the
equipment to ensure optimum operations are maintained. The agitator should always be well placed to
ensure the mixing is done in a proper and enabling manner. The optimum operating conditions are
obtained at the supersaturated and metastable conditions.
The growth of the crystals follows the increased growth which is based on the McCabe Delta-Law. The
law highlights that as the size of the crystals increases, the mass also increase therefore posing a threat of
the suspension se ling at the bo om of the crystallizer(Silla 2003). To overcome the challenge, the
agitator is maintained in circulation in order throw away any suspension se ling at the bo om. That is
mainly why the agitator is situated at the bo om of the crystallizer. The increase in mass of the crystals
results in the increase in the length. The relationship between the increase in mass and the length can be
illustrated is basically based on a computer program (Rangaiah & Kariwala 2011).
Chemical engineering design
The objective of the project is to design a crystallizer to crystallize aspirin from a batch reactor designed
in the earlier project. The temperature of the reactor is 90 degrees Celsius meaning that the exit
temperature of the products is at the same. This temperature must be reduced by cooling in order to
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form crystals of required size in an effective and economical manner. According to the scale of operation
a batch crystallizer is fit since it has small capacity, simple instrumentation and is self cleaning as
indicated in the table of general characteristics below.
Retention time
Earlier in this project we designed a batch reactor to be used to produce 5000 tonnes of aspirin per
annum(Crundwell 2008). It was assumed therefore that the plant is to run for 47.143 weeks or 330 days in
a year including day and night. This translates to7920 hours time of running annually. The remaining
time which is about 35 days takes care of emergencies, cleaning, repair and maintenance(Rangaiah &
Kariwala 2011).
The time for a batch of the reactor was earlier assumed to be five hours. Therefore retention time in the
crystallizer is related to the overall time in the crystallizer. A time of three hours apposite for cooling and
the remaining two hours for feeding and unloading for every batch and removal of dirt before feeding
the next batch. Cooling time is enough thus energy can be saved since pumps which could have been
used for forced circulation are not necessary(Tung 2009). Optimum crystallization is achieved when
batch time is long thus ensuring maximum heat transfer(Coulson 2011).
Heat transfer area
Heat transfer area can be calculated from the dimensions of the crystallizer. The curved surface of the
vessel has water (coolant) jackets and is thus the most effective surface for heat transfer (Sam Mannan
2005). Though the top and bo om are also heat transfer surfaces they may be ignored since their
contribution to the overall heat transfer is not significant compared to the curved surface. Baffles are
good conductors of heat and are fixed on the curved surface (Silla 2003). They conduct heat from the
vessel wall pass it to the vessel contents. The total heat transfer area is therefore the sum of curved
surface and the area of the baffles.
The diameter and height of the crystallizer is =1.627 m and = 1.843 m respectively. Curved surface area is
given by 2π
=2 π (1.627) (1.843)
=18.84 m2
Surface area of the baffles
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The height and width of the baffle are 1.659 m and 0.1627 m respectively. They are four and distributed
uniformly on the wall. Each baffle has two opposite surfaces(Letcher 2004).
=2(4) (1.659) (0.1627)
= 2.16 m2
Total heat transfer area =18.84+2.16
=20.1 m2
Vaporization surface
Surface area for vaporization of water is determined from diameter of the vessel. For a diameter of 1.627
m the vaporization area is given by;
Area, A= πr2
= π (1.627/2)2
= 2.08 m2
Elements of a batch crystallizer
There are three major considerations in the design of a crystallizer namely policy of operation,
performance and size of vessel. First, the capacity of the crystallizer must first be known. It is determined
by the amount of contents from the batch reactor and the time spent in the crystallizer. Particle size and
suspension density determines the size of the agitator, power requirement and the speed of the
pump(Theodore & Ricci 2011). Secondly, performance is measured based on quality of crystals and the
rate of production in terms of mass. There are aspects of design such as level of maximum super
saturation which set up constraints(Crawley, Preston, & Tyler, 2008).
Policy of operation, the suitable cooling curve, rate of evaporation must be specified. For production of
crystals of defined mass and size a seeding policy needs to be known and a suitable batch time should be
particular so that the final size of the particle is a ained. Therefore performance and policy of operation
and size of vessel are correlated(Crundwell 2008).
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Pipe diameter
The sizing of a pipe leading to and from the crystallizer is simply based on the diameter of the mixer
(Coulson 2011). Therefore to ensure smooth delivery and discharge, the mixer, entry and exit diameter
should be of the same size. It is important note that this feature is not as important for a batch crystallizer
as it is in the continuous crystallizer (Silla 2003).
Wall thickness
Wall thickness is reliant on a number of factors considered in design of a crystallizer. There are several
functions a wall executes in every vessel. These includes holding vessels contents in position, gives the
necessary strength to encounter stresses caused by pressure column, provides room for coolant jacket,
serves as a conductor of heat and acts as heat transfer surface area for the coolant and mixer
contents(Crawley, Preston, & Tyler, 2008).
Material must be selected based on heat transfer consideration. Good conductors of heat are essential for
optimal heat transfer to be a ained. From engineering standards, an allowance of 0.01 m for the water
jacket gives a range up to 0.02m wall thickness sufficient to hold the vessel contents enhancing
endurance to both thermal stresses and pressure due to column of the mixer contents(Seliger Khraisheh,
& Jawahir 2011).
Stirrer size
For effective cooling maximum heat transfer should occur between the coolant and the
crystals(Crundwell 2008). A thorough mixing in the crystals should hence be enhanced through bringing
into play a mixer. Good mixing occurs when turbulent flow transpires in the vessel warranting uniform
distribution of heat gain from the baffle and wall.
Optimum mixing is also dependent on the location of the impeller. The impeller should be in a position
that will give the best possible mixing for the batch. While power is transmi ed from the motor to the
agitator shaft, there exists an associated torque as a resultant resistance at its blades due to viscosity and
frictional resistance of the fluid.
Shear stresses are hence induced on the agitator shaft and for design purposes a consideration for this
stresses must made so as to avoid material yield and strain. Shear stresses are distributed from zero at
the neutral point (the center line) to the maximum at the outer surface(Silla 2003). Stresses and strains
affect the diameter of the shaft as well as the ratio of shaft length to the shaft diameter(Sam Mannan
2005). The choice of size, length and material type is hence based on the tensile strength(Coulson 2011).
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Figure: diagram showing the diameter and height of the agitator.
Diameter
Stirrer blades must be designed in a warped manner such that they can move the contents against
gravity without twisting or fla ening(Seliger Khraisheh, & Jawahir 2011). The agitator shaft bearing
should be firm enough to give enough reaction due to fluid acceleration. The length of the blades is
constrained by the radius of the vessel(Wan 2005). In favor of optimum fluid mixing there is a length for
optimum mixing to be achieved and is usually a point where the ratio of impeller diameter to the vessel
diameter 2:5.
Height
The principle of an impeller is to muddle up the filling in the container. The impeller (also known as the
agitator) has blades usually rotating at lower portion of container. This is the position for optimum
mixing in the container(Silla 2003). Given the height of the crystallizer if defined then the agitator height
starts from the top most point where the motor is mounted and runs down to the bo om of the vessel
leaving just a sufficient clearance for fluid sweep without formation of vortices(Crundwell 2008).
Baffle height and width
Baffle height is determined by the overall height of the vessel starting from the tangent line at the bo om
to the top. Since the stirrer blades must be located at the lowest point in the crystallizer, the baffle width
may be modified at the bo om to give room for the impeller(Ende 2011). An adequate clearance is
considered to avoid the creation of vortexes at the ends. A ratio of 10:9 (ratio of vessel height to baffle
height) is apposite for sufficient turbulence to be achieved. Heat transfer can also be enhanced by the
baffles since they increase the heat transfer surface area(Tung 2009).
Figure, vessel height, baffle height and width
The figure is half section of the crystallizer showing the key dimensions. For this design the overall
height is 1.843 m and the baffle width and height are 1.659 m and 0.1627 m respectively(Coulson 2011).
In baffle width design, viscosity is a vital factor for concern as it determines the type of flow of the vessel
fluid. If we are to achieve cooling effect through heat transfer as well as uniform crystal distribution, then
contents must be kept flowing in a turbulent state failure to which sedimentation will occur especially in
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the case of laminar flow. In this design we are aiming at a aining turbulent flow. When considering the
width of the baffle one must keep in mind the dimensional constraints due to the geometrical nature of
the vessel. A baffle is normally fixed on the vessel wall and protrudes towards the center of the mixer.
Effective mixing i.e. maximum mixing occurs at some distance between the agitator arm and the wall of
the mixer(Silla 2003). This can be done experimentally for fluids with different specific gravities,
viscosities and choosing various ratios of height to diameter(Crundwell 2008). Standard ratios for
different types of crystallizers have been determined and tabulated for quick reference. In case of batch
type crystallizer we refer to the Metric standard where the baffle width to mixer diameter ratio is
1:10(Chianese & Kramer 2012).
Power
Without energy no work can be done. Work is said to be done when a force is moved through a
distance(Theodore & Ricci 2011). The crystals in the crystallizer have mass, thus due to gravitational
acceleration this crystals experiences a pull equal its weight towards the base of the tank(Houson 2011).
There will be separation of heavy and light contents due to differences in their densities. As a result
residues are formed and they sink to lowest point of the vessel(Chianese & Kramer 2012). Power is
required to drive the impeller so that the impeller blades transmit energy to move the residues back up
and keep them evenly mixed(Rangaiah & Kariwala 2011). It is important to note that there are energy
losses in form of heat between the blades and the fluid. This is a disadvantage to the cooling in the vessel
since more work must be done encounter to this heat gain(Crawley, Preston, & Tyler, 2008). In addition,
torque must be applied on the agitator shaft so as to overcome the viscous and frictional forces imparted
on the impeller’s blades by the vessel’s fluid(Rao, 2009).
To calculate the power of an agitator, you need to know the viscosity and density of the fluid, the
diameter of the stirrer and its speed of rotation(Coulson 2011).
Design Parameters
Calculation of volume
Average densities for chemicals
Chemical Average density
Aspirin 1.04 g/cm3
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Acetic acid 1.049 g/cm3
Sulphuric acid 1.81 g/cm3
Acetic anhydride 1.08 g/cm3
Volume of; aspirin = =2.2434 m3
Acetic acid = = 0.9980 m3
Acetic anhydride = = 0.43368 m3
Sulphuric acid = = 0.1556 m3
Total volume required =2.2434 + 0.9980 + 0.43368 + 0.1556
=3.8307 m3
Overall density/specific gravity of the mixture is calculated from the component densities and is found to
be 1078 kg/m3(Crundwell 2008).
For a cylindrical crystallizer the ratio of height, to diameter 1.1333:1
This is also known as mixer height and diameter(Kle 2006).
. Hence = 1.1333
Volume =r2h =h
Substituting for h, = ×1.1333 = 3.8307 m3
=1.627 m or 1627 mm and height = 1843 mm or 1.843 m.
Calculation of baffle width
In baffle design, viscosity is an important factor for consideration as it determines whether flow could be
laminar or turbulent. For our case, it would be appropriate to assume turbulent flow in the mixer(Woo
2007). For Metric standard the baffle width to mixer diameter ratio is 1:10(Rao, 2009).
For =1.627 m or 1627 mm, baffle width w =1/10 = 0.1627m.
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Calculation of baffle height
Baffle height is determined by the overall height of the mixer, starting from the tangent line at the bo om
to the top(Silla 2003). A sufficient clearance is considered to avoid the formation of vortexes at the ends.
An appropriate ratio of 9/10 for baffle height to crystallizer height gives the height of the baffle to be
1.659 m.
Calculation of wall thickness
The thickness of the wall is dependent on a number of factors central in crystallizer design process(Vu,
2007). First, selection of the material for the vessel is a very crucial step in design of the crystallizer. A
good conductor is essential for optimal heat transfer efficiency to be achieved. Secondly, walls of a
crystallizer should be thick enough to allow for support of its contents(Crundwell 2008). High strength
material or reinforcement is required in order to meet this need. Allowance for coolant jacket is the
greatest contributor to the overall thickness of the vessel walls. From standards, if the allowance for the
water jacket is 0.01 m then a thickness of 0.02m would be sufficient to meet all vessel design
requirements(Coulson 2011).
Stirrer/ impeller diameter
The function of the impeller is to mix the contents in the vessel. Assuming high viscosity and density for
our case, four blades will ensure a good mixing is done in the vessel (Couper 2005). Let the impeller
diameter be d and the diameter of the vessel is D(Ende 2011). Optimum mixing to be achieved when
ratio of impeller diameter to the vessel diameter 2:5(Sam Mannan 2005).
Vessel diameter D = 1.627 m
Stirrer diameter d = 2D/5
=2×1.627/5
= 0.6508m
Hence impeller diameter of 0.6508m will ensure event and optimum mixing in the vessel.
The stirrer thickness is about 19 percent of the stirrer diameter.
×0.6508=0.1264 m.
Power calculations
In order to run the run the agitator the power rrequire3d is given
P=
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Where D is the stirrer diameter and N is the speed of rotation
NP is power number sg is the specific gravity of the slurry
P=
Suppose we want to run the agitator at a speed of 20 rpm and a power number of 1E13 number is given
by;
P=
=661 wa s
Design
Performance measure of crystallization is measured based on the CSD and crystal yield(Tung 2009). The
parameters being measured are constrains on the system which is mainly the supersaturation level and
the size of the vessels(Silla 2003). The two parameters are related to each other (Coulson 2011).
Mass and energy balance in the crystallizer
Energy balance around the crystallizer:
CRYSTALLISER
1 atm
273 K
Aspirin (Liquid)
Acetic acid (Liquid)
Acetic anhydride (Liquid)
Sulphuric acid (Liquid)
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Aspirin (Solid)
Acetic acid (Liquid)
Acetic anhydride (Liquid)
Sulphuric acid (Liquid)
363 K
For the components entering the crystallizer they are cooled from 363 K to 273 K. We will use the
following equation
Q = m x Cp x ∆T.
Q = heat energy
M = mass / molar flow
Cp = specific heat capacity
∆T = change in temperature
Q for Crystallizer Inlet:
Aspirin:
Q = to be calculated
M = 3140.783 kg/ batch =17.449 kmol/batch. We will use the molar value since we want the units to cancel
to KJ / batch
Cp = calculated using the equation given
We will use a Treference value of 0°C (273K) for calculating the change in temperature. The inlet
temperature of the crystalliser is 90°C
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Therefore ∆T = 363K –273K
Cp at temperature: 363K
-409.886 + (3.7262 x 363K) + (-7.08E-03 x 3632K) + (4.91E-06 x 3633K)
= 244.66 J / mol.K
Q = 17.449 kmol/batch x 244.66 J / mol.K x (363 –273K) x 1000 mol/kmol
= 384216.5 KJ / batch
Acetic acid (by product):
to KJ / batch
-18.994 + (1.0971E+00 x 363K) + (-2.892E-03 x 3632K) + (2.9275E-06 x 3633K)
= 138.206 J / mol.K
= 217040.08 KJ / batch
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Acetic anhydride:
to KJ / batch
71.831 + (8.888E-01 x 363K) + (-2.653E-03 x 3632K) + (3.3501E-06 x 3633K)
= 205.125 J / mol.K
= 84774.06 KJ / batch
Sulphuric acid catalyst:
M = 281.6296 kg/ batch = 2.873 kmol/batch. We will use the molar value since we want the units to cancel
to KJ / batch
26.004 + (7.03E-01 x 363K) + (-1.39E-03 x 3632K) + (1.03E-06 x 3633K)
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Cp at temperature: 363K= 147.301 J / mol.K
= 38087.62 KJ / batch
Q for Crystalliser outlet:
Aspirin:
to KJ / batch
We will use a Treference value of 0°C (273K) for calculating the change in temperature. The outlet
-409.886 + (3.7262 x 273K) + (-7.08E-03 x 2732K) + (4.91E-06 x 2733K)
= 179.6 J / mol.K
= 0 KJ / batch.
Energy balance
= 384216.5 KJ/batch
=217040.08 + 8477.06 + 339904.76
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=339904.76 KJ/batch
Net heat transfer is given by; 384216.5 – 339904.76
=44311.74 KJ/batch
Temperature is to be dropped from 900 to 00 and 44311.74 KJ of heat is to be removed.
Mass and energy balance in the chemical engineering design for the crystallizer is calculated from the
mass transfer; mainly the crystal yield and the heat loaded to the crystallizer(Crundwell 2008).
The overall mass balance is therefore wri en as
Mlo = M1f + Mcf + Mg + VR
Mlo is the initial mass of the seeds crystals
M1f mass of the feed
Mcf mass of the crystals
Mg mass of the by products
VR is the volume
The overall energy balance is given by
217040.08 KJ / batch
is enthalpy of the cooling
hc is the enthalpy of crystallization
Cp specific heat capacity of the solution
The calculations are on the condition of constant specific heat(Wan 2005).
For the cooling process and in the formation of the crystals, the following formula was applied
Mcf =MnR(Co-Cf)
1-Cf (R-1)
R is the universal gas constant which is 8.315Jmol-1K-1
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Therefore
From the equations the crystal yield can be estimated if the solubility of the components is known(Ende
2011). The equation does not consider the effect of nucleation, primary and the secondary. If the
nucleation is considered then the CSD can be estimated in someway(Nikrityuk 2011).
CSD prediction(Coulson 2011).
Prediction of the CSD in a batch crystallizer reactor can be done by the Mcabe’s law; “∆L law.” Analysis
by ∆L law is based on a critical assumption of the behavior of the crystals formation feature(Shioiri,
Izawa, & Konoike 2010 ). It is assumed that the crystals have the same shape throughout. The crystal
growth in the process is invariant and that the crystallizer size does not affect the structure of the crystal
formed; the primary nucleation or rather the classification of the size(Crundwell 2008). The relative
velocity of the liquor and the crystal is assumed to be constant(Vu, 2007).
Basically the calculations are based on the crystal size and the number of seed put in the crystallizer. Ns
and Ls dNp and Lp
∆L is the increment in then crystals which can then be integrated to obtain
Ls is the nuclear size
M1 is the mass of the feed
∆L and CSD can be evaluated if the Mp is known. The evaluation can be done the temperature range of
90 to 0 degrees Celsius(Rao, 2009).
Nucleation can happen at any supersaturation level even at the even that the supersaturation is low the
secondary nucleation still occur.
This implies that
Where Mcf is the crystal yield
==0.04717, the amount secondary nucleation.
A reasonable size of crystal in the yield must be accounted for. The number of crystals formed can be
obtained with the mass crystallizer reducing the crystal size.
Population balance
CSD is calculated from the Kinetic data though the crystal breakage and the agglomeration cannot be
considered in balancing the population(Sam Mannan 2005).
The population mass balance can be calculated from
Generally the nucleation depends on supersaturation whereas temperature is of li le importance in the
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growth of the crystals(Azadani 2007).
Mechanical design
.High strength material (steel) 109 MPa is enough.
Good conductor of heat and electricity is appropriate for water jacket as well as the inner heat transfer
area(Couper 2005).
Design Consideration
In the design of the crystallizer, there are a number of important elements which are considered to
ensure the design is of high quality. The size of the crystals in the crystallizer is one of the major
elements being considered. The crystals being manufactured are meant for a pharmaceutical application
thus some conditions over specification is considered(Rangaiah & Kariwala 2011). The crystals formed
rarely resemble each other mainly in symmetry about the centre, the plane and the axis
geometry(Richardson, Coulson, Harker, & Backhurst 2002). The crystals adopt some faces which can be
described in the x, y and z axes. Generally they form a characteristic feature which is crucial in the design
of the crystallizer(Barbosa-Póvoa, Matos, & Matos 2004).
Habits of the crystals
Crystals develops some shape which is proportional to the shape being formed on each side of the
crystal. The idea of heterogeneous development of the crystals has been applied in Chemical engineering
design mainly on the eve of growing the design. It was suggested that the shapes formed due to
equilibrium were basically due to the free energies the crystal areas(Crundwell 2008). This was offered in
the BFDH theory. Growth of crystals using the crystal modeling where prediction the shape of the
crystals is more sophisticated than it was before. Substances exhibit some different forms which are then
essential in determining the growth of the crystals. The habits which the crystals exhibit are affected by
the type of solvent in place and classified with the way the crystals grow.
In the manufacture of the pharmaceutical products, it is essential to apply crystallization process from
the simmerisation(Coulson 2011). The enantiomers are separated by crystallization process. The chemical
structure of the crystals applied in the process is essential in the manufacture of high quality products.
Crystals in the pharmaceutical sector have been essential in the manufacture of the pharmaceuticals. The
crystallization method of separation of the crystals is enantiomer pairs. The enantiomer pairs involves
some case of the mechanical development of the crystals which mainly the conglomerates. The structures
given should be considered as being separated in the physical means in which racemecrystal structure
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are formed.
Defects in the crystals
The crystals formed at a temperature which is above the absolute temperature have some defects in the
way the structure is presented(Silla 2003). The la ices are occupied by a regular organization of the
crystals(Nikrityuk 2011). Basically the organization results in the formation of atomic structure leaving a
vacant position for the impurities to occupy thus the purity of the crystals is then put to question. The
line defects which are essentially the major force behind development of defects in the crystals can be
classified as the screw dislocation and edge dislocation. The defects are essential in development of
secondary nucleation process(Couper 2005).
Characteristics of the particles formed
A solid appearance of the products is usually affected by the crystals’ structure. Basically the crystals
formed in the crystallization process are broken down in other physical process or the surface
development is done to ensure sizeable tablets are manufactured. The objective of the crystallization is
not only the separation process but also the formation of the crystals which have specific characteristics
that are essential in the final production of the aspirin as a finished product(Barbosa-Póvoa, Matos, &
Matos 2004). The shape and other characteristics of the crystal are the basis for the design of the
crystallizer mainly affecting the volume, the time taken in the crystallizer and the products(Crundwell
2008).
Shape of the crystals can be used in the calculation of the volume of the crystals. Basically the shape
factor aid in the calculation. The shape factor gives the relationship between the surface area of the
crystal and the volume of the crystal. The characteristics of the dimensions relating to the shape factor
are specific(Shioiri, Izawa, & Konoike 2010 ). The surface shape factor is the relationship between the
outer areas in comparison with the dimensions. It relates with various shapes of the crystals. The volume
factor relates with the shape of the crystal in relation to its volume(Silla 2003).
Particle size distribution
The crystals obtained industrially have different size and range within some limits however some sizes
are dominant over the other sizes. The size distribution follows the normal distribution curve and can be
calculated using the statistical procedure and method(Ende 2011). The mean size of the particles can be
calculated by assuming two numbers representing the whole population of crystals in the analysis(Vu,
2007). Basically classification of the groups can be done in two ways; the property of the mean size
(weight is defined and the mean calculated from the population while the mean property size is based on
fiction about the size of particles to be calculated) (Shioiri, Izawa, & Konoike 2010 ). All the essential
properties such as the size, the mean volume, the surface areas and variation are all calculated in the
same way to extract the exact qualities of the crystals being processed(Coulson 2011).
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For this design, it is considered that the external properties does not exit the internal balance as it
requires more calculation if the external features has some effects on the internal design(Theodore &
Ricci 2011).
The effects of the size distribution can be witnessed in the separation of the solids and the liquids formed
in the crystallization process. A larger distribution of the particles enables a wide packing of the particles
thus enabling the materials handling more effective. The challenge in estimating the size is basically the
size distribution which is mainly because the sizes of the crystals formed may not be of the same shape
through out thus estimating the void may lead to errors(Silla 2003).
Generally in the design of the crystallizer, the factor of the crystal shape and size has been considered as
one of the most important factors which have been taken into account in consideration of the overall
volume design and the design of a control system(Seliger Khraisheh, & Jawahir 2011).
Mixing in the crystallizer
The solid formed in the process of crystallization tends to se le in the bo om of the crystallizer(Woo
2007). The solid se ling at the bo om of the crystallizer prevents effective heat transfer from taking place
and also the quality of the crystals formed may be compromised in the process. An agitator is essentially
important in ensuring the solids do not se le at the bo om of the crystallizer and also the heat transfer to
the fluid in the crystallizer is evenly. During the mixing, it is possible that the mixture formed a vortex
therefore introducing swirling of the fluids. Swirling does not allow the fluids to mix well therefore, not
required in mixing. To solve the problem, the baffles are included in the design. Baffles are designed to
interrupt the formation of swirling which result in vortex formation. Mixing will be evenly and the
vortex formation will happen as well as se ling of the crystals at the bo om of the crystallizer.
In operating the agitator, it is necessary to use an agitator at a certain speed and with the ability to create
enough suspension of the solids. The speed however should not cause a collision in the walls of the
crystallizer which may result in the wearing of the machine. A relative average speed would be essential
in achieving optimum mixing of the slurry considering more solids are formed as the mixing
continues(Woo 2007).
Mixing in the crystallizer is not expected to be turbulent thus there is no expectation of the eddy currents
or other factors being displayed by the turbulence flow.
Simulation of the fluid mechanics in the crystallizer
The flow of the fluid in the crystallizer depends on the shape of the vessel. The dynamics of the fluids in
the crystallizer may not be understood easily without the aid of Computational Fluid Dynamics. CFD
gives both the dynamics of running the flow in the process and after the process analysis. The data
obtained from one process can be used to develop another process or rather be used in the correction of
error in the control of the crystallizer. Basically the operations within the crystallizer especially when
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stirring is very important in the analysis of the process thus in doing so, using the modeling process, it
creates an important development that would ensure a more precise production process is
followed(Couper 2005). There are a number of simulations that can be done to obtain an important data
to impose on the process(Crundwell 2008). These are some of the common modeling used in the
simulating process. There is the momentum resource modeling and the slide modeling(Vu, 2007).
Among the two modeling, the most important one is the slide modeling basically because it presents a
more detailed and precise pa erns of flow in the crystallizer. The simulation doesn’t cater for the
impurities in the Aspirin crystals which about 5 percent of the total solids formed. The flow pa ern and
the solids formation is also an important feature being accounted for in the simulator. Since the flow
pa erns are known to be difficult to study in a reactor, it is necessary to use the chemical engineering
models which are more precise in the outcome. The macromixing and the micromixing are studied all
through with the aim of coming up with one of the most important models in the design and control of
the process of crystallization(Silla 2003).
The macromixing is the study of the process in consideration of the ideal performance of the crystallizer.
Basically it would be difficult if the process’ operations within the crystallizer would be estimated using
the residence time and the distribution of the elements of the fluid dynamics in the system(Coulson
2011). The study using the model helps in development of the mathematical models which are essential
in the design of the control system for the crystallization process(Nikrityuk 2011). Basically the modeling
considers the feed to the system and the output. From the information obtained from the mixing inside
and the flow is important in developing the overall process of modeling(Azadani 2007).
In modeling the micromixing, it is possible that the process undergoes modeling which essentially
important in the reduction of the eddy current developed during the mixing process(Crundwell 2008).
Basically the micromixing model is in operation with the fluid entering the system being the main focus
whereas the rest of the operation is of li le importance in the simulation using the micromixing model.
Some of the parameters being viewed in the process though are not considered in the micromixing.
Basically the aim of the modeling involving mixing is mainly to study the impact of mixing in the
reaction or rather the crystallization process(Richardson, Coulson, Harker, & Backhurst 2002).
Mechanism Models
There are a variety of models which have been used for simulating the crystallizer both the physical
models and the mechanism models. The physical models are responsible development of a more
sophisticated process which considers the whole process of mixing. The major assumption in conducting
simulation is mainly achievement of evenly mixed mixture. Through the mass balance, the population
count and the mass balance can be obtained. The numerical figures pertaining formation of the crystals
can be obtained from the balance of population and the probabilities of the crystal growth using different
parameters. Basically the simulation is essential is providing operation of the crystallizer in a more
precise mode which is essential in the design of an optimum operating crystallizer. From the
simationation, various parameters under control can be programmed using the values obtained from
simulations. The crystallization of aspirin is a simple separation process where the process has to be
conducted in a moderate mixing with less turbulence. The crystals formed from the process are 95% with
some form of acetylene and the rest aspirin. Therefore the conditions for the operation depend mostly on
the simulation for the system to be programmed and ensure the control system is precise. The design of
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the crystallizer itself is also important in developing an optimum condition. For instance the effect of
hard mixing or improper placement of the mixer still affects the performance of the crystallizer and the
quality of the crystals produced at end of the process.
Scale up
Various processes in the chemical engineering design require a scale up in order to have a maximum
operation. Some of the major scale up processes is the constant speed of the stirring in mixing, the speed
of the tip of the mixer is also essential in the performance of the crystallizer. It ensures a constant shear is
obtained in the process basically it is expected to offer an optimum mixing which in turn cool the slurry
in a faster rate. This is done in the estimating the effect of the shear force on the fluid but there is direct
measurement of the effect. The constant power input volume is another parameter which can be used in
ensuring that maximum operation is reached(Silla 2003). The scale up pa erns in mixing can be difficult
sometimes especially when the stirring needs the conventional scale up(Crundwell 2008). The process
has been tried practically but a convention on it have not been proven rather the convention on various
parameters have not been of importance in the process. The difference between the time taken by various
parameters when the constant power input volume is applied complicate the scale since without the
conventional definition of the scale, it becomes difficult for the engineers to use the scale up. Basically the
microbehavior pa erns in the crystallizer are essential in developing the major outcome of the process
thus it is important to consider the li le effects of the convention failure and other parameters that would
adversely affect the output of the system(Sangwal 2007). Thus a good scale process results in a
production of quality crystals(Crawley, Preston, & Tyler, 2008).
Summary
The design of the batch crystallizer is mainly based on equations which are developed from the cooling
process. All the performance equations for the batch crystallizer start with the McCabe ∆L law. The ∆L
law is essential in predicting the crystal size and in development of the nuclear which is essentially used
in developing other equations for use in development of system equations(Barbosa-Póvoa, Matos, &
Matos 2004). The population balance can be obtained using the mass balance and the prediction of the
kinetics of the crystallization. The kinetics can be obtained through the use of the controlled parameter
and the application of seeding which basically essential during the crystal growth control. For the
crystallizer to form crystals of high quality, the supersaturating has to be maintained in the metastable
condition throughout the process(Kle 2006). This is achieved by application of vortex cooling or rather
the control of the cooling pa erns such as controlling the rate of cooling of the crystal and sometimes
destruction of the crystals to ensure proper crystal size is achieved.
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HAZOP (Hazards and Operations Analysis)
Hazards and operations analysis is a result of the theory that the problems in the operations failure is
mainly caused by the failure of the process design and the inability of the system to cope with the
challenges during the operations(Coulson 2011). Basically these problems can be identified from the
control system of the Piping and the instrumentation diagram. In exploration of the problems that might
have been caused by the faults in the design or any other problem developed during the processing of
the materials can be obtained mainly from the human analysis of the process. Basically it is important for
the engineers operating the crystallizer to have an assessment of the fault in the system in order to come
up with the main challenge causing the fault in the process. The major techniques that can be used in the
analysis are brainstorming and the qualitative risk assessment tool. Other method includes prediction of
the faulty of the system based on the experiences obtained in the past while operating the
process(Chianese & Kramer 2012). The engineers ought to come up with a solution at the end to ensure a
proper engineering process is precise and good quality products are process to the final products(Silla
2003).
The HAZOP is mainly used in the assessment of any crystallizer to ensure that the design specifications
are up to the standards stated by the manufacturer and according to the safety standards set by the
bodies involved in standards for instance the ISO standards. The operating conditions of the crystallizer
are also analyzed to ensure the conditions are suitable for a safer environment during working. In
addition, the machines have to be maintained to ensure a proper procedure is duly followed(Letcher
2004).
A part from the effects of the machine failure in the crystallization process, the control of the machine
might be the failure itself. Through the brainstorming process, it is necessary to consider the
instrumentation and ensure that it is well coordinated. The operational modes such as the starts of the
control, the normal operation and the emergency response of the control system.
HAZOP has a wider importance of ensuring the degree of safety in the industry is high. Errors resulting
from human activity in a plant can be recognized easily. Measurement and other procedure in solving
problems can be avoided(Vu, 2007). Instances such as the production of poor quality crystals may not be
identified through measurement but the effect of brainstorming brings out the important aspect of theory
of the behavior of crystal formation(Branan 2005). A comprehensive activity on the performance of the
crystallizer is then analyzed based on the brainstorming that the tools ready in place for the use in the
analysis of the process(Sangwal 2007).
The set back in using the HAZOP is the lack of a strategic means of directly measuring or conducting the
system analysis(Chianese & Kramer 2012). There is no particular process procedure involving the works
and the control of the team conducting the brainstorming process of the use of HAZOP thus the
proposed improvement by the team have no direct solid basis for the assurance of the process(Houson
2011).
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HAZOP process
HAZOP process can be divided into four phase(Coulson 2011). The first phase is the definition of the
problem, the objective of HAZOP and selecting of the team capable of realizing the objective of the
group.
Preparation of the process involves the procedural plan of the areas of interest, how the data is collected,
the time taken to complete the assignment and the schedule to be followed. After the examination, it is
crucial to concentrate on the next phase which is the examination phase.
In the examination process, the problem to be solved is defined and mentioned. Various design
intentions are sorted out to allow the process of reviewing the optimum operating conditions which are
then essential in the process of HAZOP. The elements selected are received stepwise with guidance to
ensure the problem is identified correctly. The problems caused by the operations resulting from the
faults in the machine and the environment(Silla 2003). The areas under investigation must be reviewed to
find if they have a significant effect on the whole process(Jones 2002). In the course of examination, a
strategy is taken mainly on the protection that can be offered to the machine, future detection of such
faults and the characteristics of a system undergoing the same problem. In the course of the analysis, a
remedy strategy can be put in place to ensure the whole process of may not be necessary stop in the
account of trying to solve a fault. The remedial strategy heavily depends on the nature of the challenge
and the magnitude. Once all the strategies are set, it is important that a consensus is set out to ensure that
everyone agrees with the proposed changes on the element. The same can be done for all the elements
under investigation.
After the investigation on the process, the findings of the investigation are taken into account. The
activity involves the documentation of the findings. The compiled document is then signed off and
documented. The products of the investigation are put into the practical during the follow up process. In
the case of unsatisfactory outcome during the follow up, it is necessary to rectify the fault in the process
and come up with the conclusion of the whole activity, where a report is finally published.
In order to conduct a successful HAZOP design, there are some words which are essential in the
brainstorming process. Words that quantify a situation are commonly used to ensure a thorough analysis
is taken into account.
In summary the objective of the HAZOP is mainly to apply the brainstorming method in solving the
industrial challenge but with the use of professional engineers in the course. Engineers have some
process to follow when solving technical problems occurring in a plant but in the case of HAZOP, the
more radical analysis is carried to ensure the process is completely taken into the account of being the
part of the solution of the industrial challenges(Branan 2005). The major parts of the HAZOP process are
the process of evaluating the various parameters which are essential in the analysis and then taking a
proper use of the guiding words with the parameters(Crundwell 2008). Some of the words commonly
used for instance are: No, Less, More, Other Than As Well As, Reverse among other essential words in
the design(Silla 2003).
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Piping and Instrumentation Diagram (P&ID)
The P&ID is an important diagram during the design and when applied in the field. Basically the
diagram is essential in showing the piping system and the control of the plant and in specific the
Crystallizer(Coulson 2011). Some of the major components in the P&ID of the crystallizer are basically
the design specifications as the installation of the instrumental and control, the flow of the process,
various components of the machine which are important in the process of accomplishing the
requirement for the processing. The use of the valves, the level of quality, the subsystems the sequence of
the plan and other important physical appearance of the process. P&ID is useful in ensuring the
orientation to the plant operation is useful to the users and the newcomers. Basically an overview of the
system will be simplified and the person might be in a position to come up with a be er understanding
of the system(Kle 2006).
The major focus in the design of the P&ID is to ensure the major parts of a system are displayed in a
be er and simpler manner that can be used for the interpretation of the overall control and management
of the plant. Location of some of the components of the plant is easier(Sam Mannan 2005). Also in the
maintenance process, it is easier to tackle the problem faced
The major components in the crystallizer P&ID are the valves, the control systems, and the essential
pumps and the power to the crystallizer. The process and the flow of cooling fluid on the crystallizer and
other major parts(Silla 2003). Since the design of a chemical plant may not be in a position to mention
most parts of the words, universal symbols which are widely used in engineering. Some of the examples
are the pipes, the mixing vessels the pump, a mixer with a jacket, valves the control and any other
essential part that may be essential in developing the system. It can be noted that the most important
components of the design are mainly displayed in the form of symbols which are universally acceptable
by the engineers and can be acceptable everyone using the instruments in the design (Coulson 2011).
Basically the difficulty is developing the P&ID is in the design and simulation of the flow and the use of
various parameters which are essential in the crystallizer for instance (Theodore & Ricci 2011).
Figure 2 The piping and instrumentation diagram for the feedstock and product in the crystallizer
Figure 3 showing the piping and instrumentation diagram for the crystallisation control system
The legend is shown below
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Control and instrumentation
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Control diagram
The figure is a control diagram for the crystallizer.
A is crystallizing cylinder/vessel indicating the mixture and the baffle; B, heater; C, heater; D,
thermometer; F, recording control; G, relay; I, coolant pump; J, coolant tank; L, coolant exit; K coolant
entry point; H, temperature controller.
Controlling the the crystallizer involves the use of an immersion heater labeled B as well as the
circulating water cooling the system. A computer is mainly used and a program that ensures all the
optimum conditions are considered as approached in the design.
Maintaining the crystallizer contents in the transient supersaturation is basically the most crucial activity
being monitored by these control parameters.
Batch crystallizer control and instrumentation
Introduction
The design of a batch crystallizer is mainly a consideration of the size of the equipment, the operating
conditions and measurement of the performance. The size of crystallizer is determined by time spend
and the cooling rate (occasioned by suspension of solids). Operating conditions depends on the cooling
curves formations and times spent in the batch. Basically time is important since it ensure the correct size
of crystals is reached. The quality of the products is usually measured on the amount of crystals formed
and Crystal Size Distribution (CSD). A part from the ideal design, other factors such as the
supersaturation affects the design of the equipment.
The major parameters in the control of the crystallizer are the feed that is the feed for the batch process
should be in the ratio stated in the design. The operating condition for the feed also has a hand in
control. The feed is expected to reach the crystallizer a temperature of 90 degrees Celsius from the batch
reactor. The temperature has to be reduced to zero degrees Celsius. The mixing process should be
moderate to avoid turbulence which might disturb the crystal from forming(Houson 2011). All the
conditions affect the most important parameter which under the control of the engineer. The quality of
the crystal is considered the output. From the chemical engineering design, the crystals formed should
have some specific shape and size from them to be considered quality. From modeling of various
mathematical models, the control of the parameters in the crystallizer design can be obtained and have
an effective control of the crystallization process(Silla 2003).
Mass and energy balance in the crystallizer includes: yielding of crystals and the heat load (Crundwell
2008). The mass balance is based on the population distribution. Among other factors the mass balance
can be obtained through the nucleation rate calculations. The mass balance of the population is
important in enhancing the control of the parameters in the crystallizer(Richardson, Coulson, Harker, &
Backhurst 2002).
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Control
The most important parameter to consider in the crystallizer control design is the supersaturation. The
parameter is responsible is responsible for the scaling of the heat transfer areas(Letcher 2004). It is also
responsible for the nucleation process and the CSD. When the natural cooling is considered in cooling
slurry in the crystallizer, the level of supersaturation is rapidly increased thus slurry reaches metastable
state in the early stage of crystallization. Basically the resulting crystals formed are finer and of poor
quality(Branan 2005).
When seeding a controlled cooling is applied, the desired crystal size is then obtained. In this case the
cooling rate is under control therefore a metastable state is maintained throughout the process of
nucleation. Also the CSD and large particles are formed with the effects of fouling in the heat transfer
areas being catered for. Basically the cooling in the crystallizer is an important factor and has been
subjected to mathematic modeling to ensure a good controlled system is established. Secondary
nucleation can occur at metastable state therefore a mass balance for the crystallization can be obtained
by taking into account the control parameters(Woo 2007).
=.+
From the mass balance equation, a correct graph equation can be obtained. In comparison with the
natural cooling, the graph obtained from the equation forms a convex curve which is a contrast to the
system under natural cooling.
Operating at Maximum control
Though the main aim of nucleation controlling cooling in crystallizer is to obtained large size crystals,
natural cooling forms the largest crystals overall(Coulson 2011). The problem is because the formation is
uneven. Nucleation happens at some point in the process. Basically that complicates the process since the
crystal growth integral cannot be easily estimated with the time taken in the batch. Batch process can
only be defined in terms operating at optimum over a period of time and not an instant performance.
In the case where the graph of the cooling rate between the natural cooling and the controlled cooling is
drawn, a natural cooling shows a rapid temperature drop whereas controlled cooling evenly and slowly
drop(Jones 2002). The principle of maximum cooling is used.
The variables for the cooling rate can be stated in the principle of maximum cooling. The principle is
used in the design of a control system for the crystallizer.
Where H is the Hamiltonian function, x is the vector and u is the control variable. The variables are
mainly the size of the crystals while the control parameter is the temperature of the solution. Since the
aim of the process is to maximize the size of the crystals, an ordinary deferential equation is obtained for
the process(Barbosa-Póvoa, Matos, & Matos 2004).
From a graph dawn from the formula, it can be deduced that maintaining a constant temperature
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throughout the operation in the crystallizer maximizes the final outcome of the particles size and the
CSD. It prevents an early nucleation and maintains an optimum operating condition(Silla 2003).
Optimization is not ideal however the process has maximum operating conditions.
Control and Instrumentation
Control in the crystallizer is mainly done by the immersion heater as well as the circulating water cooling
the system. Water circulates in the crystallizer through a draft-tube in the walls of the crystallizer and a
controller which is mainly computer programmed to ensure the set point is not exceeded. Cooling curves
are observed and any deviation from the predicted curve is considered a fault in the process.
The data obtained from experiment done by researchers’ shows the importance of the controlled cooling
as compared the cooling process as result of natural cooling. Maintaining the slurry in the transient
supersaturation is basically the most crucial activity being monitored by the control parameters. In a
situation where the transient supersaturation is kept low, the crystal size is likely to be below the average
required size. Therefore it is important to consider the shapes the graphs drawn.
While doing the programming of parameters for control, the projected size and shape are preset. The
preconditions such as the determination of the seeding in the crystallizer are basically helpful in the
programming of the system (Coulson 2011). Programming is based on the theories of seeding, the
equations on the population is also balanced and programmed to cater for variation to acceptable limits
(Houson 2011).
Feedback controllers
In the control system, there is either a positive or a negative feedback. Whenever there is a negative
feedback, the controllers are used to rectify the arising problem. In the case of positive feedback, the
system will just operate in the same condition. The integrated controller is an important element in
control since the controlled variables are brought back to the set point so that the offsets are rectified
(Crundwell 2008).
Economic Appraisal of Process
The main purpose for installing a chemical plant is to gain profits. In order to achieve the goals and
objective of the project, it is important that the chemical plant is taken into account the cost of installation
and the start capital before projecting the profits expected from the process. The highest cost in the
project is encountered during the installation process but the working capital is a bit cheaper to operate
(Coulson 2011).
In the economic evaluation of design in the Chemical engineering, the working and the fixed capital are
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considered. The fixed capital includes the design, initial engineering activities and the construction of the
plant. Installation of equipment for the process, instrumentation and control installations, piping and
other land development. This kind of investment doesn’t offer the return to investment but can be
disposed at the end of business as scrap. The working capital is needed to start up the business. For this
case, the working capital is mainly the cost of the raw materials, inventories, and other charges which are
required to start up a business(Branan 2005). The working capital is recovered in the course of the
business the working capital is about 5 % for the products produced single while 30 % for the products
produced in a varieties. For the case of Aspirin manufacture the product is a single but the process might
be a bit complex thus the estimate of the working capital is projected at 10 %. A typical pharmaceutical
manufacture projects the working capital at 10% of the fixed assets. The percentage is arrived at by
pu ing into considerations the complexity of the process of manufacturing the pharmaceutical products
(Silla 2003).
Since the source of estimation of the cost is from an historical data, it is possible that the data may have
been escalated for sometimes thus the index for the calculation of inflation is obtained from a published
data as well the index of the calculations
Cost in the current year= cost in the year published ×
Various components of the process have some specific indexes therefore they are broken down into
various components of the plant applied in the composite index application. The data obtained was from
the process engineering indexes which cater for the cost indexes for all the chemical plant costing
(Crundwell 2008).
The fixed cost for the plant will be the building the plant housing or the civil work, offices for the staff,
the control room, power room, installation of electricity within the plant, preparation of the site for the
business to set up(Barbosa-Póvoa, Matos, & Matos 2004). The store for the raw materials as well as the
finished products should be included in the calculation of the total cost of the installation and other
auxiliary requirement for the plant design to be completed ready for the operation (Silla 2003). All the
requirements are ensured that the index for the price is multiplied to ensure the cost of installation is
well project and avoid too much deviation during the installation of the project (Coulson 2011).
The annual costing of the capital charge can be calculated from the overall cost of one time through the
annual charge ratio (Sam Mannan 2005).
Cost of establishing a similar facility in china
Plant capacity = 10000 ton of acetylsalicylic acid
Plant costs = 175,000,000 USD
8.1.1 Rapid Capital Cost Estimate – Historical Cost
The costs are estimated using the cost of another established factory.
Estimating the capital costs using this method
36 of 43 12/10/2015 6:12 PM
(C2 / C1) = (Q2 / Q1)n
C2 Capital cost of the project with

capacity Q2
C1 Capital cost of the project with

capacity Q1
n Value of Index
The cost and capacity of se ing up an acetylsalicylic acid in china is shown below
C1 Capital cost of china $150 million
C2 Capital cost of UK £
Q1 Capacity in China 10,000 tones
Q2 Capacity in UK 5,000 tones
n Value of Index 0.85
Rearranging and substituting the values in equation 1, we get C2
= 83 million $
Converting dollars to sterling pounds
1$ = 0.653£
= 83 × 0.653 = £ 54 million
37 of 43 12/10/2015 6:12 PM
Location factor
It is cheaper to setup a factory in China as compared to the UK. Using a factor of 1.25%
1.25 × £ 54 million = £ 67.5 million
Raw materials costs
Cost of acetic acid
Cost of 1tonof acetic acid = 650/ T
Ton used per year = 5000 T/yr
Cost per year = 5000 × 650
Cost per year = $ 3 million
Cost of sulphuric acid
Cost of 1ton of sulphuric acid = 95/ T
Cost per year = $ 475,000
Cost of salicylic acid
Cost of 1ton of salicylic acid = 40/ T
Cost per year = $ 200,000
Total materials cost = 3 million + 475,000+ 200000= $ 3,675,000
Total raw materials cost in £ = $ 3,675,000 × 0.653 = £ 2,399,775
38 of 43 12/10/2015 6:12 PM
References
Azadani, A. N, 2007. Flow enhanced protein crystallization at the air/water interface. Texas: ProQuest.
Barbosa-Póvoa, A., Matos, H., & Matos, H, 2004. European Symposium on Computer- Aided Process
Engineering-14: 37th European Symposium of the Working Party on Computer-Aided Process
Engineering. ESCAPE-14, (pp. 1200-1780). Lisbon: Elsevier.
Branan, C, 2005. Rules of thumb for chemical engineers: a manual of quick, accurate solutions to everyday process
engineering problems. New y: Gulf Professional Publishing.
Bröckel, U., Meier, W., & Wagner, G, 2007. Product Design and Engineering: Best Practices. Munich:
Wiley-VCH.
Chianese, A., & Kramer, H. J, 2011. Industrial Crystallization Process Monitoring and Control. Chicago: John
Wiley & Sons.
Coulson, J. M, 2011. Chemical engineering. Chicago: McGraw-Hill Pub. Co.
Couper, J. R, 2005. Chemical process equipment: selection and design. Arkansas: Gulf Professional Publishing.
Crawley, F., Preston, M., & Tyler, B, 2008. HAZOP: guide to the best practice for the process and chemical
industries. Texas: IChemE.
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Crundwell, F. K, 2008. Finance for Engineers: Evaluation and Funding of Capital Projects. New York:
Springer.
Du a, 2007. Principles of mass transfer and separation processes. New Delhi: PHI Learning Pvt. Ltd.
Ende, D. J, 2011. Chemical Engineering in the Pharmaceutical Industry: R&D to Manufacturing. New York:
John Wiley and Sons.
Ende, D. J, 2011. Chemical Engineering in the Pharmaceutical Industry: R&D to Manufacturing. New York:
Houson, I, 2011. Process Understanding: For Scale-Up and Manufacture of Active Ingredients. New York: John
Wiley & Sons.
Jones, A. G, 2002. Crystallization process systems. New York: Bu erworth-Heinemann.
Kle , T. A, 2006. Hazop and Hazan. Texas: IChemE.
Letcher, T. M, 2004. Chemical thermodynamics for industry. London: Royal Society of Chemistry.
Myerson, A. S, 2002. Handbook of industrial crystallization. New York: Bu erworth- Heinemann.
Nikrityuk, P. A, 2011. Computational Thermo-Fluid Dynamics: In Materials Science and Engineering. New
York: John Wiley & Sons.
Rangaiah, G. P., & Kariwala, V, 2011. Plantwide Control: Recent Developments and Applications. New York:
Rao, 2009. Fundamentals Of Food Engineering. Chicago: PHI Learning Pvt. Ltd.
engineering: Particle technology and separation processes. Texas : Bu erworth- Heinemann.
Sam Mannan, F. P, 2005. Lee’s loss prevention in the process industries: hazard identification, assessment, and
control, Volume 1. Chicago: Elsevier.
Sangwal, K, 2007. Additives and crystallization processes: from fundamentals to applications. Chicago: John
Wiley and Sons.
Seliger, G., Khraisheh, M. M., & Jawahir, I. S, 2011. Advances in Sustainable Manufacturing. kansas:
Springer.
Shioiri, T., Izawa, K., & Konoike, T, 2010. Pharmaceutical Process Chemistry. New York: John Wiley & Sons.
Silla, H, 2003. Chemical Process Engineering: Design and Economics. Vatican City: CRC Press.
Sinno , R. K., & Towler, G, 2009. Chemical engineering design. New York: Elsevier.
Theodore, L., & Ricci, F, 2011. Mass Transfer Operations for the Practicing Engineer. New York: John Wiley
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Vu, K. M, 2007. Optimal Discrete Control Theory: The Rational Function Structure Model. Chicago: AuLac
Technologies Inc.
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APPENDIXES
1. Cost Index for some equipment.
List of General Characteristics
Type of Size of Type of Typical products comments

equipment crystals solubility
Forced 30-150 Flat, , citric acid. Well visible

circulation normal/ operation.
inverted , 1, lactose. Usually large or
small operation.
Fluid 6- 65 Normal, , , ,, Salting at the

suspension flat wall is a
problem. It is
possible to
operate above
natural slurry
specific gravity.
Craft tube 6- 48 Normal ,, Low salting on

baffle flat the walls
Reactive 6 – 100 All ,, Destruction

type ability
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Surfaced 20 – Normal Possible to

cooled 150 operate above
slurry specific
gravity and is
suitable for low
temperature
operation.
Direct 6 – 48 Normal Paraxylene, , Salting on the

contact wall is li le, can
refrigeration run at low
temperature and
has no problems
with the cooling
on the walls.
Batch 20 – Normal, , Usually has

100 small capacity,
, Tri P.E simple
instrumentation
and is self
cleaning
Teflon tube 14 – 65 normal , Normally

designed for low
temperature
cooling
Air cooled 30 – Normal , Operate at

200 ambient
,. temperature and
is used where
minimal energy
consumption is
required
2. General characteristics for various equipment

types(Coulson 2011).
42 of 43 12/10/2015 6:12 PM
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1.0 Project Brief 6

1.1 Project Objectives 6

1.2 Project Plan 8

1.3 Technical Objectives 8

1.4 Personal Objectives 9

1.5 Techniques to Accomplish the Objectives 10

Design of a batch crystallizer 11

Chemical engineering design 12

Heat transfer area 13

Elements of a batch crystallizer 14

Baﬄe height and width 17

Calculation of baﬄe width 20

Calculation of baﬄe height 20

Calculation of wall thickness 20

Mass and energy balance in the crystallizer 23

Energy balance around the crystallizer: 23

Q for Crystallizer Inlet: 24

Acetic acid (by product): 25

Sulphuric acid catalyst: 26

Q for Crystalliser outlet: 27

Habits of the crystals 32

Defects in the crystals 33

Characteristics of the particles formed 33

Mixing in the crystallizer 35

Simulation of the ﬂuid mechanics in the crystallizer 36

HAZOP (Hazards and Operations Analysis) 40

Piping and Instrumentation Diagram (P&ID) 44

Control and instrumentation 48

Batch crystallizer control and instrumentation 48

Operating at Maximum control 50

Control and Instrumentation 51

Economic Appraisal of Process 52

A.Cost Index for some equipment. 62

B. General characteristics for various equipment types(Coulson 2011). 64

1.0 Project Brief

1.1 Project Objectives

1.2 Project Plan

1.3 Technical Objectives

The main technical objectives are;

1.4 Personal Objectives

1.5 Techniques to Accomplish the Objectives

In order to archive the set objectives, the researcher will;

Where the ∆Xo can be determined by

Design of a batch crystallizer

Chemical engineering design

Heat transfer area

Surface area of the baﬄes

=2(4) (1.659) (0.1627)

Total heat transfer area =18.84+2.16

Elements of a batch crystallizer

Figure: diagram showing the diameter and height of the agitator.

Baffle height and width

Figure, vessel height, baﬄe height and width

Average densities for chemicals

Chemical Average density

Aspirin 1.04 g/cm3

Acetic acid 1.049 g/cm3

Sulphuric acid 1.81 g/cm3