Student: Vagif Hajiyev

Lecturer: Javid Kocharli

Distillation Column

Abstract
Styrene monomer is the fourth largest chemical produced on an industrial scale and most ethyl-
benzene is utilized in styrene monomer production. The largest chemical produced on an
industrial scale is ammonia for fertilizer production, followed by crude oil refining, and then
ethylene by furnace pyrolysis. Styrene monomer has been manufactured commercially for
more than fifty years with advances in the key unit operation areas of reactor design and
distillation.

Introduction
One of the most important operation in the chemical and petroleum industry is the separation
of liquid mixtures into several components. It is sometimes referred to as fractional distillation.
It is one of the oldest unit operation processes. The technical publication of distillation was first
developed in 1957, however, distillation had been practiced for many centuries prior to this.
Distillation is one of the most common and widely used separation processes in the chemical
industry. However, it is also an extremely energy intensive process. It requires large amounts of
energy for both cooling and heating. 50% of plants operating costs are produced from
distillation. At present distillation is commonly used in the petroleum, chemical, petrochemical,
beverage and pharmaceutical industries. Distillation is a process which is important in the
development of new products and for the recovery and reuse of volatile liquids. A great deal of
research has been carried out into techniques of distillation due to the demand for purer
products and a persistent requirement of greater efficiency. When designing a distillation
column it is essential to consider process control. Many distillation columns usually operate
with the combination of many other separate units. The correct design of a distillation column
is not always a simple procedure as it is regarded as a specialised technology. Compared to
other types of processing equipment distillation columns have to be designed with a larger
range in capacity with single columns varying from 0.3 to 10m in diameter and 3m to 75m in
height. It is important that designers are able to provide the desired product quality at a
minimum cost but also at a constant purity. Distillation is usually used to separate liquid
mixtures into two or more vapour or liquid products which have different compositions. The
separation of liquid mixtures is dependent on the differences in the volatility between the
components. Separation is easier if the relative volatilities are larger. There are two major types
of distillation, this includes continuous distillation and batch distillation. In continuous
distillation the feed is supplied continuously. There are usually no interruptions however,
problems may occur with the column or surrounding units. This type is the more common of
the two types of distillation. However, in batch distillation the feed is supplied to the column
batch-wise. The column is charged with a batch and the distillation process is then carried out.
Once the desired task has been achieved the next batch of the feed is then introduced.

Process Description
The product distillation unit will be fed with Ethyl Benzene/Styrene mixture. The mixture fed to
the product distillation column is obtained from the bottom stream of the first multicomponent
distillation column. Within the product distillation column cooling water which enters the
condenser and steam which enters the reboiler is utilised.

Key Components
Before the design stage of a distillation column the designer must select the key components
which are to be separated. The light key is described as the component that is desired to be
kept out of the bottom product. The heavy key is described as the component that is desired to
be kept out of the top product. Usually it is relatively easy to determine which the key
components are. However, there may be situations in which close boiling isomers are present
so judgement must be used in their selection. The light key is described as the most volatile
component in the bottom product and the heavy key is described as the least volatile
component in the top product. In this case the light and heavy keys are as follows:

 Light Key: Ethyl Benzene (A)

 Heavy Key: Styrene (B)

Operating Conditions
It is assumed that the process operates at a steady state and the system is ideal. It is assumed
that the inlet temperature of the feed to the column will be at the boiling point i.e. ‘boiling
liquid feed’. The feed temperature is used as operating temperature.

Operating pressure at the top is often set just equal or above atmospheric pressure to avoid
any vacuum operation, unless the temperature at the bottom of column is limited by
decomposition, polymerization, excessive corrosion or other chemical reactions. In that case
vacuum operation is required.
In our ethyl benzene/styrene distillation tower vacuum operation is required to maintain a
temperature low enough to prevent styrene polymerization in the reboiler. For this, tray
spacing, weir height, pressure drop per tray should be in a standard vacuum operation ranges.
That is why, of course, all of these are considered below.

Process Equipment Design (T-402).

The design of a distillation column requires extensive research, careful calculations, and an
overall economic analysis. In this project, the distillation column for the separation of ethyl
benzene and styrene will be designed. The important parameters involved in the design of a
distillation column include column diameter, column height, types of tray, tray efficiency, weir
height and materials of construction.

The first step of the process for designing a distillation column is to determine the minimum
reflux ratio, and the number of trays required to obtain the desired separation. There are
several methods available for determining these design parameters for distillation towers,
including the FUG method and the McCabe-Thiele method. The FUG method is an analytical
approach, whereas McCabe-Thiele uses a graphical approach. Both of these methods have their
merits, and were both in the design of the ethyl benzene-styrene distillation tower.

Since the column is binary, I used McCabe-Thiele method, because it is easier and nowadays
mostly used method.

Equilibrium Curve (Relative Volatility)

First of all, vapour-liquid equilibrium (VLE) data which I got from PROII required for the
McCabe-Thiele is shown in Figure 1 for an ethyl benzene-styrene mixture at atmospheric
pressure.
Figure 1.

This is the nearly the same plot when I take the relative volatility (=1.38) which is given in our
Separation Process Principles book (Table 7.1) for ethyl benzene/styrene mixture and plot the x
and y diagram in my Excel document by this relationship:

Figure 2.

Reflux Ratio
In a McCabe-Thiele method there is a pinch point which is the intersection of rectifying,
equilibrium and q (feed) line. At this point, the intersection of ordinate line and the continued
line of rectifying line is the function of Rmin.

Intersection point= XD/(Rmin+1) Eq-1

Figure 3.

To find more accurate value of Rmin, I did all of these lines, intersections in excel. First of all,
after plotting equilibrium curve, should be started to plot with 45®line.

q-line
After that, continue and plot the q-line. Initial point of this line is the fraction of light
component in the feed ( xF=yF=0,461). To find the second line we should find the slope of the
line.
𝑞
Slope of the q-line= 𝑞−1 . Eq -2

Here, q equals to:

Eq-3

Because of the lack of information, I assume as an Example 7.1 in Separation Process Principles
book. The feed enters the column with a molar percent vaporization equals to the distillate-to-
feed ratio.
VF/F= D/F=102.79/222.88=0.461

q=LF/F= (F-VF)/F=1-VF/F=1-D/F=-0,539

Now, just need a q-line to pass from the equilibrium curve for intersection point. This linear
equation can easily be used to find any second point by assuming x2.

y2=k(x2-x1) + y1

Stripping line
There is no any role of stripping line. It will just join to the intersection point of equilibrium
curve, rectifying and q-lines. Start point of this line is fraction of light component in bottom
stream ( xW=yW=0.0004).

Rectifying line
Finally, for rectifying line the initial point of rectifying line-fraction of light component in
distillate (xD=yD=0,999) is noted. The end point of this line is on the ordinate line. So the x is 0
and y is Eq-1. End point of y is a function of Rmin . Because rectifying line should be intersected
with equilibrium and q-line at pinch point, by giving various values to Rmin we find the pinch
point and accurate Rmin at Excel.( Rmin=6.02)

It is suggested that for many systems the optimum reflux ratio lies between 1.2 to 1.5 times the
minimum reflux ratio. Therefore:

R= Rmin x 1.3=8.06

Number of plates
In the attached excel spreadsheet (file name: Number of plates), after input of data (Reflux
ratio, Relative volatility, q-line, etc.) following results are obtained :

Number of theoretical plates (Plus reboiler): 80

Feed plate (From top of the column): 38

It is not difficult to find number of trays and feed tray in excel after finding a pinch point and
reflux ratio in a graph, especially for less tray numbered columns. However, because there is 80
trays it would take hours to find the exact number. That is why I used the prepared excel
spreadsheet.
Tray Efficiency
To find tray efficiency, Equation 4 is used:

E0=13.3 - 66.8 log μ = 52.4% (4)

Where E0 is in % and μ (cP) is liquid viscosity in a feed. Viscosity is taken from the stream
property table in PROII. S1 is the feed stream.
𝑇ℎ𝑒𝑜𝑟𝑜𝑡𝑖𝑐𝑎𝑙 𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑡𝑟𝑎𝑦𝑠
Actual Number of Trays= 𝐸𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦
*100=152.73=153

This number is too close to the number of trays which is given in Turton_AppB result T-402
tower(158).

Diameter of Column
Generally, diameter of column is determined the same as absorber design. However, we have
no any vapor in the feed of column, because it is the bottom stream of the multicomponent
distillation column. Ethyl Benzene and Styrene are heavy components in multicomponent
distillation column (T-401). Therefore another method could be used. In this method there is no
need for vapor flow rate or density of the feed stream.

1. Determination of the tray load.

Tray load is characterized by the vapor load VL..

The design tray for which the diameter of column is calculated is the tray that has the greatest
vapor load VLMAX. The following calculations are relative to the working conditions of this tray.
For maximum vapor load the tray that has the highest actual vapor flow rate should be used
from text report of PROII. Third tray has the highest vapor flow rate (129.377 K*M 3/HR) and
actual density of liquid and vapor, flow rate of liquid (QL) should be chosen from this tray.

2. Approximation of internal diameter Di at the level of design tray.

The tray spacing value is TS is chosen according to the range of internal diameter.

If the internal diameter is in the range of 0.8 to 1.2 m, the TS=0.45 m

If the internal diameter is in the range of 1.2 to 6 m, the TS =0.6 m.

By putting data to the equations above, final answer is:

Di=4.5 m. TS =0.6 m.

Tray Spacing
Another important parameter to consider when designing any distillation column is the
distance between the trays, or tray spacing. The tray spacing is often dependent on whether
the system is operated under vacuum conditions, moderate to high pressures, or at
atmospheric. Towers that operate under vacuum conditions often are spaced between 0.6 to
0.76m apart, while atmospheric distillation columns tend to be between 0.31 and 0.76m apart.

As discussed in the Operating Conditions section, Ethyl Benzene-Styrene distillation tower

should be under vacuum conditions. And TS above is in the range of 0.6-0.76 m for vacuum
operation. Therefore this value is feasible for this condition.

When the number of trays is known,more refined computations give approximately 0.1 psi/tray
( 0.7kPa/tray) pressure drop for atmospheric and superatmospheric pressure operation, and
0.05 psi/tray(0.35 kPa/tray) pressure drop for vacuum operation. Therefore, pressure drop per
tray in our column for vacuum condition is 0.05 psi/tray(0.35 kPa/tray).

Tray Type Selection

Distillation towers commonly use bubble-cap trays, sieve trays, valve trays, or dual-flow trays
depending on the separation process. Figure below shows the market presence of the various
types of trays and since no information was found for dual-flow trays its market presence was
assumed to be minimal.

Figure shows that valve trays are one of the more popular tray types to use in distillation
towers, but a decision on the type of tray should not be based on this alone. An extensive
comparison of the different tray types was performed in order to reach a decision on the best
tray for the ethyl benzene-styrene distillation tower. Table below summarizes some of the key
points that were considered in choosing the tray type:
In consideration of the above factors for designing a distillation column, the valve tray seems to
be the best suited tray type for the separation of ethyl benzene-styrene. A graphical
representation of a valve tray has been included in Figure above. It has a low cost relative to
the other types, requires a small amount of maintenance, has the capacity to handle high flow
rates, and is highly efficient. Valve trays also account for approximately 70% of all tray types,
and can handle a turndown ratio of approximately 4-5 to 1.

Height of Column
Height of the column in meters is given by the relation:

H=N*TS+2= 97 m.

Where N is the real number of trays .Furthermore, 2 meters take into account supplementary
heights at the top and bottom of the column.

This value is too big for a column. Actually when it is taller than 75 m, second column should be
used in industry. In Turton result section, because of too small tray spacing (6 in) height of the
column is smaller.

Materials of Construction
The choice of materials of construction is an extremely important step in the design of
distillation towers, as it affects the safety of the process and also the capital costs. In
consideration of this, the following factors should be examined when choosing a particular
material for construction (Coulson, 2003):

 Mechanical Properties (i.e., strength, wear resistance)

 Effect of temperature on the mechanical properties
 The materials resistance to corrosion
 Ease of fabrication
 The availability of the material particularly in the desired size
 Cost

In the separation of ethyl benzene and styrene via a distillation column, there are no inherent
corrosion concerns. Therefore, the material of construction does not necessarily need to resist
corrosion, and for this reason, carbon steel was an ideal choice for the tower and also the trays.

Figure below compares the relative cost of carbon steel and other materials of construction for
trays (Kister, 1992). These relative costs of materials will likely represent the costs involved for
other pieces of equipment too, including the column vessel, reboiler, condenser, and reflux
drum materials. Using carbon steel as the material of construction for all of these pieces of
equipment will result in significant capital cost savings.

Weir Height
The volume of liquid on the plate is determined by the height of the weir. It is also an important
factor in the determination of plate efficiency. Plate efficiency increases as the weir height
increases. However, this is at the expense of a higher plate pressure drop. For distillation
columns which require a vacuum lower weir heights are suggested as this reduces the pressure
drop. Recommended weir heights are typically in the range of 6 to 12mm for vacuum
operation. For columns which operate above atmospheric pressure weir heights are generally
between 40mm and 90mm. It is recommended that weir heights of 40 to 50mm are used.In this
case, because our column works under vacuum operations, weir height is 10 mm (0.39 in).

Summary of Tower
T-402
Carbon Steel
D= 4.5m
153 sieve trays
52.4% efficiency
80 theorotical trays
Feed on tray 38
0.6 m tray spacing
10 mm weir height
Column height = 94 m

Other Equipments.

Reflux Drum Design

Vapor flows from the top plate to the condenser and then to a cylindrical reflux drum, usually
located near ground level, which necessitates a pump to lift the reflux to the top of the column.
If a partial condenser is used, the drum is oriented vertically to facilitate the separation of vapor
from liquid—in effect, acting as a flash drum. When vapor is totally condensed, a cylindrical,
horizontal reflux drum is commonly employed to receive the condensate.

Because vapor in our reflux drum is totally condensed, horizontal reflux drum calculations
should be used.

To handle process fluctuations and otherwise facilitate control, vessel volume, VV, is
determined on the basis of liquid residence time, t, which should be at least 5 min, with the
vessel half full of liquid.
Where, L is the molar liquid flow rate leaving the vessel. L*ML is the mass flow rate of liquid
leaving vessel. That is the sum of distillate and reflux stream= L+D. Distillate flow rate is given
and reflux stream flow rate could be found by Reflux Ratio*Distillate flow rate.

L*ML=D+R*D=10912.9+8.06*10912.9=98870.874 kg/hr (1)

L is the density of liquid at distillate that is equal to reflux stream density assuming as equal to
tray 1 (786.115 kg/m3). All of these are taken from text report:

After finding Volume of drum (21 m3), for minimum drum diameter (1.88m) equation below is
used:

For complete design, ratio of L/D should be found. Drum is in the cylindrical shape. The volume
∗𝐷^2
of drum is: V= *L
4

L is a length of drum and could be easily found from above equation: L=7.5 m.

L/D=4. Optimal value for a drum.

Reflux Drum Summary:
T-402
Carbon Steel
Horizontal
L/D = 4
V=21 m3

Reflux Pump

The aim is to determine power of the pump PP and electric driving motor PM. Because there is
no any line sizing for pump designing , diameter, length, etc. of line is unknown. That is why,
another method is used. The schematically illustrated view:

Here Pressure of column (P2) will not be calculated. Because distillate stream which is mostly
ethyl benzene is recycled back to the other unit and flow meter and control valve will be used.
To find P1 and P3 following equations will be used.
Necessary data are:

-Volumetric flow rate of liquid to be pumped. Above in the reflux drum section it is calculated.
(1)

-P1 and P3. P1 is the reflux drum pressure. It is assumed as tray 1 pressure in bar
(65kPa=0.642bar)

P3 is the distillate pressure in bar (25 kPa=0.247 bar)

-Specific gravities. Specific gravity of tray 1 is used in reflux drum section calculations = Actual
density /1000.

And that of distillate stream specific gravity is used in discharge (S2 stream) section
calculations.
Differential Pressure: P= P3-P1

Differential Height:

After these, Power of the pump is obtained by relation:

Where, efficiency of pump is assumed p=0.8 as in Turton.

Finally from following table, power of the motor is determined: 20 HP

Type of Pump: Again when choosing appropriate pumps type we should consider vacuum
conditions. For vacuum operation, generally positive displacement pumps are used such as
reciprocating and diaphragm pumps. Also steam jet ejectors as a pump and vacuum pumps are
also used for vacuum operations.

Pump Summary
P-403A/B
Carbon Steel
Reciprocating,diaphragm
pumps; vacuum pumps.
W=14 KW(actual)
80%efficient

Condenser
Condensers are units similar to heat exchangers, which are used to condense the vapours to
their liquid state. For condensers used in distillation columns, the process fluid generally flows
through the shell side and the cooling fluid is made to flow through the tube side. The two
fluids never come in contact with each other.

Column pressure and condenser type are established by the algorithm shown in Figure 7.16,
which is formulated to achieve, if possible, a reflux-drum pressure, PD, between 0 and 415 psia
(2.86 MPa) at a minimum temperature of 120F (49C), corresponding to the use of water as
condenser coolant.
To calculate bubble-point pressure of distillate flash is used which in specifications bubble-point
is chosen for pressure.

After running simulation, at T=120C, bubble-point pressure of distillate (S2) is 56.308 kPa (8.17
psia).
If we start the algorithm, PD=8.17 215 psia. Therefore total condenser should be used. All the
vapor condensed.

Condenser design
Assumptions:

There is one shell and 2 tube pass inside the condenser and the flow is counter current.

The cooling fluid chosen is chilled water that enters the tube side at 30 C.

The tube layout for this particular design is arranged in a squared pitch.
No need for procedure. Because my team -mate have done it for heat exchangers. Data
extracted from PROII simulator software.

Data for shell-side:

Temperature:

T1 is the tray 1 temperature which enters condenser. 394.4 K=121.25 C

Because there is no any information for temperature of hot side leaving heat exchanger, thus
temperature is assumed to be the same as distillate temperature. T2 = 90.8 C

Mass flow rate:

It is the sum of reflux and distillate flow rate which is calculated many times above:
95837.0878kg/hr

Density: The first tray vapor density is used: 2.1599 kg/m3

Viscosity and thermal conductivity from first tray:

Heat Capacity:

Data for Tube-side:

Temperature:

t1 is assumed to be 30 C. t2 is calculated QH=QC

Mass flow rate is given of hps: 1105980 kg/hr.

After simulation of stream that has water at above conditions following results are obtained:

U is assumed to be 600 W/m2*C from graph. Condensate and organic vapors are considered.
Data are used in heat exchanger calculations which are designed in excel by expressions for Tlm,
U, Q, Re, Pr, Nu and etc.

After finding a result, it is observed that final U0 is close to the estimated U. Therefore,
resultant data are feasible.

Number of tubes:108

Tube out-side diameter: 0.02 m. Inside diameter: 0.016 m.

Tube length: 4 m.

Condenser Summary
E-408
Carbon Steel
A=27m2
Process fluid in shell, cooling water in tubes
1 shell––2 tube passes
Q=4600MJ/HR
 Reboiler

Reboilers are used with the distillation column to vaporise a fraction of the bottom product.
There are three different kind of reboilers used: Forced Circulation, Thermosyphon, Kettle
Reboilers.

In this design a kettle reboiler will be used. In kettle reboilers boiling takes place on tubes which
are immersed in a pool of liquid.

Inlet Temperature of steam is assumed 150 C.

Inlet Temperature in tube side is assumed bottom stream temperature. 123.7 C

Outlet Temperature in tube side is bottom tray pressure. 129.45 C

All other data are found the same as what is done in condenser. Viscosity, Conductivity, Density
and so on are of bottom tray liquid in tube side. In shell side again from stream property table
all data are found as condenser.

Final answer:

Number of tubes: 49

Tube out-side diameter: 0.02 m. Inside diameter: 0.016 m.

Tube length: 4 m.

Reboiler Summary
E-409
Carbon Steel
A=13m2
Desuperheater––steam saturated at 150°C
1 shell––2 tube passes
Q=1259,963MJ/HR

As a rule, reboiler duty should be less than the condenser. It is obtained in the current results.
 Control Systems over the Distillation Column

Various control measures have been taken into account to meet the objectives of the plant
such as safety, operation, environmental constraints and economics. Sensors have been
installed at various process lines and equipments to make the operator aware of the situation
with the equipment and the process. The sensors transfer signals to the controller which then
send back commands to the respective valves to carry out the action. In PID they are not given.
These sensors could be used in my distillation column.

FC-Flow controller in the feed. The feed pipe is installed with a flow controller, which helps to
control the flow throughout the pipe. The flow rate is received as input to the FT, which then
sends output signals to the flow controller FC, which then sends on information to the
automated control valve. This ensures a steady state and control flow rate of feed to the
distillation column.

PC-Pressure Controller at top

The distillation column is operating under high pressures. The pressure is a very crucial variable
and has to be controlled to avoid flooding. The condenser would reduce the flow rate of water
if the pressure drops; this intern increases the temperature of the distillate entering the reflux
drum as desired heat exchange was not possible; which increases the pressure back into the
column. The reverse action is carried out if the pressure inside the column increases. There is a
relief valve on the reflux drum which also operates when the pressure inside the column
increases drastically.

LC-Level Controller in reflux drum

For desired separation to take place, it is important to maintain the ratio of the distillate to the
reflux Liquid. Hence it is vital to maintain the level in the reflux drum. The level is read by a level
indicator which sends the information to the LT 1 which further forwards the signal to the
control valve on the pipe back to the condenser. If the level in the drum falls, the controller
sends signal to close the valve which results in maintaining the level in the drum.

TC-Temperature Controller

The temperature should be well maintained inside the column to provide vaporisation of the
volatile fluids for desired separation. Heat is provided by the steam flow in the reboiler. Hence
a controller valve is installed on the pipe which carries steam to the reboiler. If the temperature
inside the column reduces, the controller sends signal to the control valve to open slightly. This
increases the flow rate of steam into the reboiler increasing the temperature of the column.
 Safety Considerations

Some of the safety considerations that should be considered in the design and operation of a
distillation column include: prevent the tower from reaching high pressures, the presence of
manholes for column access, and proper waste treatment.

Distillation towers, as well as other towers and drums, must be protected from any
overpressure that may occur as a result of malfunction, fire or utility failure (Stellman, 1998).
Important measures must be employed in order to develop a process safety strategy that will
improve safety, minimize any losses, and also protect the workers health. The proper way to
protect against overpressure in distillation towers is by using pressure relief valves. Often the
pressure relief valve is located near the top of the tower to handle the vapour load, but there
have been towers where different locations have been used for the pressure relief valves.
Basically how a pressure relief valve works is by discharging to the atmosphere or a closed
system. If it is decided that the discharge should be to the atmosphere, then it is imperative to
determine whether this discharge may potentially put the workers health at risk or not.

Another safety concern for distillation towers is the presence of manholes for column access.
These manholes are essential for cleaning any fouling that may occur within the column, and
the number of manholes is often dependent on the number of trays. There should be at least
one manhole per 30 trays in a clean and noncorrosive column .When the maintenance crew are
entering the manholes for cleaning, they should wear the appropriate personal protective
equipment (PPE) .

Other considerations for the maintenance crew working within the confines of the distillation
column include:

- Check their safety equipment before entering the column

- Ensure that workers are aware of any hazards present within the column

- Be confident that the column is safe for entry

- Ensure that a worker is stationed outside the column in case the maintenance worker inside
the column is injured

Also, if it is deemed necessary that a damaged tray be removed and replaced then special
safety requirements should be upheld in order to protect the maintenance worker. Often,
sharp pieces of metal from the trays can be left hanging, or may become brittle and therefore
not support the worker’s weight.
 Conclusion

The design project has been successful in its aims of providing a detailed knowledge a chemical
process unit. This project was a learning process where different challenges were faced. At this
stage, such a project is aimed to increase general design knowledge of a given operating unit in
this case; a binary plate distillation column. As this was just a preliminary design, the amount of
detail of the design and the accuracy of the final calculations might be questionable. However,
it remains a fact that this project targets more than just design but also gives an idea of how to
make reasonable assumptions and where data is not available, the use of values which can be
used to make reasonable estimates. Overall the project enhances one’s ability to play around
with available data in order reach a reasonable estimate.

I designed 5 equipments: Distillation column, reflux drum, condenser, reboiler and a pump.
During designing of equipments, vacuum conditions for ethylbenzene/styrene distillation
column are considered. In general, resultant data are similar to the results in Turton besides
some of them.