INDIVIDUAL DESIGN

ASSIGNMENT 1 – CHEMICAL DESIGN

(Design of a de – ethanizer column)

Name: Perera A. T. K.

Index Number: 100375D

Date of Submission: 05/01/2015

INTRODUCTION

Ethylene is a widely using industrial chemical as a raw material in producing various

products like polyethylene, polyvinyl chloride, ethylene dichloride and etc. Ethylene is
mostly produced by steam or catalytic cracking of Naphtha or Natural Gas. As per the
economists views the global demand for ethylene may increase at a compounding rate of 10
million tons per year. In Sri Lankan scenario, amount of ethylene based products imported in
year 2011 was 52,000 MT. This figure can be expected to be grown by now with the
increasing global demand. So to match this increasing demand in house ethylene production
in the country can be considered.

As the comprehensive design project of our group, it was decided to address this matter and
develop an ethylene production facility with steam cracking of Natural Gas as there’s a huge
potential of having Natural Gas in Mannar basin oil exploration sites. However to begin the
process imported LNG is used. The process flow for the production follows several
separation columns before and after the steam cracker along with other common equipments
like heat exchangers and compressors. For separation of the key components along the
process, distillation can be used in most of the steps.

The mixture of hydrocarbons obtained after the cracking should be separated at several stages
and separation of C2 components from C3 and other heavier hydrocarbon components is
crucial prior to the final fractionation of ethylene from C2 components. This separation is
done using the de-ethanizer, a distillation column designed to match the separation
requirements.

Based on the boiling points at standard temperature and pressure C2 components can be
separated from C3 and other heavier components using distillation.

Table 1.1 : Boiling points of Feed components at 1 atm

Component Boiling Point at 1 atm (°C)

Ethylene -104
Ethane -88
Ethyne -84
Propylene -48
Propane -42
Propyne -23.2
Butene -6
Butane 0
Butyne 8.1
Pyrolysis gasoline 32 - 204
Cyclobutadiene 41.2
Benzene 80.1
Toluene 110.6
Styrene 145
Pyrolysis fuel oil 169 – 579.4

Maximum recovery of C2 components at the top product is required as the final product
outcome is ethylene and ethyne (Acetylene) can be converted into ethylene by catalytic
hydrogenation which is financially beneficial. At the final fractionators ethylene is separated
from ethane and ethane is sent back to steam cracker for production of ethylene.

Commercially the separation of C2 components is done almost completely from C3

components. Because of these reasons maximum recovery of 99.99% of ethyne at the
distillate and 0.01% recovery of propene at the top product are taken as design considerations
while designing the tower secondary de-ethanizer.

Further for the conversion purpose of ethyne, the top product is collected and transferred to
the next unit in gaseous phase. Therefore a partial condenser is used at the top of the
distillation tower.

DISTILLATION COLUMN

Distillation columns can be designed with different column internals. According to the
column internal the column may be a packed column or a tray column. In both columns there
are few advantages and disadvantages. Therefore the selection of the tower type should be
done carefully.

Packed bed columns

These are columns in which the internal is packed with random or structured shape packing
material and provides a larger surface area for vapor liquid mixing. These are most often used
for absorption but can be used in distillation too. The associated advantages and
disadvantages of packed bed columns can be listed as follows.

Advantages:
For columns less than 0.6 m in diameter, most efficient tower type.
Lower pressure drop compared to tray columns.

Can be used to handle corrosive liquid mixtures as packing material can be made by inert
material.
Suitable for thermally sensitive liquid separations.
Disadvantages:

Packing material may get damaged during installation or under extreme temperatures due to
thermal expansion or contraction.
Contact efficiency is low when liquid flow rates are smaller.
Higher cost at high liquid flow rates.

Tray distillation columns

These are columns in which the internal upward and downward flow of liquid and vapor is
disturbed by placing trays with a definite gap in between them in order to obtain a good
liquid vapor mixing. These are widely used in distillation applications. The number of trays
varies according to the application. This type also has some pros and cons.

Advantages:
Most efficient type of distillation column when column diameter exceeds 0.6 m.
Suitable for cryogenic distillation applications as it is easy to equip with cooling coils.
Liquid vapor contact in cross flow tray column is more effective than countercurrent flow in
packed columns.
Can use for high liquid flow rates cost effectively.
Can handle cryogenic conditions of distillation.
Disadvantages

Higher pressure drop compared to packed beds.

Possibility of foaming as a result of agitation of liquid through vapor.

Considering all the above factors, it is clear that packed bed columns are not suitable for
operation at cryogenic conditions and hence can be eliminated from selection. Then the
viable option becomes using tray type column for the separation of desired components. This
is because the separation should be done under cryogenic conditions.

Selection of tray type for the column

The trays that are used as column internals can be designed in several ways. The types
include sieve trays, valve trays and bubble cap trays. Each of these types brings its own
advantages and disadvantages to the distillation column. Those advantages and disadvantages
can be considered as follows.

Sieve tray Valve tray Bubble cap tray

Cost Ratio (Compared 1 1.5 3
to Sieve tray)
Efficiency Very similar for all three types
Capacity Very similar for all three types
Pressure drop Lowest value Moderate Highest value
Application Depend on the vapor Has a greater Suitable for low
flow rate flexibility vapor flow rate
Weeping can occur applications as
design provides a
liquid seal.

Considering all the factors above discussed it is decided to select valve type trays to complete
the column internal as it has a greater flexibility and the capital cost for the construction also
is reasonable when compared to bubble cap trays. Further the capacities and efficiencies
being nearly similar for all three types it would be better to select a cost effective and flexible
design for the column.

Flow arrangement

The arrangement of flow on the trays can be decided

MATERIAL BALANCE

Since the feed consists of number of components, multicomponent distillation should be

considered in order to separate the components as desired. Therefore determination of key
components for the material balance becomes a crucial step of calculation. As the major
requirement of de-ethanizer is to separate C2 components from C3 and other heavier
components, ethyne was selected to be the light key with a recovery of 99.99 mol% at the
distillate and propene was selected to be the heavy key with a recovery of 0.01 mol% at the
distillate.

 Light key: The most volatile component in the bottoms, but in a significant
concentration is known as the light key. Therefore more volatile components than
light key does not go to the bottoms
 Heavy key: The least volatile component in the distillate, but in a significant
concentration is known as the heavy key. Therefore less volatile components than the
heavy key does not go the distillate

Only ethyne (Light key) and propene (heavy key) is distributed between top and bottom
products as there are no other components in between the light and heavy key according to
boiling points.

The following formulae were used in calculation of mass fractions, mole fractions and molar
or mass flow rates during material balance.

During calculations a constant molar overflow of components through the column was
assumed.

Based on the above formulae the calculated feed composition for the secondary de-ethanizer
is as follows.

Table 2.1: Feed composition for the secondary de-ethanizer

Component MT/day W/W % kmol/day mol/mol % MW (kg/kmol)

Ethylene 294.3411 57.3304 10512.1821 59.9835 28
Ethane 193.4509 37.6795 6448.3633 36.7950 30
Ethyne 4.1544 0.8092 159.7846 0.9117 26
Propylene 5.5164 1.0745 131.3429 0.7495 42
Propane 0.8196 0.1596 18.6273 0.1063 44
Propyne 0.1195 0.0233 2.9875 0.0170 40
Butene 0.8955 0.1744 15.9911 0.0912 56
Butane 1.2167 0.2370 20.9776 0.1197 58
Butyne 9.1517 1.7825 169.4759 0.9670 54
Pyrolysis gasoline 1.3393 0.2609 13.3930 0.0764 100
Cyclobutadiene 0.3328 0.0648 6.4000 0.0365 52
Benzene 1.4555 0.2835 18.6603 0.1065 78
Toluene 0.224 0.0436 2.4348 0.0139 92
Styrene 0.0568 0.0111 1.1360 0.0065 50
Pyrolysis fuel oil 0.3375 0.0657 3.3750 0.0193 100
Total 513.4117 100 17525.1313 100

General equation for the material balance;

For a multicomponent distillation column, the material balance equations can be expressed in
the following form.

Overall material balance for the tower;

Overall material balance for the ith component;

Where;
F = Feed flow rate

D = Distillate flow rate

W = Bottom flow rate

XiF = Molar fraction of ith component in the Feed

XiD = Molar fraction of ith component in the Distillate

XiW = Molar fraction of ith component in the Bottom

Further, XiF, XiD and XiW can be calculated using the following formulae.

D kmol/day

F kmol/day

W kmol/day

Being heavy key and light key only ethyne and propene are distributed between top and
bottom products according to the specified recovery molar fractions. The components lighter
than light key are only found in tracer amounts in the bottoms and components heavier than
heavy key are only found in tracer amounts in the top product. Therefore the material balance
for the distillation tower will be as follows.
 Table 2.2: Distribution of feed composition over distillate and bottom

F. XiF D. XiD W. XiW XiD XiW

XiF
Component kmol/day (kmol/day) (kmol/day)

0.5998 10512.1821 10512.1821 0 0.6140 0.0000

Ethylene
0.3679 6448.3633 6448.3633 0 0.3766 0.0000
Ethane
0.0091 159.7846 159.7686 0.0160 0.0093 0.0000
Ethyne
0.0075 131.3429 0.0131 131.3297 0.0000 0.3244
Propylene
0.0011 18.6273 0 18.6273 0.0000 0.0460
Propane
0.0002 2.9875 0 2.9875 0.0000 0.0074
Propyne
0.0009 15.9911 0 15.9911 0.0000 0.0395
Butene
0.0012 20.9776 0 20.9776 0.0000 0.0518
Butane
0.0097 169.4759 0 169.4759 0.0000 0.4187
Butyne
0.0008 13.3930 0 13.3930 0.0000 0.0331
Pyrolysis gasoline
0.0004 6.4000 0 6.4000 0.0000 0.0158
Cyclobutadiene
0.0011 18.6603 0 18.6603 0.0000 0.0461
Benzene
0.0001 2.4348 0 2.4348 0.0000 0.0060
Toluene
0.0001 1.1360 0 1.1360 0.0000 0.0028
Styrene
0.0002 3.3750 0 3.3750 0.0000 0.0083
Pyrolysis fuel oil
1 17525.1313 17120.3272 404.8041 1 1
Total

Therefore;
 Further for flow rate calculations inside the tower material balances for rectifying and
stripping section are required.

Rectification Section Stripping Section

F
D
V’
L L’

V L

Assuming Constant Molar overflow,

Material balance for the system shown, Material Balance for the system shown,

V= L+D - - - (eqn 2.8) L’ = V’+W - - - (eqn 2.10)

Further, R = L/D [defined] - - - (eqn 2.9)

Material Balance over feed plate,

F+ L+ V’ = V+L’
F V L
V’ – V = L’ – L – F - - - (eqn 2.11)
L’
V’

Further, as feed is saturated liquid,

L’ = L+ F - - - (eqn 2.12)
ENERGY BALANCE

Energy balance for a distillation column simply implies the condensing and heating energy
requirements in condenser and reboiler. In order to find these it is essential to know distillate
and bottom products temperatures. This is because the energy required for condensation of
distillate or vaporization of bottoms is a function of its enthalpy at that temperature.

Temperature Calculations for Towers

Bubble point calculation
A temperature is assumed for the bubble point of tower
 Feed or liquid phase composition and operating pressure are known
 K values are obtained from the literature for the corresponding temperature and
pressure for each component.
 Vapor phase mole fractions were calculated for all the components using,

Where;
Yi = mole fraction of ith component in vapor phase

Ki = K value of ith component where,

Here, = Saturated vapor pressure of ith component and,

P = Operating pressure of the distillation tower
Xi = mole fraction of ith component in liquid phase

 If ƩYi = 1 the assumed temperature is correct and if not a new K value is calculated
for one component and a temperature that satisfies the new K value is taken.

 Calculation was repeated from step 1 until ƩYi =1

Dew point calculation

 The known composition is taken as vapor phase composition when operating

pressure is known.
  A temperature is assumed for the dew point and K values for all the components
were found at corresponding temperature.
 Liquid phase composition (Xi) was calculated for all the composition using the
following equation.

 If ƩXi = 1 the assumed temperature is correct and if not a new K value for one
component is calculated.

 New temperature (Tnew) to match the new K value is chosen and K values for all
the components at new temperature are found.
 Calculation was repeated until ƩX i =1.

The calculated liquid and vapor phase compositions and temperatures of distillate and bottom
can be tabulated as below.

Table 2.3: Distillate and Bottom temperatures with compositions

Distillate temperature (Vapor Bottom temperature ( Liquid

dew point) bubble point)
Component Yi K (-23.15) Xi2 Xi K(95.85) Yi
Ethylene 0.6140 1.3117 0.468101 0.0000 0
Ethane 0.3766 0.725 0.519517 0.0000 0
Ethyne 0.0093 0.75 0.012443 0.0000 0
Propylene 0.0000 0 0.3244 2.431493 0.788844
Propane 0.0000 0 0.0460 2.2 0.101234
Propyne 0.0000 0 0.0074 0.6285 0.004638
Butene 0.0000 0 0.0395 0.148 0.005846
Butane 0.0000 0 0.0518 0.835 0.043271
Butyne 0.0000 0 0.4187 0.1342 0.056184
Pyrolysis gasoline 0.0000 0 0.0331 0.0283 0.000936
Cyclobutadiene 0.0000 0 0.0158 0.2034 0.003216
Benzene 0.0000 0 0.0461 0.0639 0.002946
Toluene 0.0000 0 0.0060 0.0127 7.64E-05
Styrene 0.0000 0 0.0028 0.00637 1.79E-05
Pyrolysis fuel oil 0.0000 0 0.0083 0.0283 0.000236
Total 1.0000 1.00006 1.0000 1.007447

Therefore;
Distillate temperature = -23.15 °C

Bottom temperature = 95.85 °C

Average column temperature =

Therefore, average column temperature = 36.35 °C

Since the distillate is taken as saturated vapor and bottom product is taken as saturated liquid,
only latent heats of vaporization and condensation counts for the energy balance or Reboiler
and condenser heat loads.

Condenser Heat Load

Where, λL = Latent heat of liquid mixture which is at equilibrium with distillate vapor

L = Liquid flow rate of rectifying section (only this part is condensed while product is taken
as vapor)

Latent heat of a mixture can be calculated as,

From the calculations, λL = 487052.212 J/kg

LW = Liquid mass flow rate in rectifying section = 224622.1158 kg/day

Therefore,

Condenser Heat Load = 109402.698 MJ

Reboiler Heat Load

In similar manner, Reboiler heat load is calculated. Here Latent heat of vaporizing vapor and
its mass flow rate is taken for calculation.

From the calculations, λL = 503139.3 J/kg

LW = Vapor mass flow rate in stripping section = 929639.3296 kg/day

Therefore,

Condenser Heat Load = 467738.0815 MJ

COLUMN DESIGN

Minimum Reflux Ratio (Rm)

Minimum reflux ratio for the column can be found using Underwood equations for multi
component systems.

First Underwood equation;

Second Underwood equation;

Where;
αi = Relative volatility of ith component at average column temperature
ϕ = A factor defined for the calculation
q = L/F where, L- Liquid fraction of feed and F- Feed flow rate
q = q factor of the feed
Table 2.4: α values of feed components at column average temperature

Component α value at 36.35 °C

Ethylene 5.2941
Ethane 3.4118
Ethyne 4.0588
Propylene 1
Propane 0.8235
Propyne 0.3981
Butene 0.1071
Butane 0.2368
Butyne 0.0908
Pyrolysis gasoline 0.0164
Cyclobutadiene 0.1255
Benzene 0.0198
Toluene 0.0074
Styrene 0.0017
Pyrolysis fuel oil 0.0164

α values are defined with respect to heavy key of the system which in this case is propylene.
Where; KA = K value of considering component

KB = K value of heavy key

q Factor for the feed = L/F,

As the feed is saturated liquid or liquid at its boiling point L=F,

Therefore, q = F/F =1

For the convenience of calculation, the components below the heavy key and which are not included
in the mixture with great percentages were considered as groups.

C3 components are considered as propane (pink), C4 components as butyne (green) and other heavier
components as Heptene (Blue) as most of them are C7 components.

Table 2.5: Feed composition to the tower

Component XiF F. XiF kmol/day

Ethylene 0.5998 10512.1821

Ethane 0.3679 6448.3633

Ethyne 0.0091 159.7846

Propylene 0.0075 131.3429

Propane 0.0011 18.6273

Propyne 0.0002 2.9875

Butene 0.0009 15.9911

Butane 0.0012 20.9776

Butyne 0.0097 169.4759

Pyrolysis gasoline 0.0008 13.3930

Cyclobutadiene 0.0004 6.4000

Benzene 0.0011 18.6603

Toluene 0.0001 2.4348

Styrene 0.0001 1.1360

Pyrolysis fuel oil 0.0002 3.3750

Total 1 17525.1313

Table 2.6: Categorized feed composition and their relative volatility at average temperature

Component XiF F. XiF kmol/day α Values

Ethylene 0.5998 10512.1821 5.2941
Ethane 3.4118
0.3679 6448.3633
Ethyne 0.0091 159.7846 4.0588
Propylene 0.0075 131.3429 1
Propane 0.0013 21.6148 0.8235
Butyne 0.0118 206.4446 0.0908
Heptene 0.0027 42.0241 0.0164

Using 2nd Underwood equation the following polynomial equation is obtained.

Using MATLAB software, the roots of the above polynomial are founded to be,

4.0096 + 0.0446i, 4.0096 - 0.0446i, 1.001, 0.8467, 0.1007 and 0.0202

Choose ϕ = 1.001 [In between heavy key and light key]

Then, applying ϕ = 1.001 in first Underwood equation,

Rm = 0.3007

Optimum Reflux ratio (R)

The optimum reflux ratio of distillation lies between 1.2 -1.5 times Rm at many instances.

Therefore, choose

Using equations from eqn 2.9 to eqn 2.12, When R = 0.45,

L = 7704. 1472 kmol/day

V =24824.2945 kmol/day

L’ = 25229.2785 kmol/day

V’ = 24824.4744 kmol/day

All flow rates within the column are positive. Therefore the Reflux Ratio of 0.45 is acceptable.

Minimum Number of theoretical stages (Nm)

Fenske equation for determination of Nm,

Where;

αlk ,ave = relative volatility of light key ( the geometric average)

Then, Minimum number of theoretical stages = 10.68

Number of theoretical stages required for the separation (N)

Gilliland correlation for the estimation of number of theoretical plates is used,

Fitted equations

x = a finite value for the ratio between reflux ratios

Here, x= 0.103

For, 0.01 ≤ x ≤ 0.9 

So the number of theoretical stages required,

N= 22.9119 ≈ 23

Feed tray location

 Feed tray location at minimum number of theoretical plates (NF, min) is given by;
α values are given at column average temperature, and molar fractions at total reflux are similar to
calculated values as there are no distributed components in between the heavy key and light key.
Therefore; from calculation;
NF, min = 6.3846
 Feed tray location at finite Reflux (NF)

Feed tray Location when R=0.45,

NF = 13.697

Efficiency of column (E)

O’connel correlation provide with a means of obtaining overall column efficiency. This correlation is
mostly suitable for hydrocarbon mixtures. Therefore can be used for this system also with a high
accuracy.
To read the graph, the product of Molar average liquid viscosity (µ a mNs/m2) and average relative
volatility of light key (α a) is required.
Viscosity of a liquid mixture can be expressed with following relationship,

For molar fractions of components in liquid mixture, molar fractions of feed components are used.
Viscosity of liquid mixture = µ

αa = 4.8415 [from calculation of Nm]

From the graph of O’connel correlation,

Overall efficiency of the column = 55%

This lies between typical efficiency range of 30 -70%. Therefore it is an acceptable value.

Actual Number of plates (Na)

The overall column efficiency (E) is related to Number of ideal stages (N) as per the
following equation.
From solving the equation,

Actual number of plates in the column (Na) =41.658 ≈ 42

Diameter Calculation

Mass flow rates

Rectifying section

Where;

Lw, Vw = liquid or vapor mass flow rate through rectifying section

L, V = Molar flow rates of liquid and vapor

ML,V,avg = Average molar mass of liquid or vapor

ML,avg = 29.156 kg/kmol, MV,avg = 29.734 kg/kmol

Mi = Molar mass of ith component

Xi = Molar fraction of ith component in liquid or vapor respectively

Therefore;

LW = 224622.116 kg/day = 2.5998 kg/s

VW = 738125.5727 kg/day = 8.5431 kg/s

Stripping section

Lw’, Vw’ = liquid or vapor mass flow rate through stripping section

L’, V’ = Molar flow rates of liquid and vapor

ML,avg = 41.1609 kg/kmol, MV,avg = 37.4485 kg/kmol

Therefore;

LW ‘ = 1038459.809 kg/day = 12.0192 kg/s

VW’ = 929639.3296 kg/day = 10.7597 kg/s

Average densities

Rectifying section

ρ L,avg = Average density of liquid phase in rectifying section = 556.0817 kg/m3

ρi = Density of ith component in liquid phase

For vapor phase consider all the components behave as ideal gases and use ideal gas law.

Here, P = Operating pressure of the tower = 2000 kPa

R= Universal Gas Constant = 8.314 J/mol K

T = Average temperature in Kelvin = 252.575 K

ρV,avg = Average vapor density

ρV,avg
Stripping section

Here also same equations are used. But the notification is given as ( ) ’ for the convenience of
identification.

Therefore;
ρ L,avg’ = Average density of liquid phase in stripping section = 605.1199 kg/m3
T = Average temperature in Kelvin = 312.075 K

ρV,avg’

Flow parameters

Flow parameters for rectifying and stripping section can be found using following equation.
When calculations for stripping section are done ( )’ is used as notification.

Rectifying section

Therefore, FLV = 0.0687

Stripping section

Then from calculation, FLV’ = 0.244

Area calculation

Rectifying section

From the graph for the relationship of Flow parameter vs. Flooding vapor velocity, (Vol 6,
p567)

K1 factor = 0.101 , for a tray spacing of 0.6 m.

Then,

Uf = Flooding vapor velocity based on the net column cross sectional area in m/s

Uf = 0.4360 m/s

Assume 70% of flooding condition inside the tower

Then, Actual vapor velocity (Ua ) can be given by,

Ua =0.3052 m/s

The volumetric flow rate of vapor can be given as,

Vg = 0.3017 m3/s

The net area of the column cross section can be then found using,

The down comer area of the column is usually,

The net area and column area is related by,

Therefore;

And the Active area of the plate is given by,

Where;

An = Net area of column cross section

AC = Column cross sectional area

Ad = Down comer area

Aa = Active area

Also the hole area of plate (Ah) can be found as.

From the calculation, following results are obtained;

An = 0.9885 m2
AC = 1.1233 m2

Ad = 0.1348 m2

Aa = 0.8537 m2

Ah = 0.08537 m2

Stripping section

Same procedure of calculation for rectifying section was used. But the notification is used as
( )’ for the convenience of identification.

Therefore the calculated parameter values are as follows,

From the graph for the relationship of Flow parameter vs. Flooding vapor velocity, (Vol 6,
p567)

K1’ factor = 0.076, for a tray spacing of 0.6 m.

Uf’ = 0.3396 m/s

Assume 70% of flooding is maintained in the tower

Then, Ua’ = 0.2377 m/s

Vg’ = 0.3727 m3/s

An’ = 1.568 m2

AC’ = 1.7818 m2

Ad’ = 0.2138 m2

Aa’ = 1.3542 m2

Ah’ = 0.1354 m2

Column diameters

Rectifying section

Once the column cross sectional area is known, the diameter of the column can be calculated
as follows.
Where,

DC = Column diameter

The column diameter for the rectifying section,

DC = 1.1959 m

Diameter of the column is greater than 1 m. Therefore the tray spacing of 0.6 m is acceptable.

Stripping section

Using the same equation, the diameter of the stripping section (DC’) is found to be,

DC’ = 1.5062 m

The diameter of the stripping section is greater than 1 m. Therefore the tray spacing of 0.6 m
is acceptable.

Column Height

Column height can be obtained by,

H = Column height

Na = Number of actual trays = 42

Tray spacing = 0.6 m

Therefore, H = 25.2 m