EH2208O

DESIGN PROJECT II (MARCH 2017)

PRODUCTION OF 20,000 METRIC TONNES OF

POLYTETRAFLUOROETHYLENEPER YEAR

CHAPTER 3:
BINARY DISTILLATION COLUMN (T-101)

STUDENTS NAME:
AIMAN HAKIM BIN ROSLAN
2013849224

SUPERVISOR:
MS CHRISTINA VARGIS

FACULTY OF CHEMICAL ENGINEERING

UNIVERSITI TEKNOLOGI MARA
SHAH ALAM
 CHAPTER 3

EQUIPMENT DESIGN

DESIGNED BY: AIMAN HAKIM BIN ROSLANN

3.4.1 Binary Distillation Column (T-102)

3.4.1.1 History of Distillation

The method of separating a mixture of two or more components into their respective
constituents has been practiced for over a century and dates as far back as the first
century A.D. According to (Seader & Henley, 1998), distillation was widely used in Italy
to produce alcoholic beverages in the eleventh century. During that time, distillation
was performed as a batch process and based on the use of a single stage, the boiler.
The term distillation was derived from the Latin word destillare, which means dripping
or trickling down. Over time, it was discovered that the extent of separation could be
improved by introducing multiple vapor-liquid contacts, or also known as stages. This
phenomenon is known as rectification which has its origin from the Latin word recte
facere, meaning to improve

3.4.1.2 Introduction

Within the chemical industry, distillation column is commonly used to separate a

multicomponent mixture to obtain a high purity product at the overhead and bottom.
The working principles of distillation are primarily based on the boiling point and
relative volatility; whereby less volatile components will evaporate as vapor meanwhile
volatile components will remain as liquid. Some examples of the industries which
utilize distillation in the production process are petrochemical, oil-refining,
pharmaceutical and many others.

325
 Figure 3.3: Components of a distillation column

The basic components of a distillation column include a condenser, reboiler

and reflux drum. As seen from Figure 3.3, the location of feed entering the column will
determine two section, which are enriching section and stripping section. Components
with low boiling points will have higher volatility which makes it easy to evaporate and
travel upwards in the enriching section. Conversely, components with high boiling
points have low volatility where it will remain as liquid and travel downwards in the
stripping section. The vapor at the top then enters a condenser where it is condensed
into liquid and stored within a reflux drum. The liquid that is withdrawn from the vessel
is known as the overhead product or condensate. Meanwhile, the liquid at the bottom
enter a reboiler where a source of heat is supplied to produce vapor. In most chemical
plants, steam is used as the main source of energy (Gumilar, 2009).

326
3.4.1.3 Determination of Light Key and Heavy Key

If the mixture contains only two components, the process is then called binary
distillation meanwhile if two or more components are present, it is called
multicomponent distillation. Before designing a distillation column, two key
components have to be initially identified, which are the light key component and
heavy key component. The definition of both terms is simply that the component which
is most volatile is referred as the light key meanwhile component that is least volatile
is referred as the heavy key. Another definition that can be used to describe light key
and heavy key components are such that the former is the component of the feed
mixture which is desired to be kept out of the bottom product, meanwhile the latter is
the component which is desired to be kept out of the top product (Seader & Henley,
1998).

According to (Seader & Henley, 1998), the main goal of distillation is to produce a
distillate that is rich in the light key and bottom rich in heavy key. For this process, the
two key components are:

Light key component = Hydrochloric acid (HCl)

Heavy key component = Tetrafluoroethyelene (TFE)

HCl is chosen as the light key component because it has a lower boiling point of -
85.05C which makes it more volatile, compared to TFE which has a boiling point of
76.3C.

3.4.1.4 Equipment and Design Considerations

According to (Seader & Henley, 1998), there are several factors which influence the
design or analysis of a binary distillation. Amongst them are:

1. Feed flowrate, composition, temperature, pressure and phase condition.

2. Desired degree of separation between two components.
3. Operating pressure.

327
 4. Vapor pressure drop, particularly for vacuum operation.
5. Minimum reflux ratio and actual reflux ratio.
6. Minimum number of equilibrium stages and actual number of equilibrium
stages (stage efficiency).
7. Type of condenser (total, partial or mixed).
8. Degree of subcooling.
9. Type of reboiler (total or partial)
10. Type of contacting (trays or packing or both).
11. Height of the column.
12. Feed entry stage
13. Diameter of the column.
14. Column internals.

3.4.1.5 Description of Distillation Column (T-101)

For this process, a distillation column is used to separate a binary mixture containing
HCl and TFE that is produced from the pyrolysis reaction. The reason for using
distillation method is because it is able to produce high purity products compared to
other methods such as membrane separation and solvent extraction ("CO2 Capture
Project," 2008).

Table 3.1: Summary table for T-101

Parameters Feed (F) Overhead (D) Bottom (W)
Vapour Fraction 0 0 0
Temperature () -41.68 -56.76 -40.16
Pressure (kPa) 600 400 500
Mass Flow (kg/h) 4107.56 1721.83 2385.72
Mol Flow (kmol/h) 71.26 47.19 24.06
Composition (kg/kg)
TFE 0.5783 0.0010 0.9950
HCl 0.4217 0.9999 0.005
Composition (mol/mol)
TFE 0.3333 0.0004 0.9864
HCl 0.6667 0.9996 0.0136

328
 The separation occurs continuously whereby HCl evaporates and is collected
at the overhead stream meanwhile TFE is collected at the bottom stream. According
to (Turton, Bailie, Whiting, Shaeiwitz, & Bhattacharyya, 2013), processes which
exceed 5,000 ton per year would best suited with continuous mode of operation.

Additionally, a total condenser is used to produce liquid HCl at the overhead

stream. This is because the condensate will eventually be diluted with water and sold
off as a source of revenue. Based on the general principles of mass transfer, liquid-
liquid mixing will be more effective compared to gas-liquid mixing, hence a total
condenser is used.

3.4.1.6 Bubble Point and Dew Point

Before calculating the number of stages, the bubble and dew point need to be
determined. By definition, bubble point is referred as the point where the first of bubble
of a liquid mixture begins to vaporize meanwhile dew point is the point at which the
first drop of a gaseous mixture beings to condense (Smith, Ness, & Aboitt, 2005). Both
of these are represented from the following equation:

: =

: =

Where;
yi = vapor mol fraction of component i,
xi = liquid mol fraction of component i,
Ki = equilibrium constant of component i

329
3.4.1.7 Calculation of Bubble Point

Table 3.2: Antoines constant for HCl and TFE (Sinnot & Towler, 2009)
Component A B C
HCl (1) 16.504 1714.25 -14.45
TFE (2) 15.88 1574.6 -27.22

Pressure (at reboiler) = 500 kPa = 3750.31 mmHg

xw1 = liquid molar composition of HCl at reboiler = 0.0136
xw2 = liquid molar composition of TFE at reboiler = 0.9864

Table 3.3: Result summary for calculation of bubble point

Operating pressure = 3750.31 mmHg
Component xwi Tsat (K) Tguess (K) Psat (mmHg) P2 sat Tnew yi
HCl (1) 0.0136 221.62 5745.02 0.0208
232.88 1.5407 3722.937 232.84
TFE (2) 0.9864 233.04 3728.72 0.9792
Total 1.0000

Hence, the boiling point is 232.84 K or -40.16C

3.4.1.8 Calculation for Dew Point

Pressure at condenser = 400 kPa = 3000.25 mmHg

yD1 = vapor mol composition of HCl at condenser
yD2 = vapor mol composition of TFE at condenser

330
 Table 3.4: Result summary for calculation of dew point
Operating pressure = 3000.25 mmHg
Component yDi Tsat (K) Tguess (K) Psat (mmHg) P1 sat Tnew xi
HCl (1) 0.9996 216.18 3000.80 0.9994
216.19 1.58 3000.95 216.19
TFE (2) 0.0004 227.21 1895.84 0.0006
Total 1.0000

Hence, the dew point is 216.19 K or -56.76C

3.4.1.9 Relative Volatility, AB

Relative volatility (AB) is an indicator that is used to measure the ease of separation
between components. This is defined as the ratio of concentration A in the vapor to
the concentration of A in the liquid divided by the ratio of concentration of B in the
vapor to the concentration of B in liquid. According to (Seader & Henley, 1998), AB
greater than 1 shows that separation is possible.

/
AB =
/

If the system is ideal, the equation can be simplified by relating with Raoults law to
become:

AB =

Where;
PA = vapor pressure of component A
PB = vapor pressure of component B

331
At bubble point:
5745.02
AB = =
3728.72
AB = 1.54
At dew point:

3000.80
AB = =
1895.84
AB = 1.58

Since AB is greater than 1, separation between HCl and TFE is possible.

3.4.1.10 Minimum Reflux Ratio, Rm

Minimum reflux ratio is the reflux ratio, R m that will require an infinite number of trays
to achieve the desired specification at the overhead and bottom streams. The ratio
can be calculated through the following equation:

1 (1 )
= [ ]
1 1
1 0.9996 1.58(1 0.9996)
= [ ]
1.58 1 0.6667 1 0.6667
= 2.57

3.4.1.11 Reflux Ratio, R

According to (Wauquier, 1998), the optimum value of Reflux ratio for a cryogenic
column that reaches -100C is 1.05Rmin.

= 1.05
= 1.05(2.57) = 2.70

332
3.4.1.12 Tray Efficiency

According to (Sinnot, 2005), the overall efficiency for the trays can be calculated using
OConnell correlation which states:

= 51 32.5 log(avg avg )

Where;
EO = Tray efficiency
avg = relative volatility at average column conditions
avg = average molar liquid viscosity, mNs/m 2

Table 3.5: Parameters for calculation of tray efficiency

Parameters Overhead Bottom
Viscosity, (mNs/m2) 0.2519 0.9144
Relative volatility, 1.58 1.54

+
avg =
2
0.2519 + 0.9144
avg = = 0.5832 /2
2

+
avg =
2
1.58 + 1.54
avg = = 1.56
2

Therefore,
= 51 32.5 [(0.5832)(1.56)] = 52.32%

According to (Douglas, 1988), typical values for tray efficiency range between 50% to
70%. Since the calculated tray efficiency is 53.32%, it is acceptable.

333
3.4.1.13 Theoretical Number of Stages using McCabe-Thiele Method

3.4.1.13.1 Vapor-Liquid Equilibrium

Assumption:
- System is ideal, hence Raoults law is applicable.

Table 3.6: Vapor-Liquid Equilibrium Data of HCl-TFE

Pressure Temperature Liquid mole fraction of Vapor mole fraction of

(kPa) (C) HCl, xHCl HCl, yHCl

400 -56.764 0.9996 0.9993

410 -56.161 0.9992 0.9984
412.759 -55.987 0.9983 0.9966
415.517 -55.799 0.9963 0.9927
418.276 -55.584 0.9923 0.9846
421.035 -55.313 0.984 0.9682
423.793 -54.933 0.9677 0.9364
426.552 -54.366 0.9379 0.8796
429.31 -53.526 0.8888 0.7900
432.069 -52.389 0.8186 0.6701
434.828 -51.042 0.7319 0.5357
437.586 -49.655 0.6385 0.4077
440.345 -48.374 0.5478 0.3001
443.103 -47.276 0.4662 0.2173
445.862 -46.369 0.3964 0.1571
448.621 -45.63 0.3386 0.1147
451.379 -44.91 0.2788 0.0777
454.138 -44.313 0.2289 0.0524
456.897 -43.811 0.1875 0.0352
459.655 -43.384 0.1535 0.0236
462.414 -43.016 0.1257 0.0158
465.172 -42.692 0.1028 0.0106
467.931 -42.402 0.0841 0.0071
470.69 -42.141 0.0689 0.0047
473.448 -41.901 0.0563 0.0032
476.207 -41.678 0.0461 0.0021

334
 478.966 -41.469 0.0377 0.0014
481.724 -41.271 0.0308 0.0009
484.483 -41.083 0.0252 0.0006
487.241 -40.901 0.0205 0.0004
*Refer to sample
*Values obtained from Aspen HYSYS
calculation

Sample calculation:

Partial pressure of HCl at 400 kPa:

Using Raoutls law:
=

Where;
pi = partial pressure of component i
Pi = vapor pressure of pure component i

=
= 0.9996(400) = 399.84

Vapor mole fraction of HCl at 400 kPa:

=


=

(400 )0.9996
= = 0.9993
399.84

335
 VLE Diagram of HCl-TFE
1.2000

1.0000

0.8000
Vapor mol fraction, y

0.6000

0.4000

0.2000

-
0.0000 0.2000 0.4000 0.6000 0.8000 1.0000 1.2000
Liquid mol fraction, x

Figure 3.4: VLE diagram of HCl-TFE

3.4.1.13.2 Enriching operating line, yn+1

The enriching section of equilibrium stages extends from the top stage to just above
the feed stage. The equation which produces the most useful form of the operating
line for the enriching section is as follow:

+1 = +
+1 +1
2.70 0.9996
+1 = +
2.70 + 1 2.70 + 1
= 0.73 + 0.27

336
3.4.1.13.3 q-line Equation

The term q refers to the quality of feed condition or also the enthalpy change to bring
the feed to dew point vapor over the enthalpy of vaporization of the feed. The equation
that describes this is as shown below:

1
=


=

( ) + ( )
=

Where;
Hv = enthalpy of feed at dew point
HF = enthalpy of feed at at its entrance conditions
HL = enthalpy of feed at boiling point (bubble point)
CpL = specific heat capacity of feed
TB = boiling point of feed
TF = inlet feed temperature

Table 3.7: Parameters for calculation of q-line

Parameter Value
Specific heat capacity of feed, cpL 120.3 kJ/kmolC
Enthalpy of feed, HF 61,730 kJ/kmol
Enthalpy of feed at dew point, HL 28,640 kJ/kmol
Enthalpy of feed at bubble point, HV 126,600 kJ/kmol
Boiling point of feed, TB -40.16C
Feed temperature, TF -50C

(126,600 28,640) + 120.3[40.38 (50)]

=
(126,600 61,730)
= 1.52

337
Therefore, q-line equation:

=
1 1
1.52 0.6667
=
1.52 1 1.52 1
= 2.91 1.28

3.4.1.13.4 Theoretical Number of Stages

Using the McCabe-Thiele method, the q-line and enriching operating line were drawn
on top of the VLE diagram. Based on the Figure 3.5, the number of stages obtained
is 9, including a reboiler.

VLE Diagram of HCl-TFE -

Theoretical Number of Stages
1.2000

1.0000
Vapor mol fraction, HCl, y

0.8000

0.6000

0.4000

0.2000

-
0.0000 0.2000 0.4000 0.6000 0.8000 1.0000 1.2000
Liquid mol fraction, x

Figure 3.5: Theoretical number of stages for T-101

338
3.4.1.13.5 Minimum Number of Theoretical Stages, Nm

Total reflux is defined as a condition whereby all of the condensate is fed back to the
column and no product is taken off as well as there is no feed. The minimum number
of theoretical stages can be determined using the VLE diagram as shown in Figure
3.6.

VLE Diagram of HCl-TFE

1.2000

1.0000

0.8000

0.6000

0.4000

0.2000

-
0.0000 0.2000 0.4000 0.6000 0.8000 1.0000 1.2000

Figure 3.6: Minimum theoretical number of stages

Hence, the minimum theoretical number of stages required when a total condenser is
used is 7.

339
3.4.1.13.6 Actual Number of Stages

The actual number of stages can be calculated using the following equation (Sinnot,
2005):

( )
=
( )
9 1 ( )
= =
0.5232
16

3.4.1.14 Feed Stage Location

The location where the feed is introduced into the column can be calculated using
Kirkbrides equation (Geankoplis, 2014):

2
log ( ) = 0.206 [( )( )( ) ]

Where;
Ne = theoretical number of stages above the feed plate
Ns = theoretical number of stages below the feed plate
xHF = liquid mole fraction of heavy key component at feed
xLF = liquid mole fraction of light key component at feed
W = molar flowrate at distillate
D = molar flowrate at bottom
xLW = liquid mole fraction of light key component at bottom
xHD = liquid mole fraction of heavy key component at distillate

0.3333 24.06 0.0136 2

log ( ) = 0.206 [( )( )( ) ]
0.6667 47.19 0.0004

340

= 3.22

= 3.22 . (1)
+ = = 9 . (2)
Substitute (1) into (2)

+ 3.22 = 16
4.22 = 16
4 (3)

Substitute (3) into (2)

4 + = 16
12

Hence, the feed point location is 4th tray from the top or 12th tray from the bottom.

3.4.1.15 Average Molecular Weight

Table 3.8: Molecular weight and composition of each component

Component Molecular Feed Distillate Bottom
Weight Composition Composition Composition
(g/mol) (xF) (xD) (xW)
HCl 36.45 0.6667 0.9996 0.0136
TFE 100.02 0.3333 0.0004 0.9864

The relative molecular weight can be calculated by:

Where;
MW = molecular weight of component (g/mol)

341
xi = mass fraction of component i (kg/kg)
At feed:

= (36.54 ) (0.6667) + (100.02 ) (0.3333)

= 57.64 /

At top (overhead) section:

= (36.54 ) (0.9996) + (100.02 ) (0.0004)

= 36.48 /

At bottom section:

= (36.54 ) (0.0136) + (100.02 ) (0.9864)

= 99.16 /

3.4.1.16 Vapor and Liquid Density

The liquid and vapor density can be calculated using the following equations:

At feed:

: , = ,

: , =

At top (overhead) section:

: , = ,

342

: , =

At bottom section:

: , = ,

: , =

Table 3.9: Density and composition of each component

Component Density (kg/m3)
HCl 1.49
TFE 1520

At feed:

: , = (1.49 3 ) (0.6667) + (1520 3 ) (0.3333)

, = 507.61 /3

57.64 273 6
: , =
22.4 223 1
, = 18.90 /3

At top (overhead) section:

: , = (1.49 3 ) (0.9996) + (1520 3 ) (0.0004)

, = 2.10 /3

36.48 273 4
: , =
22.4 216.24 1
, = 8.22 /3

343
At bottom section:

, = (1.49 3 ) (0.0136) + (1520 3 ) (0.9864)

, = 1499.35 /3

99.16 273 5
: , =
22.4 232.83 1
, = 25.95

3.4.1.17 Vapor and Liquid Flowrate

Table 3.10: Vapor and liquid flowrate at distillate and bottom

Stream Liquid flowrate (kmol/h) Vapor flowrate (kmol/h)
Distillate 1436.00 1483.00
Bottom 1534.00 1510.00

3.4.1.18 Column Sizing

3.4.1.18.1 Liquid and Vapor Streams in the column

Above feed point,

, = ( + 1)
, =

Where;
D = distillate flowrate, kmol/h
R = reflux ratio

= 47.19 (2.70 + 1)


= 174.49

344

= 174.49 47.19


= 127.30

Below feed point,

, = +
, =

Where;
F = feed molar flowrate
W = bottom molar flowrate

= 127.30 + 71.26


= 198.56

= 198.56 24.06


= 174.50

3.4.1.18.2 Liquid Flow Factor, FLV

0.5

= ( )

Where;
FLV = liquid flow factor
v = density of vapor, kg/m3
L = density of liquid, kg/m3

345
At top section:
0.5

127.30 8.22 3
() = ( )

174.49 2.10 3

() = 1.44

At bottom section:

0.5
198.56 25.95
() = ( 3 )

174.50 1499.35 3

() = 0.15

Figure 3.7: Flooding velocity, sieve plates

As initial guess, assume plate spacing is 0.6 m. Referring to Figure 3.7, the K values
are:

1 () = 0.09
1 () = 0.028

346
3.4.1.18.3 Flooding Velocity

( ) 0.5
= 1 [ ]

Where;
uf = flooding velocity, m/s
v = density of vapor, kg/m3
L = density of liquid, kg/m3

At top section:
8.22 2.10 0.5
() = 0.09 [ ]
8.22
() = 0.08 /

At bottom section:
1499.35 25.95) 0.5
() = 0.028 [ ]
25.95
() = 0.21 /

According to (Sinnot, 2005), the velocity is normally between 70% to 90% of that which
would cause flooding. Using 90% as basis of calculation

() = 0.08 90% = 0.07


() = 0.21 90% = 0.19

347
3.4.1.18.4 Volumetric Flowrate, Q

( )
=

Where;
Vm = vapor flowrate, kmol/h
MW = molecular weight, kg/kmol
v = density of vapor, kg/m 3

At top section:

36.48
(1483 ) 1

() =
3600
8.22 3

() = 1.83 3

At bottom section:

99.16
(1510 ) 1

() =
3600
25.95 3

() = 1.60 3

3.4.1.18.5 Area of Column

Where;
Q = volumetric flowrate, m 3
uf = flooding velocity, m/s

348
At top section:

3
1.83
() =

0.06

() = 26.14 2

At bottom section:
3
1.60
() =

0.19

() = 8.44 2

Hence, diameter of column:

4()
=

At top section:

4(30.16 2 )
() =

() = 5.77

At bottom section:

4(8.44 2 )
() =

() = 3.28

For the design, the overall diameter is taken as 3.28 m.

Add 10% for safety margin:

= 3.28 1.1
= 3.61

349
3.4.1.18.6 Column Height

=
= 16 0.6 = 9.17

According to (Geankoplis, 2014), the general rule of thumb for calculating column
height is to add 1.2 m to the top to minimize entrainment and extra spacing for man
hole and add 1.8 m at the bottom of the reboiler.

= 9.17 + 1.2 + 1.8 = 12.17

Add 10% for safety margin:

= 12.17 1.1
= 13.39

3.4.1.19 Justification for Column Diameter and Height

According to (Turton et al., 2013), the ratio of height to diameter for a distillation
column should be less than 20.

=

13.39
= = 3.71
3.61

Since the ratio obtained is less than 20, the calculated diameter and height is
acceptable.

3.4.1.20 Selection of Plate

The selection of plate type is an important factor which will determine the overall
separation efficiency of the distillation column. There are various types of plates used
within the chemical industry such as sieve plate (perforated plate), bubble cap plate

350
and valve plates. Table 3.11 presents a comparison summary between different types
of plates (Geankoplis, 2014).

Table 3.11: Comparison between different types of plates

Parameter Bubble-cap Tray Sieve Tray Valve Tray

Capacity Moderately high High Very high

Pressure drop High Moderate

Moderate
High
Efficiency Moderately high High

High
(approximately 2 20% more
Cost to 3 times more Low expensive than
expensive than Sieve Tray
Sieve Tray)
Maintenance
Relatively high Low
requirement Moderate
High. Tends to
Fouling tendency Low
collect solids. Moderate
Effects of High
Low
corrosion Moderate

Hence, the type of plate that will be used for this unit will be sieve plate as it has the
most advantages such as high capacity and efficiency as well as low cost,
maintenance, fouling and corrosion tendency.

3.4.1.21 Plate Areas

The necessary areas that needs to be calculated when designing the plates are
Ac = column cross-sectional area,
Ad = cross sectional area of downcomer
An = net area
Aa = bubbling area
Ah = hole area, total area of all the active holes

351
 Table 3.12: Summary of plate areas
Cross sectional area, Ac 2
=
4
(3.61)2
= = 10.21 2
4

Cross-sectional area of downcomer, Ad The downcomer area is assumed to be

12% of the total cross-sectional area

= 12% 10.21 2 = 1.23 2

Net Area, An =
= 10.21 1.23 = 8.99 2
Active (Bubble) Area, Aa = 2
= 10.21 2(1.23) = 7.76 2

Hole Area, Ah Assume hole area is 10% of active area

= 10% 7.76 = 0.78 2

3.4.1.22 Number of Holes per Tray

According to (Sinnot, 2005), hole sizes vary from 2.5 mm to 12 mm; however, 5 mm
is the preferred size. Using 5 mm as basis of calculation:

Area of one hole:

2
=
4
(12 103 )2
=
4
= 1.964 105 2

352
Number of holes:

=

0.78 2
=
1.964 105 2
= 39,499

For 16 trays,

39,499
=
16
= 2469

3.4.1.23 Weir Length, lw

100%

Where;
Ad = downcomer area, m2
Ac = column area, m2

1.23
= 100% = 12%
10.21

353
 Figure 3.8: Relation between weir length and downcomer area (Sinnot, 2005)

Referring to Figure 3.8, when Ad/Ac = 12%, the value of lw/Dc is 0.76.

= 0.76

= 0.76(3.61 )
= 2.74 `
3.4.1.24 Check Weeping

=
3600

Where;
F = feed molar flowrate
MW = molecular weight of feed (kg/kmol)

354

71.26 57.64
: = = 1.14

3600

For minimum liquid flowrate, take 70% as turn down ratio (Sinnot, 2005):

: = 1.14 0.70 = 0.80

3.4.1.25 Weir Liquid Crest, how

2
3
= 750 ( )

Where;
how = weir crest, mm liquid
lw = weir length, m
Lw = liquid flow rate, kg/s
L = liquid density at feed, kg/m3

2
3
1.14
, = 750 [ ]

507.61 3 (2.74 )

= 6.87

2
3
0.80
, = 750 [ ]

507.61 3 (2.74 )

= 4.81

At minimum rate, clear liquid depth:

+ = 6.87 + 4.81
+ = 11.67

355
Referring to Figure 3.9.

Figure 3.9: Weep point correlation

When how + hw = 11.24 mm,

2 = 27.4

3.4.1.26 Weep Point

According to (Sinnot, 2005), the lower limit of the operating range occurs when the
liquid leakage through the plate holes become excessive.

Minimum design vapor velocity is given by:

2 0.9(25.4 )
= [ ]
0.5

Where;
= minimum vapor velocity through the hole, m/s
v = vapor density at bottom, kg/m 3

356
dh = hole diameter, mm
K2 = constant, dependent on the depth of clear liquid on the plate, obtained from Figure
3.9

27.4 0.9(25.4 5.00 )

= [ ]
(25.95)0.5
= 1.77 /

The minimum vapor velocity through the hole is compared against the operating vapor
velocity:

,
() =

Where;
Q = volumetric flowrate, m 3/s
Ah = hole area, m2
3
1.83
() =
0.78 2
() = 2.36 /

The actual vapor velocity is greater than minimum vapor velocity. Hence, weeping will
not occur.

3.4.1.27 Plate Pressure Drop

As initial guess, assume:

Weir height, hw = 50 mm
Plate thickness = 5 mm
Hole diameter, dh = 5 mm

5.00
= =1
5.00

357
Percent perforated area:

0.78
100% = 100%
7.76
= 10%

Based on Figure 3.10,

Figure 3.10: Relationship between orifice coefficient and sieve plates

When Ah/Aa = 10%, orifice coefficient (Co) = 0.84

Dry pressure drop, hd:

2
= 51 ( ) ( )

Where;
= actual vapor velocity through the hole, m/s
Co = orifice coefficient

358
v = vapor density at bottom, kg/m 3
L = liquid density at bottom, kg/m 3

2
2.36 25.95 3
= 51 ( ) ( )
0.84
1499.35 3

= 7.11

Residual head, hr
(12.5 103 )
=

(12.5 103 )
=

1499.35 3

= 8.34

Total pressure drop, hT:

= + + ( + )
= 7.11 + 8.34 + 6.61 + 4.63
= 27.12

3.4.1.28 Downcomer Liquid Backup

Down comer pressure drop, hap:

= 10

Where;
hw = wier height, mm
= 50 10
= 40

359
Area under downcomer, Aap:

= 40 103 (2.74)

= 1.10 2

Downcomer area, Ad = 1.22

Since Aap < Ad, Ad will be used to calculate head loss in downcomer, hdc:

2
= 166 ( )

Where;
Lw = liquid flowrate below feed point, kg/s
L = liquid flowrate ate bottom, kg/m 3

2
5.47
= 166 [ ]
1499.35(1.22)
= 0.0018

Back up in the downcomer, hb:

= + + +
= 6.61 + 4.63 + 25.25 + 0.0018
= 38.80 @ 0.39

Check,
1
0.39 < ( + )
2
1
0.39 < [0.6 + (50103 )]
2
0.39 < 0.55

So, tray spacing is acceptable to avoid flooding.

360
3.4.1.29 Residence Time, t

=

Where;
Ad = downcomer area, m 2
hb = head loss in downcomer, m
L = liquid density at feed, kg/m3
Lwd = maximum liquid flowrate, kg/s

1.23 2 (0.39 )(507.61 /3 )

=

1.14

= 211.41 @ 3.52

According to (Sinnot, 2005), the residence time should be greater than 3s. Hence, it
is acceptable.

3.4.1.30 Check Entrainment

Actual velocity (based on net area),

=
An
Where;
Q = volumetric flowrate, m 3/s
An = net area, m2
3
1.60
=
8.99 2
= 0.18 /

361
Percentage flooding:

0.18
100% = 100%
0.19
= 94.74%

Figure 3.11: Entrainment correlation for sieve plates

Based on Figure 3.11 When FLV (top) = 0.15 and percentage flooding is 94.74%,

= 0.052

According to (Sinnot, 2005), when < 0.1, the column diameter is acceptable.

3.4.1.31 Perforated Area

2.74
= = 0.76
3.61

362
 Figure 3.12: Relation between angle subtended by chord, chord height and chord
length

Based on Figure 3.12, when lw/Dc = 0.76, = 100

Angle suspended at plate edge by unperforated strips:

180 100 = 80

363
3.4.1.32 Summary of Chemical Design for T-101

Table 3.13: Summary of chemical design

Specifications Value Unit

Design data
Feed 71.26 kmol/h
Distillate 47.19 kmol/h
Bottom 24.06 kmol/h
Key components
Heavy component TFE
Light component HCl
Bubble point (at reboiler) -40.16 C
Dew point (at condenser) -56.81 C
Theoretical number of trays 9 trays
Minimum theoretical number of trays 7 trays
Actual number of trays 16 trays
Tray efficiency 52.32 %
Feed point location 4th tray from top
Minimum relfux ratio 2.57
Column diameter 3.28 m
Column diameter (10% margin) 3.61 m
Column height 12.17 m
Column height (10% margin) 13.39 m
Column area 10.21 m
Plate design
Type of plate sieve plate
Downcomer area 1.22 m2
Net area 8.98 m2
Active area 7.76 m2
Hole area 0.78 m2
Diameter of one hole 5 mm
Number of holes per plate 2469 holes
Weir
Weir height 50.00 mm
Hole diameter 5.00 mm
Plate thickness 5.00 mm
Weir length 2.74 m
Weir liquid crest
Minimum vapor velocity 1.77 m/s
Weep point 2.36 m/s

364
 Table 3.13: Summary of chemical design (cont.)

Plate pressure drop

Dry pressure drop 7.11 mm of inch water
Residual head 8.34 mm of inch water
Total pressure drop per plate 27.12 mm of inch water
Downcomer design
Downcomer pressure drop 40 mm of inch water
Back up in downcomer 38.80 mm of inch water
Residence time 3.52 min

365
3.4.2 MECHANICAL DESIGN

3.4.2.1 Design Pressure

When designing an equipment, it is important to consider the safety margin so that it

could compensate the effect of external disturbances or unpredictable circumstances.
This is particularly useful for equipment used in chemical industries as it involves
higher risks such as explosion, toxic release and others.

= 6

Consider a safety margin of 10% for design pressure:

= 10% 6
= 6.6
= 0.66 /2

3.4.2.2 Material of Construction

The strength of material depends greatly on the operating temperature and

components present within the equipment. Hence, the type of material used should
be able to withstand the corrosive nature of the component and operating temperature
so that it will not damage easily and cause equipment failure.

= 56.76
= 216.24

Table 3.14: Components present in T-101

Component Feed Overhead Bottom

TFE (kg/kg) 0.5783 0.0001 0.995

HCl (kg/kg) 0.4217 0.9999 0.005

366
 Referring to (Dillon, 1991) the most suitable type of material for the
construction of this equipment would be molybdenum-nickel alloy or also known as
Hastelloy B2 (N010665). This is because Hastelloy is able to withstand the corrosive
nature of HCl whereas other metals and alloys do not possess the resistivity.

Table 3.15: Maximum allowable stress at different temperature

Temperature (C) Maximum Allowable Stress (S) (ksi)

-56.76 x
25.00 131.00
204.00 126
Source: ("Hastelloy B2 Fasteners," 2016)

Interpolating,

= 132.80
= 919.08 /2

Therefore, the maximum allowable stress for Hastelloy at -40.17C is 919.08 N/mm2.

3.4.2.3 Vessel Wall Thickness

For cylindrical vessel,

=
2 1,2

Where;
tc = column wall thickness, mm
E = joint efficiency (assume double welded butt joint or equivalent)
Di = column diameter, mm
S = maximum allowable stress, N/mm 2

367
Based on previous calculation,
Di = 3.82 m

(0.55 /2 )(3.61 103 )

=
2(919.08 /2 )(1) 1.2(0.66/2 )
= 1.30

Add 2 mm for corrosion allowance. Hence, actual thickness:

= 1.30 + 2
= 3.30

3.4.2.4 Weight of Vessel, Wv

For cylindrical vessel, weight of vessel can be calculated using the following formula
(Sinnot and Towler, 2009):

= 240 ( + 0.8 )

Where;
Wv = total weight of the shell, excluding internal fittings, such as plates, kN
Cw = a factor to account for the weight of nozzles, manways, internal supports, etc;
which can be taken as 1.15 for distillation column
Hc = height, or length, between tangent lines (the length of the cylindrical section), m
Dm = mean diameter of vessel = (Dc + tc 10-3), m
Dc = column diameter, m
tc = wall thickness, m

Based on earlier calculation, Hc = 13.39 m

= 3.61 + (3.30 103 )

= 3.61

368
 = 240(1.15)(3.61 )[13.39 + 0.8(3.61 )](3.30 103 )
= 53.51

3.4.2.5 Weight of Plates, Wp

2
, =
4
(3.61)2
=
4
= 10.21 2

According to (Sinnot and Towler, 2009), contacting plates, steel, including typical liquid
loading is 1.2 kN/m 2 plate area.

= 1.2 10.21
= 12.26

For 16 plates,
= 12.26 16
= 196.08

3.4.2.6 Weight of Insulation, Wins

Referring to ("Corrosion Resistant Products," 2013), fiberglass would be the most

suitable type of insulation as it is able to withstand corrosive materials such as HCl.

, = 100 /3

Assume thickness of insulation, tins as 75 mm

Volume of insulation, Vins:

369
 = (3.61 )(13.39 )(75 103 )
= 11.38 3

Weight of insulation, W ins:

= 9.81


= 11.42 3 9.81 100 3

= 11,162.76

Double this to allow for fitting,

= 11,162.76 2
= 22.3

3.4.2.7 Weight of Column

= + +
= 53.51 + 196.08 + 22.3
= 271.92

3.4.2.8 Wind Loading

Take dynamic wind pressure as 1280 N/m 2 which corresponds to 100 mph.

Mean diameter, including insulation:

= + 2( + )

= 3.61 + 2[(3.30 + 75)(103 ) ]

= 3.76

370
Loading per unit length:

=

= 1280 3.76
2
= 4815.79 /

Bending moment:

2
= ( )
2
4815.79
= (13.392 )
2
= 431,837.08
= 431.84

3.4.2.9 Analysis of Stress

At bottom tangent line,

Pressure stress:

=
4
(0.66 /2 )(3.61 103 )
=
4(3.30 )
= 180.28 /2

=
2
(0.66 /2 )(3.61 103 )
=
2(3.30 )
= 360.56 /2

371
Dead weight stress:

=
( + )
271.92 103
=
(3610 + 3.30)3.30
= 7.27 /2 ()

Bending stresses:

= + 2
= 3610 + 2(3.30)
= 3616.6

4
= ( 4 )
4

= (3616.6 4 36104 )
4
= 6.08 1010 4

= ( + )
2
431,837.08 103 3610
= ( + 3.30)
6.08 1010 2
= 12.82 /2

The resultant longitudinal stress is:

= +

() = 180.28 + 7.27 + 12.82

() = 200.64 /2

372
 () = 180.28 + 7.27 12.82
() = 175.00 /2

200.64 N/mm2 175.00 N/mm2

360.56 N/mm2 360.56 N/mm2

Up-wind Down-wind

The greatest difference between the principal stresses will be on the down-wind side

= 360.56 175.00
= 186.09 /2

Check failure against the maximum allowable stress:

186.09 /2 < 919.08 /2

Hence, bending will not occur and choice of material is acceptable.

3.4.2.10 Type of Head

Flat head:

= + 2 ( )

373
Where;
th = head thickness, mm
De = nominal plate diameter, mm
C = a design constant; 0.1
S = maximum allowable stress
E = joint efficiency (assume double welded butt joint or equivalent)

0.1(0.66 /2 )
= 3610 +2
915.63 /2 (1)

= 32.61

Hemispeical head:

= + 2 ( )
4 0.4
0.66 /2 (3610 )
= +2
4(915.63 /2 )(1) 0.4(0.66 /2 )
= 2.65

Ellipsoidal head:

= + 2 ( )
2 0.2
0.66 /2 (3820 )
= +2
2(915.63 /2 )(1) 0.2(0.66 /2 )
= 3.30

Hence, ellipsoidal head is the most suitable type of head because it has the same
thickness as the column wall.

374
3.4.2.11 Check Elastic Stability (buckling)

Critical buckling stress:

= 2 104 ( )

3.30
= 2 104 ( )
3610
= 18.30 /2

When the vessel is under pressure (where maximum stress occurs):

= +
= 12.82 + 7.27
= 7.29 /2

The maximum stress is well below the critical buckling stress. Hence, design is
acceptable.

3.4.2.12 Choice of Vessel Support

According to (Sinnot, 2005), there are 3 types of support, which are:

Skirt support used for tall and vertical column

Brackets, or lugs; used for all types of vessel
Saddle support; used for horizontal vessel

Since the design is for a distillation column, hence skirt support would be the most
suitable type of vessel support.

375
3.4.2.13 Design of Skirt Support

Figure 3.13: Skirt support design

Table 3.15: Description of skirt support

Type of support straight cylindrical skirt (s = 90)

Material of construction carbon steel

Yield stress (at 20C), fs 89.43 N/mm2
Youngs modulus 120,000 N/mm2
Density of liquid, L 507.61 kg/m3

The maximum dead weight load on the skirt will occur when the vessel is full of liquid:

2
, =
4

Where;
Dc = column diameter, m g = gravitational acceleration, m/s
L = density of liquid, kg/m 3
hs = height of skirt, m

376
According to (Sinnot, 2005), for vessels with 3.6 m diameter, the skirt and thickness
of skirt support should be 1.78 m and 12 mm, respectively

(3.61 )2
= (1.78 )(507.61 /3 )(9.81 / )
4
= 90,521.87
= 90.52

Total weight:
= +
= 271.92 + 90.52
= 362.36

Bending moment at base of skirt:

( + )2
=
2
(13.39 + 1.78)2
= 4815.79
2
= 554.26

Bending stress at skirt:

4
=
( + )

Where;
Ds = diameter of skirt (assume = Dc)
ts = skirt thickness, 12 mm

4(554.26 103 103 )

=
(3610 + 1)(12)(3610)
= 4.51 /2

377

() =
( + )
554.26 103
() =
(3610 + 12)(12)
() = 2.66 /2

() =
( + )
271.92 103
() =
(3610 + 12)(12)
() = 1.99 /2

Maximum s (compressive):

() = + ()

() = 4.51 + 2.66
() = 7.16 /2

Maximum s (tensile):

() = ()

() = 4.51 1.99
() = 2.51 /2

3.4.2.14 Design Criteria

Take joint factor (J) as 1,

(, ) <
6.69 /2 < 89.43(1) sin(90)
7.16 /2 < 89.43

378

(, ) < 0.125 ( )

15
2.61 /2 < 0.125(200,000)( )(sin 90)
3610
2.51 /2 < 92.98

Both criteria are satisfied. Hence, diameter and thickness of skirt is acceptable.

3.4.2.15 Base Ring and Anchor Bolts

According to (Sinnot, 2005), several factors should be considered, such as:

1. Bolts smaller than 25mm in diameter should not be used.

2. Minimum number of bolts is 8.
3. Use multiple of 4 bolts.
4. Bolt pitch should not be less than 600mm.

Table 3.17: Design of base ring and anchor bolts

Number of bolts required, Nb 3762.34
=
600
= 19.70
Closest multiple of 4 is 5 bolts
Approximate pitch circle, D b = + 2( + )
= 3610 + 2(3.30 + 75)
= 3762.34
Circumference of bolt circle 3762.34
Recommended spacing between bolt 600
Bending moment at skirt base, Ms 554.26
Total weight of column, Wc 271.92
Bolt design stress, Sb 125 /2

379
Area of bolt, Ab:

1 4
= [ ]

1 4(554.26 103 )
= [ (271.92 103 ) ]
5(125) (3762.34 103 )
= 515.56 2

Table 3.18: Bolt size

Based on Figure 3.18, it is estimated that the bolt size is of M30, as it is closest to the
calculated bolt area.

Bolt root diameter:

4
=

515.56 4
=

= 25.62

380
According to (Sinnot, 2005), total compressive load on the base ring per unit length
can be estimated by:

4
= +
D2s Ds

Where;
Ds = skirt diameter, m
Wc = weight of column, kN

4(554.26 103 ) 271.92 103

= +
(3.61)2 (3.61)
= 78.27 /

Minimum width of base ring, Lb,min:

1
=
103
Where;
fc = maximum allowable bearing pressure on the concrete foundation pad. Typically
ranges from 7 N/mm2 to 305 N/mm2

78.27 103 1
, = 3
7 10
, = 11.18

Actual width required, Lb:

= + + 50
= 150 + 12 + 50
= 212

381
Actual bearing on concrete foundation,

=

78.27 103
=
212 103
= 0.37 /2

Thickness of bolt, tb:

3
= 150

Where;
fr = allowable stress in the ring material, typically 140 N/mm2

3(0.37)
= 150
140

= 14

3.4.2.16 Pipe Design

The optimum diameter for carbon steel pipe:

= 293 0.53 0.37

Where;
G = mass flowrate, kg/s
= density, kg/m3

, =
20 +

382
Where;
P = internal pressure, 0.154 N/mm 2
= design stress at working temperature, 120 N/mm 2

Table 3.19: Summary of pipe design for feed, top and bottom
Nominal
Density Mass flowrate doptimum t
pipe size
Stream (kg/m3) (kg/s) (mm) (mm)
Feed 263.25 1.14 39.97 0.0026 40
Top 5.16 0.48 108.00 0.0069 125
Bottom 762.65 0.66 20.22 0.0013 25

Table 3.20: Typical standard flange design

Figure 3.14: Dimensions of flange

383
3.4.2.17 Summary of Mechanical Design for T-101

Table 3.20: Summary of mechanical design

Specification Value Unit
Design operation
Molybdenum-nickel alloy
Material of construction (Hastelloy B2 )
Type of insulation fibreglass
Operating pressure 6 bar
Design pressure 6.6 bar
Design temperature -56.76 C
Resultant longitudinal stress 47.28 N/mm2
Maximum allowable stress 919.08 N/mm2
Minimum thickness 1.30 mm
Corrosion allowance 2.00 mm
Design of head and closure
Type of head Ellipsoidal
Joint factor 1
Minimum thickness 1.30 mm
Corrosion allowance 2.00 mm
Column weight
Weight of vessel 53.53 kN
Weight of plates 196.08 kN
Weight of insulation 22.33 kN
Total weight 271.84 kN
Bending moment 431.84 kNm
Design of support
Type Skirt
Material of construction Carbon steel
Angle 90
Support thickness 12.00 mm
Support height 1.78 m
Elastic stability
Critical buckling stress 18.28 N/mm2
Maximum compressive stress 7.29 N/mm2
Design of base ring and anchor bolts
Pitch circle diameter 3762.33 mm
Number of bolts 5 bolts
Area of bolts 515.58 mm2
Bolt diameter 25.62 mm
Base ring thickness 13.34 mm

384
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387