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Design of o-xylene Plate/Tray Distillation Column

Technical Report · February 2017


DOI: 10.13140/RG.2.2.26922.41929

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CH 4033 Comprehensive Design Project(Individual)
Final Report
Design of o-xylene Plate/Tray Distillation Column
Para-Xylene Manufacturing Plant

NAME : W.M.H.E. WIJESINGHE


INDEX NO : 120722J

Supervisors : Dr. Walpolage S.


Date of Submission : February 13th, 2016

Department of Chemical and Process Engineering


University of Moratuwa
ACKNOWLEDGEMENT
I would make this an opportunity to convey my gratitudes to everyone who was behind the
successful completion of this design.

Among them, first and foremost I extend my heartfelt gratitude to Dr. S. Walpolage, my
supervisor for the encouragement and the motivation given to expand our vision regarding the
industrial importance of proper process designing. If not for the motivation provided by my
supervisor, this report wouldn’t have been a reality.

Also, I must be thankful to Professor Padma Amarasinghe, the module coordinator for always
guiding and encouraging me to do my best.

I would also like to extend my sincere gratitude to the academic staffs of the Department of
Chemical and Process Engineering, for their support on completing this project.

Last but not least, I am thankful to my fellow colleagues of my department for the friendly
support given to complete this report successfully.

ii
ABSTRACT
Para-xylene is a commercial isomer of xylene. It is a hydrocarbon, based on benzene with two
methyl substituents bonded to the aromatic ring. Para-xylene production process has several
unit operations and distillation is one of the most important.

o-xylene is a byproduct of the para-xylene production process. Being a commercial product,


proper recovery of otho-xylene is important. The o-xylene recovery column designed in this
report is an intermediate process which is used to recover 99.9% (mole basis) of o-xylene as a
liquid. The feed to the designed column, which is a mixture of xylenes, aromatics (A9, A10,
A11) and i-paraffin is fed to the 9th plate of the column, from which the desired product is
recovered.

The designed distillation column is a plate/tray multicomponent distillation column with a


total condenser and a partial reboiler. The operating pressure is 340kPa and average
temperature in the column is 222℃. It operates at a reflux ratio of 0.4 and height of the column
is 13.80m. The internal diameter of the rectifying section is 1.34 m and that of the stripping
section is 1.16m. The column consists with 23 sieve plates with holes having a diameter of
5mm. Also, down comer area, weir height, weir length, active area and number of holes in a
sieve plate are also have been calculated in this report.

Column is fabricated using carbon steel SA-299 with a design stress of 148MPa. The calculated
values of nominal plate thicknesses of shells and reducers are 7.94mm (5/16 inch) and 6.35mm
(1/4 inch) respectively. Two ASMI coded tori-spherical heads are designed for the top and the
bottom with plates of 7.94mm (5/16 inch) nominal thickness.

Openings are constructed for feed in, reflux in, top vapor out, bottom vapor in and out with
suitable dimensions. Two man holes are fabricated at the top and the bottom of the column to
access into the column for servicing. The vessel as well as the pipe lines are insulated with an
insulation layer made up of glass mineral wool with a nominal thickness of 12.7 cm (5 inch.).
Combined loading and principle stress calculations are done to verify the thickness is able to
handle the stresses due to combined loadings. A skirt support with a height of 3m is provided
along with the basement and foundation. M30 bolts are chosen to fix the support to the
basement based on acceptable conditions. Methods of fabrication also have been discussed.

Pipes are designed for the feed flow, vapor out, reflux in, bottom product out and bottom vapor
in using standard ASMI schedule. Carbon steel SA-299 is selected to manufacture pipes. Plug

iii
valves are selected as shut-off valves and globe and butterfly valves are selected as control
valves. Flow, pressure, level of the column and pressure equipment are selected according to
safety standards. An orifice plate is selected for measuring flow rates and diaphragm pressure
indicators and sensors are selected in here for controlling the operation safely. Platinum
resistance temperature detectors are selected as temperature sensors. Centrifugal pumps are
selected to pump top and bottom products. Carbon steel Y strainers are installed in each pump
to protect them from sediments and impurities. Also, pressure indicators are installed in each
pump in and out for easy maintenance.

Classical feedback control structure is used to control the flow, temperature, pressure and level.
Detailed drawing of P & I diagram, is attached with the report. All startups, shutdowns and
emergency shutdown procedures are discussed in here. Safety aspects are discussed under
headlines of personal protection, fire measures, accidents release measures and handling and
storage. A HAZOP study has also been done to inspect the safety of operation. Total capital
cost of the distillation column is calculated in detail.

Economic aspects are being considered and the total capital cost investment is found as 85.818
million LKR.

iv
CONTENTS

ACKNOWLEDGEMENT .........................................................................................................ii
ABSTRACT ............................................................................................................................. iii
CONTENTS ............................................................................................................................... v
LIST OF TABLES .................................................................................................................... ix
LIST OF FIGURES ................................................................................................................... x
CHAPTER 1 - INTRODUCTION ........................................................................................ 1
1.1 Comprehensive Design Group Project ........................................................................ 1
1.2 Comprehensive Design Project - Individual ............................................................... 3
CHAPTER 2 - LITERATURE SURVEY............................................................................. 4
2.1 Distillation ................................................................................................................... 4
2.1.1 Types of Distillation ............................................................................................ 4
2.2 Type of Distillation columns ....................................................................................... 5
2.2.1 Plate/Tray Column .............................................................................................. 5
2.2.2 Packed Bed Columns ........................................................................................... 7
CHAPTER 3 - DISTILLATION COLUMN SELECTION.................................................. 8
3.1 Selecting the column type ........................................................................................... 8
3.1.1 Selection of Tray Type......................................................................................... 8
3.1.2 Vapor flow Condition .......................................................................................... 9
3.1.3 Selection of the condenser and reboiler type ..................................................... 10
CHAPTER 4 - CHEMICAL DESIGN OF THE COLUMN .............................................. 11
4.1 Material Balance ....................................................................................................... 11
4.2 Determination of the minimum reflux ratio and product compositions under
minimum reflux ratio (Rmin) ................................................................................................. 12
4.3 Determination of minimum number of plates required and product composition
under total reflux .................................................................................................................. 13
4.3.1 Minimum number of plates ................................................................................ 13
4.3.2 Determination of the composition of the non-key components at total reflux .. 13
4.4 Determination of Feed tray location and actual number of plates ............................ 14
4.4.1 Feed tray number(𝑵𝑭, 𝒎𝒊𝒏) ............................................................................... 14
4.4.2 Estimation of actual number of plates required for a finite reflux ratio (R) using
𝑵𝒎 and 𝑹𝒎 and Gilliland correlation ............................................................................. 14
4.4.3 Feed plate location ............................................................................................. 14
4.5 Determination of the composition of products when R=0.4 ..................................... 15

v
4.6 Determination of liquid flow rate and vapor flow rates inside of the column .......... 16
4.7 Determination of number of trays and compositions of each tray by Lewis and
Matheson calculation method .............................................................................................. 17
4.7.1 Rectifying section .............................................................................................. 17
4.7.2 Striping Section .................................................................................................. 21
4.7.3 Number of trays ................................................................................................. 23
4.8 Determination of average density of vapor /liquid in rectifying and stripping
sections ................................................................................................................................. 24
4.8.1 Rectifying Section .............................................................................................. 24
4.8.2 Stripping Section ................................................................................................ 25
4.9 Determination of average molecular weights & l/V mass flow rates in the column 27
4.10 Determination of liquid/vapor mass flow rates ..................................................... 27
4.11 Internal column design .......................................................................................... 28
4.11.1 Rectifying section .............................................................................................. 28
4.11.2 Stripping section ................................................................................................ 30
4.11.3 Verification of Tray Spacing ............................................................................. 32
4.12 Tray hydraulic design ............................................................................................ 32
4.12.1 Liquid flow arrangement.................................................................................... 32
4.12.2 Rectifying Section .............................................................................................. 32
4.12.3 Stripping Section ................................................................................................ 35
4.13 Height of the column ............................................................................................. 36
4.13.1 Estimate of overall plate efficiency using o’Connell’s correlation .................... 36
4.13.2 Number of actual trays required ........................................................................ 37
4.13.3 Height of the column ......................................................................................... 37
4.14 Summary of chemical design ................................................................................ 38
CHAPTER 5 - OVERVIEW TO DETAILED MECHANICAL DESIGN ........................ 39
5.1 Main geometry of the vessel ..................................................................................... 39
5.2 Main dimensions of the vessel .................................................................................. 39
5.3 Operating conditions ................................................................................................. 39
CHAPTER 6 - MATERIAL SELECTION FOR CONSTRUCTION ................................ 40
6.1 Selection of Material ................................................................................................. 40
6.2 Welding Technique ................................................................................................... 41
6.3 Corrosion Allowance................................................................................................. 41
CHAPTER 7 - MECHANICAL DESIGN OF THE DISTILLATION .............................. 42
7.1 Parameter calculation ................................................................................................ 42

vi
7.1.1 Design Pressure .................................................................................................. 42
7.1.2 Design Temperature ........................................................................................... 42
7.1.3 Design Stress ...................................................................................................... 43
7.2 Thickness Calculation ............................................................................................... 43
7.2.1 Rectifying section .............................................................................................. 43
7.2.2 Stripping Section ................................................................................................ 44
7.3 Design of top and bottom enclosures ........................................................................ 44
7.3.1 Thickness and height calculation of top head .................................................... 44
7.3.2 Thickness and Height calculation of bottom closure ......................................... 46
7.4 Design of column reducer ......................................................................................... 47
7.4.1 The thickness of the reducer .............................................................................. 47
7.4.2 Checking for reinforcement ............................................................................... 47
7.4.3 Height of the reducer ......................................................................................... 48
7.5 Height of the Column ................................................................................................ 48
7.6 Design of Openings and Reinforcements .................................................................. 48
7.6.1 Determination of size of the Column openings ................................................. 48
7.6.2 Thickness and Reinforcements for Openings .................................................... 50
7.7 Design of Insulation .................................................................................................. 53
7.8 Combined loading calculations ................................................................................. 54
7.8.1 Stresses due to pressure ..................................................................................... 55
7.8.2 Load due to weights of the column .................................................................... 55
7.8.3 Load due to wind ............................................................................................... 57
7.8.4 Calculation of principle stresses ........................................................................ 57
7.9 Design of supports ..................................................................................................... 59
7.9.1 Determination of skirt wall thickness ................................................................ 59
7.9.2 Design of Bearing plate and Bolt ....................................................................... 60
7.10 Description of Fabrication ..................................................................................... 62
7.11 Mechanical Drawings ............................................................................................ 63
CHAPTER 8 - CONTROL, PIPING, INSTRUMENTATION & OTHER ASPECTS ...... 64
8.1 Selection of Pipes ...................................................................................................... 64
8.2 Selection of Valves.................................................................................................... 64
8.2.1 Selection of shut off valve ................................................................................. 65
8.2.2 Selection of pressure relief valve ....................................................................... 66
8.2.3 Selection of flow control valve .......................................................................... 66
8.3 Selection of pumps and strainers ............................................................................... 67
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8.4 Instrumentation.......................................................................................................... 68
8.4.1 Pressure measurement ........................................................................................ 68
8.4.2 Temperature Measurement ................................................................................ 69
8.4.3 Level measurement ............................................................................................ 70
8.4.4 Flow measurement ............................................................................................. 70
8.5 Process Control Aspects ............................................................................................ 71
8.5.1 Pressure control in the column ........................................................................... 71
8.5.2 Controlling the overhead and bottom product ................................................... 72
8.6 PI Diagram ................................................................................................................ 74
CHAPTER 9 - column Operating Procedure ...................................................................... 75
9.1 Startup procedure of a distillation column ................................................................ 75
9.2 Shutdown procedure of a distillation column ........................................................... 75
9.3 Emergency shutdown procedure of a distillation column ......................................... 75
9.4 Useful Startup and shutdown lines ............................................................................ 76
9.5 Troubleshooting of distillation column ..................................................................... 76
9.5.1 Flooding ............................................................................................................. 76
9.5.2 Foaming ............................................................................................................. 77
CHAPTER 10 - Safety Aspect .............................................................................................. 78
10.1 Personnel protection .............................................................................................. 78
10.1.1 First aid measures .............................................................................................. 78
10.2 Fire measures ......................................................................................................... 79
10.3 Accidental release measure ................................................................................... 79
10.4 Handling and Storage ............................................................................................ 80
10.5 HAZOP Study Applied to the Distillation Column ............................................... 80
CHAPTER 11 - Economics Aspects ..................................................................................... 84
11.1 Capital cost of the shell ......................................................................................... 84
11.2 Capital cost of the sieve trays ................................................................................ 85
11.3 Capital cost of the condenser ................................................................................. 86
11.4 Capital cost of the Process furnace ........................................................................ 86
11.5 Total capital cost of the distillation system ........................................................... 88
CONCLUSION ........................................................................................................................ 89
REFERENCES ........................................................................................................................ 90

viii
LIST OF TABLES
Table 1- Distillate and Bottom Compositions.......................................................................... 12
Table 2-A9 Composition Calculation at R-0.4......................................................................... 15
Table 3-Actual Compositions of Distillate & Bottom ............................................................. 15
Table 4- 1st Plate Vapor and Liquid Compositions .................................................................. 17
Table 5-2nd Plate Vapor and Liquid Compositions .................................................................. 18
Table 6-3rd Plate Vapor and Liquid Compositions .................................................................. 18
Table 7-4th Plate Vapor and Liquid Compositions .................................................................. 19
Table 8-5th Plate Vapor and Liquid Compositions................................................................... 19
Table 9-6th Plate Vapor and Liquid Compositions................................................................... 19
Table 10-7th Plate Vapor and Liquid Compositions................................................................. 20
Table 11-8th Plate Vapor and Liquid Compositions................................................................. 20
Table 12-9th Plate Vapor and Liquid Compositions................................................................. 21
Table 13-1st Plate Vapor and Liquid Compositions ................................................................. 21
Table 14-2nd Plate Vapor and Liquid Compositions ................................................................ 22
Table 15-3rd Plate Vapor and Liquid Compositions ................................................................ 22
Table 16-4th Plate Vapor and Liquid Compositions................................................................. 23
Table 17-5th Plate Vapor and Liquid Compositions................................................................. 23
Table 18-Density calculation of the vapor leaving from 1st plate of rectifying section .......... 24
Table 19-Density calculation of the liquid leaving from 1st plate of rectifying section .......... 25
Table 20-Summary of density calculations .............................................................................. 26
Table 21-Summary of Average molecular weights Calculations ............................................ 27
Table 22- Summary of mass flow rates of stripping section and rectifying section ................ 27
Table 23-Liquid/vapor flow rate inside the rectifying section of the column......................... 28
Table 24-Liquid/vapor flow rate inside the Stripping section of the column ........................ 30
Table 25-Summary of Chemical Design .................................................................................. 38
Table 26- Properties of the Selected Material .......................................................................... 41
Table 27-Dimeters vs thickness-Chemical Engineering Volume 6 ......................................... 43
Table 28-Semi-Apex Angle ..................................................................................................... 47
Table 29-Volumetric Flowrate Calculations ............................................................................ 49
Table 30-Typical pipe velocities .............................................................................................. 49
Table 31- Calculation of Theoretical Diameters ...................................................................... 50
Table 32- Pipe Selection .......................................................................................................... 50

ix
Table 33-Thickness and Schedule of openings ........................................................................ 52
Table 34-Reinforcement Area Calculation .............................................................................. 52
Table 35-Reinforcement Thickness Calculation ...................................................................... 53
Table 36-Column Weight Calculation ..................................................................................... 56
Table 37-Stress intensity Values .............................................................................................. 58
Table 38-List of Drawings ....................................................................................................... 63
Table 39-Designed Pipe Diameters.......................................................................................... 64
Table 40-HAZOP Study of the Distillation Column ............................................................... 81
Table 41-Total Capital Cost Calculation ................................................................................. 88

LIST OF FIGURES
Figure 1-1-Process Flow Chart of the p-xylene manufacturing plant ....................................... 2
Figure 2-1-(a ) Sieve Tray, (b) Valve Tray, (c) Bubble Cup Tray .............................................. 7
Figure 2-2-(a) Randomly dumped packing material, (b) Structured Packing Material .............. 7
Figure 3-1-(a) Entrainment of Sieve Plate, (b) Flooding of Sieve Plate, (c) Weeping of Sieve
Plate.......................................................................................................................................... 10
Figure 4-1-Liquid/Vapor Flow Pattern of the Column............................................................ 16
Figure 4-2-Stripping Section ................................................................................................... 21
Figure 4-3-Liquid & Vapor Flow Through The Column ........................................................ 24
Figure 4-4-Aspen Plus Simulation Results .............................................................................. 24
Figure 4-5-Flooding Velocity Sieves Plates ............................................................................ 29
Figure 4-6-Recommended General Condition & Dimensions for Tray Towers ..................... 32
Figure 4-7-Selection of Liquid Flow Arrangement ................................................................. 32
Figure 4-8-Relation between Down-Comer Area and Weir Length ....................................... 33
Figure 4-9-Weep Point Correlation ......................................................................................... 34
Figure 4-10-Entrainment Correlation for Sieve Plates ............................................................ 34
Figure 6-1-ASME Boiler & Pressure Vessel Code 2008 - DIVISION 1-- SECTION
VIII;AND SECTION XII; SECTION I; SECTION II ............................................................ 40
Figure 7-1-Cross section of the Reducer ................................................................................. 48
Figure 7-2-Welded Pad ............................................................................................................ 51
Figure 7-3-Skirt Support ......................................................................................................... 59
Figure 8-1-Side View of an Eccentric Plug Valve(Partially open) .......................................... 65
x
Figure 8-2-API 520-Conventional safety relief valve ............................................................. 66
Figure 8-3-Tee Pattern Globe Valve ........................................................................................ 67
Figure 8-4-Wafer Type Butterfly Valve .................................................................................. 67
Figure 8-5-Carbon steel Y strainer .......................................................................................... 67
Figure 8-6-Diaphragm Pressure Gauge ................................................................................... 68
Figure 8-7-Platinum Resistance temperature Detector ............................................................ 69
Figure 8-8-Distillation column overhead control system ....................................................... 72
Figure 8-9-distillation column bottom control system ............................................................ 73
Figure 11-1-50 trays -Cost of sieve tray distillation ................................................................ 85
Figure 11-2-25 trays -Cost of sieve tray distillation columns ................................................. 85
Figure 11-3-Cost equations for Distillation Equipment .......................................................... 85
Figure 11-4-Process Furnace (Loh & Lyons , 2002) ............................................................... 87
Figure 11-5-Correction Factors Fc for process furnace ........................................................... 87

xi
CHAPTER 1 - INTRODUCTION
This chapter contains a brief description about the work carried out during the Comprehensive
Design Group Project of designing a para xylene production plant. This also includes an
introduction to the Comprehensive Design Individual Project.

1.1 Comprehensive Design Group Project


As per the literature survey conducted during the Comprehensive Design Group Project, Para
xylene has 80% demand of total xylene demand and mainly processed into terephthalic acid
(TPA), which in turn is largely utilized to manufacture PET. Second largest application of p-
xylene is in plastic PET containers, especially plastic bottles. Para xylene is the main product
and o-xylene, benzene, light naphtha and hydrogen are the byproducts of the process. Straight
run heavy naphtha is the main raw material of the plant.

The annual production capacity of the plant is 5% of the gap (5,000,000MT) between the Asian
p-xylene demand and supply. The total feed flow rate is 50MT/hr and the product flow rate is
6.975MT/hr. The payback period is 4 years and an internal rate of return of 28% is achievable
while maintaining 658,842,937.36 USD of NPV. Hambanthota area is selected as the plant
location considering several factors such as population, access to raw materials (assuming a
future petroleum refinery establishment in Hambanthota), access to Asian customers through
Hambanthota port, access to required utilities (steam and electricity) and social and climate
aspects.

The manufacturing process start from straight run heavy naphtha and catalytic cracking of
straight run heavy naphtha which is done in a CCR. Then the extract is sent to the reformate
splitter and C8 - C10 aromatics are separated from C6 and C7 aromatics.

Raffinate from the reformate splitter is sent to the xylene splitter, where o-xylene and C9-C10
are separated and sent to the o-xylene column where o-xylene is recovered. The extract from
the xylene splitter is sent to the parex unit to separate p-xylene through adsorption. Then the
raffinate of parex unit is sent to the isomer unit and m-xylene and ethyl benzene get isomerized
to p-xylene. The out let of the isomer unit is sent to the deheptanizer where light ends are
separated and the raffinate is sent to the xylene splitter.

The extract of the reformate splitter is sent to the sulfolane unit to extract C6 and C7 aromatics
and is then sent to the benzene column to separate benzene. Then raffinate of benzene column
is sent to the toluene column to separate toluene. Then raffinate of the toluene column is sent

1
to the xylene splitter. Extract of the toluene column and extract from the C9 aromatic column
is sent to the Tatoray unit, where trans alkylation and disproportionation reactions occur,
producing p-xylene and benzene. Extract of the Tatoray unit also is sent as the feed of the
benzene column.

C10
A9 Column

Light End

De-heptanizer Column
Toluene Column
Benzene
MATERIAL FLOW SHEET - PARA-XYLENE PRODUCTION

Benzene Column

Para-Xylene

Isomar Unit

O-xylene
Raffinate

O-xylene Column
Sulfolane Process

Parex Unit
Tatoray Unit
Sulfolane

Reformate Splitter

Xylene Splitter
Light End

Stripper
Hydrogen

Separator

Naphtha+Hydrogen
R-03
R-02
R-01
Regenerator

Figure 1-1-Process Flow Chart of the p-xylene manufacturing plant

2
1.2 Comprehensive Design Project - Individual
The aim of this project is to design the o-xylene separation column. A mixture of xylenes,
aromatics (A9, A10, A11) and i-paraffin is fed to the column to recover 99% of the o-xylene with
the distillate. The feed rate of the column is obtained as 135.85 kmol/hr (material balance) and
65% of the feed consists of saturated liquid (Aspen Plus simulation). Based on the literature
references, feed temperature is taken as 212℃ and the operating temperature of the column is
obtained as 340 kPa (WU, et al., 2011). Chapters to come will concentrate on a literature survey
on available distillation technologies and the selection of the most suitable distillation process
and finally the parameter calculations.

3
CHAPTER 2 - LITERATURE SURVEY
2.1 Distillation
Distillation is one of the most economical methods for purifying liquids and separating
mixtures of liquids into their individual components by utilizing the difference in their relative
volatilities or boiling points. Distillation is widely used in the petroleum and chemical
industries and as examples for the fractionation of crude oil into useful products such as
gasoline, xylene, benzene, toluene and heating oil and distillation of crude fermentation broths
into alcoholic spirits such as gin and vodka. There are alternatives to distillation process like
solvent extraction, membrane separation or adsorption mechanisms. However, these processes
often have higher investment costs and thus distillation process is widely used.

Distillation works by the application and removal of heat to exploit differences in relative
volatility. The heat causes components with lower boiling points and higher volatility to be
vaporized, leaving less volatile components as liquids. Thus, Liquid mixtures with having high
relative volatilities, are easier to separate from distillation. So the liquid mixtures that having
close-boiling points and azeotropic are more difficult to separate. Thus, special distillation
techniques have to be used to separate these mixtures.

Distillation can be used to separate binary or multi-component mixtures. Many variables, such
as column pressure, temperature, height and diameter are determined by the properties of the
feed and the nature and quality of desired products. Some specialized columns perform other
functions, like reactive distillation, which combine reaction and separation of products into a
single unit. Distillation can be carried out either as a continuous or batch system. In batch
operation, the feed to the column is introduced batch-wise while continuous columns operate
at a continuous feed stream.

2.1.1 Types of Distillation


This section contains brief descriptions about different types of distillation methods such as
simple, fractional, steam, vacuum and reactive distillation.

2.1.1.1 Simple distillation.


In simple distillation process, the liquids are separated by evaporating and capturing them at
various points in their cooling cycle and then immediately channeling into a condenser to
condense the vapor into liquid. Double distillation is also can be done on the collected liquid,
in order to enhance the purity of the separated compounds.

4
2.1.1.2 Fractional distillation
Fractionating columns are used to separate constituents whose volatilities are nearly similar
which cannot be separated by simple distillation process. They mostly applied in alcohol
purification and gasoline purification in petroleum refining industries.

2.1.1.3 Steam distillation


In steam distillation process, steam is introduced to the column and the temperature of the
compounds are depressed, by vaporizing them at lower temperature. This way, the temperature
sensitive compounds are separated before decomposition.

2.1.1.4 Vacuum distillation


In vacuum distillation, the pressure inside the distillation column is maintained at a vacuum to
lower the temperature needed to vaporize the liquid. This method of distillation is applied in
situations with heat sensitive products, liquids with low viscosities, and liquids that tend to foul
or foam (Sandhyarani, 2016).

2.1.1.5 Reactive distillation


Reactive distillation, or catalytic distillation, is a process where the chemical reactor is also the
still. It combines reaction and distillation into a single column.

2.2 Type of Distillation columns


Distillation columns can mainly be classified into two types based on the interior material i.e.
plate/tray columns or packing material columns. This section describes the differences as well
as advantages and disadvantages of these two types.

2.2.1 Plate/Tray Column


Plate/tray columns are the widely used type of distillation columns. The number of trays or
stages in the column is depended on the desired purity and difficulty of separation. The number
of stages also determines the height of the column. They are more efficient in the separation
process than packed towers and also costlier.

Different types of trays are used in plate columns. The type to be selected depends upon the
degree of product purity required, the type of fluids, fluid velocity and other process parameters
of the system.

Distillation trays can be classified as:

 Cross-flow trays with down comers

5
 Countercurrent trays without down comer (Dual-flow tray)

Dual flow trays allow the vapor and liquid to pass through the same tray openings. This results
in a limited operating range because the dispersion height is very sensitive to the vapor/liquid
flow rates. In general, they are employed only in cases where high capacity or high resistance
to fouling are required.
Cross-flow trays utilize a weir on the down comer to control the liquid height on the tray. Thus,
it provides a stable vapor/liquid dispersion over a wide range of vapor/liquid flows. The bulk
of the vapor rises from the aerated liquid through the holes of the tray and the liquid passes
from the top to the bottom of the column through down comers.
The types of cross flow trays used in plate distillation columns are as follows.

 Sieve plate
Sieve plates offer high capacity and efficiency, low pressure drop, ease of cleaning, and low
capital cost, but smaller turndown ratio. Sieve trays are simple and easy to fabricate. They
consist of metal plates with holes of varying numbers, sizes and patterns. The vapor is directed
straight upward through the liquid on the trays.
 Valve Plate
Mainly there are two types of valve trays namely fixed valve trays and floating or movable
valve trays. Floating valve trays have lift able caps which operate like check valves. These caps
make valve trays more expensive than sieve trays. However, they also increase the operating
range of the tray. At low vapor velocities, caps get closed and thus prevent dumping. In general,
these valves are more prone to fouling and mechanical damage. The fixed valve trays are
manufactured by punching and forming integral valves over the tray deck. They give higher
capacity than sieve trays due to punching fixed slots in a parallel way to the liquid flow
arrangement.
 Bubble cup Plate
Bubble cap plates consist of bell shaped caps fixed to cylindrical risers through which the vapor
passes the tray deck. A cap is fitted over each riser, with a space left between, to allow vapors
to pass. Vapors come up through the risers, and the caps filter them downward. Vapors escape
through slots in the caps and pass through the liquid on the trays, causing bubbling.
Bubble cap trays are able to operate at low vapor and liquid rates, because liquid and foam is
trapped on the tray to a depth at least equal to the weir height. They also work well in high
turndown applications since the orifices in the bubble caps are in the form of risers whose top

6
openings are elevated significantly above the tray deck. The cost of bubble cap tray is by far the
highest.
Figure 2-1 shows the typical structures of a sieve tray, a valve tray and a bubble cap tray.

Figure 2-1-(a ) Sieve Tray, (b) Valve Tray, (c) Bubble Cup Tray

2.2.2 Packed Bed Columns


Packed bed columns are used most often for absorption and extraction. However, they are also
used for the distillation of vapor-liquid mixtures. The packing provides a large surface area for
vapor-liquid contact and it increases the time of contact, which increases the separation
efficiency. It is more preferable to use packed bed columns over tray packing when the diameter
of the column is less than 0.6 m (Naik, et al., n.d.).
Packed bed columns are also useful in vacuum fractionation and also it is the best option when
handling corrosive chemicals, since packing can be made using inert materials. However, the
maintenance cost is high compared with the plate columns due to the difficulty in cleaning the
packing material. The packing material may be randomly dumped objects or it may be specially
designed structured packing material as shown in the Figure 2-2(a). The randomly dumped
packing may be steel, ceramic or plastic objects of various geometric designs. The structured
packing may be sheet metal, woven wire gauze or plastic of various designs and stacked in
various arrangements.

Figure 2-2-(a) Randomly dumped packing material, (b) Structured Packing Material

7
CHAPTER 3 - DISTILLATION COLUMN SELECTION
This chapter includes the criteria for selecting the best suited distillation column type and the
tray type for it.

3.1 Selecting the column type


As mentioned in section 2.2, two main types of columns are used in distillation, namely
plate/tray distillation columns and packed bed columns. Packed bed towers would normally be
selected instead of tray towers in the columns less than 2ft in diameter, packing is generally
cheaper. However, a packed bed tower must have a larger diameter than a tray tower to handle
the same feed rate. Also they are often used for vacuum distillations and distillation of corrosive
fluids.

In this process, o-xylene separation has a feed rate of 16007.65 kg/hr and o-xylene should be
separated continuously. However, xylenes, A9 and other compounds are not much corrosive
and this separation can be achieved by using multicomponent fractionation distillation. Thus it
is more suitable to use a plate\tray column rather than a packed bed column.

3.1.1 Selection of Tray Type


As mentioned in section 2.2, Sieve plates offer high capacity and efficiency, low pressure drop,
ease of cleaning, simple and easy to fabricate than valve trays and bubble cup trays. Thus, sieve
tray type would be the most suitable for this particular application.

3.1.1.1 Hole Diameter


The sieve plate with a hole diameter in the range of 3/16 to 1/4 in (4.76-6.35 mm) give better
hydraulic and mass transfer performance than the large ones in the range of ½ to ¾ in (12.7-
19.0 mm) (Chuang & Nandakumar, 2000). However, large-hole trays are cheaper and show
more resistance to fouling.

3.1.1.2 Hole Area


The hole area is normally in the range of 5-16% of the bubbling area (Chuang & Nandakumar,
2000). Lower hole area allows the tray to operate at higher efficiency and turndown ratio. But
it gives higher pressure drop. Hole areas below 5% are not used because the distance between
holes becomes excessive and liquid channeling may occur. However, the distance can also be
adjusted by changing the hole diameter. In general, weeping and entrainment can be consisted
when the hole area greater than 16%.

8
3.1.1.3 Weir Design
Outlet weirs are used to maintain a head of liquid on the tray deck as well as to ensure a positive
vapor seal to the bottom of the down comer. In general, in distillation columns operating above
atmospheric pressure, the weir heights will normally be between 40 mm to 90 mm (1.5 to 3.5
in.) and recommended value is 40 to 50 mm (Sinnott, 2005).
The weir length will normally be between 0.6 to 0.85 of the column diameter. A good initial
value to use is 0.77 equivalent to a down comer area of 12% (Sinnott, 2005).
3.1.2 Vapor flow Condition
Adverse vapor flow conditions can cause due to following problems.
3.1.2.1 Entrainment
The liquid may be carried away with the vapor from a plate to the plate above. This may
decrease the efficiency of the column. Thus, the design is checked for the entrainment and if
the conditions are unsatisfactory, calculations should be repeated with small alterations.

Entrainment can be estimated from the correlation given by Fair (1961), which gives the
fractional entrainment 𝜓 as a function of the liquid-vapor factor FLV, with the percentage
approach to flooding as a parameter. The upper limit of 𝜓 can be taken as 0.1.

3.1.2.2 Flooding
Flooding is brought about by excessive vapor flow, causing liquid to be entrained in the vapor
up the column. Tray efficiency falls and the liquid may force out of the existing pipe at the
tower top. Generally, columns are designed for 80%-85% flooding at maximum feed rate.

3.1.2.3 Weeping
This phenomenon is caused by low vapor flow. Here, the pressure exerted by the vapor
becomes insufficient to hold up the liquid on the tray. Thus, liquid starts to leak through
perforations. Excessive weeping will lead to dumping. Therefore, the hole area must be chosen
so that, at the lowest operating rate the vapor flow velocity is still well above the weeping point.

9
3.1.2.4 Foaming
Expansion of liquid when aerated is foaming. It is desirable to a certain limit since it increases
the interfacial contact area. If foaming is expected within 50%-60% flooding is recommended.
However, foaming won’t be happened in this designed column. Thus, 80% flooding is chosen.
Figure 3-1 depicts the phenomena of entrainment, flooding and weeping of sieve plates.

Figure 3-1-(a) Entrainment of Sieve Plate, (b) Flooding of Sieve Plate, (c) Weeping of Sieve Plate

3.1.3 Selection of the condenser and reboiler type


The condenser above the column can be either a total or partial condenser. In a total condenser,
all vapors leaving the top of the column is condensed to liquid. Thus, the reflux stream and
overhead product have the same composition. On the other hand, only a portion of the vapor
entering the condenser is condensed to liquid in a partial condenser. In most of the cases, the
condensed liquid is refluxed into the column and the overhead product is drawn out in the vapor
form (Jaya, 2011).

In this process, condensed liquid should be obtained from the top of the distillation column.
Thus, total condenser is selected for the design of o-xylene separation distillation column.

Reboilers provide vapor for a distillation column. Most reboilers are shell and tube heat
exchangers and normally steam is used as the heat source. Commonly used reboilers are kettle
reboilers, thermosyphon reboilers and fired reboilers (Sloley, 2012).

10
CHAPTER 4 - CHEMICAL DESIGN OF THE COLUMN
4.1 Material Balance
Since this is a multicomponent distillation, determination of key components for the material
balance becomes a crucial step of the design. Major function of this column is to separate o-
xylene from the mixture which is coming from the bottom of the xylene splitter.

Key components can be divided in to two types as follows.

 Light key - The most volatile component in the bottoms, but in a significant
concentration is known as the light key.
 Heavy key - The least volatile component in the distillate, but in a significant
concentration is known as the heavy key

In this o-xylene column, o-xylene is selected as the light key which is recovered 99% (mole
basis) as the distillate and P11(iso paraffin) is selected as the heavy key which is recovered as
1% (mole basis) at the distillate.

General material balance equation:

𝐴𝑐𝑐𝑢𝑚𝑢𝑙𝑎𝑡𝑖𝑜𝑛 = 𝐼𝑛𝑝𝑢𝑡 + 𝑔𝑒𝑛𝑒𝑟𝑎𝑡𝑖𝑜𝑛 − 𝑜𝑢𝑡𝑝𝑢𝑡 − 𝑐𝑜𝑛𝑠𝑢𝑚𝑝𝑡𝑖𝑜𝑛

If no accumulation, generation and consumption,


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

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

𝑀𝑎𝑠𝑠 𝑜𝑓 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡
𝑀𝑎𝑠𝑠 𝐹𝑟𝑎𝑐𝑡𝑖𝑜𝑛 = × 100%
𝑇𝑜𝑡𝑎𝑙 𝑚𝑎𝑠𝑠 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 𝑜𝑓 𝑠𝑡𝑟𝑒𝑎𝑚

𝑀𝑜𝑙𝑒𝑠 𝑜𝑓 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡
𝑀𝑜𝑙𝑒 𝐹𝑟𝑎𝑐𝑡𝑖𝑜𝑛 = × 100%
𝑇𝑜𝑡𝑎𝑙 𝑀𝑜𝑙𝑎𝑟 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 𝑜𝑓 𝑠𝑡𝑟𝑒𝑎𝑚

𝑀𝑎𝑠𝑠 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 𝑜𝑓 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡


𝑀𝑜𝑙𝑎𝑟 𝑓𝑙𝑜𝑤 𝑟𝑎𝑡𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡 =
𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑚𝑎𝑠𝑠 𝑓𝑙𝑜𝑤𝑟𝑎𝑡𝑒 𝑜𝑓 𝑐𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡

11
4.2 Determination of the minimum reflux ratio and product compositions
under minimum reflux ratio (Rmin)
Feed rate – 135.85 𝑘𝑚𝑜𝑙/ℎ
At minimum reflux
Table 1- Distillate and Bottom Compositions

Component Xi,F F.Xi,F D.Xi,D W.Xi,W K222 α I,222 F.Xi,F.α I,222 D.Xi,D.α I,222
P5 0.06 8.1 8.1 Nil 15.942 29.394 236.842 236.842
m-xylene 0.01 1.5 1.5 Nil 1.814 3.345 5.127 5.127
o-
0.43 59.0 57.8 1.2 1.618 2.982 175.878 172.361
xylene(LK)
A9 0.16 21.7 x y 1.346 2.482 53.901 2.482x
P11(HK) 0.11 15.3 0.2 15.1 0.542 1.000 15.251 0.153
A10 0.19 26.1 nil 26.1 0.327 0.603 15.746 nil
A11 0.03 4.2 nil 4.2 0.177 0.327 1.375 nil
Assumptions;
 Α is a constant at average column temperature
 Constant molar overflow
 Optimal feed location
 Reflux is saturated liquid

∝𝑖 . 𝑥𝑖,𝐹 . 𝐹
∑( ) = 𝐹. (1 − 𝑞)
∝𝑖 − 𝜑
236.842 5.127 175.878 53.901 15.251 15.746 1.375
+ + + + + +
29.394 − 𝜑 3.345 − 𝜑 2.982 − 𝜑 2.482 − 𝜑 1 − 𝜑 0.603 − 𝜑 0.327 − 𝜑
= 135.85(1 − 0.65) − − − −→ 𝟎𝟏
𝜑 Values calculated from equations (01) are following.
𝜑 = 25.3995, 3.3366, 2.6096, 1.2004, 0.7295, 0.3370, -4.0822
𝜑3= 2.6096 𝜑4= 1.2004
These data can be used to solve Underwood equation and determine D and Rm.
∝𝑖 . 𝑥𝑖,𝐷 . 𝐷
∑( ) = 𝐷. (𝑅𝑚 + 1)
∝𝑖 − 𝜑
478.05 − 19.43𝑥 = 𝐷(1 + 𝑅𝑚 ) ----------------------- (1)
106.76 + 1.94𝑥 = 𝐷(1 + 𝑅𝑚 ) ------------------------ (2)
𝒙 = 𝟏𝟕. 𝟑𝟕
12
By equation 01, 𝐷(1 + 𝑅𝑚 ) = 110.93 --------------------- (3)
Apply material balance for A9, 𝑦 = 4.35 𝐷 = 84.91
By equation 03,
84.91 × (1 + 𝑅𝑚 ) = 110.93
Minimum reflux ratio , 𝑹𝒎 = 𝟎. 𝟑𝟎𝟔
Top Product Flowrate – 𝟖𝟒. 𝟗𝟏 𝒌𝒎𝒐𝒍/𝒉𝒓
Bottom Product Flowrate – 𝟓𝟎. 𝟗𝟒 𝒌𝒎𝒐𝒍/𝒉𝒓
Then the assumed average column temperature should be checked,

 Distillate dew point(trial and error) - 194.7 ℃


 Residue Bubble point (trial and error) – 258.5 ℃
 Average column temperature – 223.6 ℃
 Assumption Tcolumn avg = 222 ℃ is valid

4.3 Determination of minimum number of plates required and product


composition under total reflux
4.3.1 Minimum number of plates
𝑥 .𝐷 𝑥 .𝑊
ln |(𝑥 𝐿𝐾,𝐷. 𝑊 )( 𝑥𝐻𝐾,𝑊 . 𝐷 )
𝐿𝐾,𝑊 𝐻𝐾,𝐷
𝑁𝑚 + 1 =
ln | ∝𝐿𝐾,𝑎𝑣𝑒𝑟𝑎𝑔𝑒 |

𝑁𝑚 - Number of plates in the column excluding the reboiler


∝𝐿𝐾,𝑎𝑣𝑒𝑟𝑎𝑔𝑒 is the relative of the light key

∝𝐿𝐾,𝑎𝑣𝑒𝑟𝑎𝑔𝑒 = √∝𝐿𝐾,𝑇,𝐷,𝑑𝑒𝑤 𝑝𝑜𝑖𝑛𝑡 × ∝𝐿𝐾,𝑇,𝑅,𝑏𝑢𝑏𝑏𝑙𝑒 𝑝𝑜𝑛𝑡

∝𝐿𝐾,194.7,𝐷,𝑑𝑒𝑤 𝑝𝑜𝑖𝑛𝑡 = 3.319 ∝𝐿𝐾,145.1,𝑅,𝑏𝑢𝑏𝑏𝑙𝑒 𝑝𝑜𝑛𝑡 = 2.658

∝𝐿𝐾,𝑎𝑣𝑒𝑟𝑎𝑔𝑒 = √3.319 × 2.658 = 2.97


57.8 15.1
ln| × |
𝑁𝑚 + 1 = 1.2 0.2
= 7.53  𝑁𝑚 = 6.53 ≈ 7 Stages
ln|2.97|

Minimum number of stages – 7 stages

4.3.2 Determination of the composition of the non-key components at total reflux


𝑥𝑖,𝐷 .𝐷 (𝑁 +1) 𝑥 .𝐷
𝑚
=∝𝑖,222 × (𝑥 𝐻𝐾,𝐷.𝑊)
𝑥𝑖,𝑊 𝑊 𝐻𝐾,𝑊

For A9,
𝑥𝐴9 ,𝐷 . 𝐷 0.2
= 2.4827.53 × ( )
𝑥𝐴9 ,𝑊 𝑊 15.1

13
𝑥𝐴9 ,𝐷 . 𝐷 = 12.44 × 𝑥𝐴9 ,𝑊 𝑊 --------------- (1)

Applying material balance for 𝐴9 ,


𝑥𝐴9 ,𝑊 𝑊 = 21.7 − 𝑥𝐴9 ,𝐷 . 𝐷 ----------------- (2)

By solving 1 and 2 equations


𝑥𝐴9 ,𝑊 𝑊 = 1.61 kmol/hr 𝑥𝐴9 ,𝐷 . 𝐷 = 20.09 kmol/hr

4.4 Determination of Feed tray location and actual number of plates


4.4.1 Feed tray number(𝑵𝑭,𝒎𝒊𝒏 )

𝑥𝐿𝐾,𝐷
57.8
𝑥𝐻𝐾,𝐷
ln | ⁄𝑥𝐿𝐾,𝐹 | ln | 0.2⁄
59.0|
𝑥𝐻𝐾,𝐹 15.3
𝑁𝐹,𝑚𝑖𝑛 = ∝𝐿𝐾 =
ln | ⁄∝𝐻𝐾 | ln| 2.982⁄1|

Feed tray number at total reflux-𝑁𝐹,𝑚𝑖𝑛 = 3.95 ≈ 4 stages

4.4.2 Estimation of actual number of plates required for a finite reflux ratio (R) using
𝑵𝒎 and 𝑹𝒎 and Gilliland correlation
The optimum reflux ratio of many systems will lie between 1.2 to 1.5 times the
minimum reflux ratio.
Assume reflux ratio - 0.4(1.3 times of minimum reflux ratio)
0.4 − 0.306
𝑥= = 0.133
0.4 + 0.306
𝑁−𝑁𝑚 0.002743
= 0.545827 − 0.591422x + or by graph
𝑁+1 𝑥
𝑁−6.53
= 0.49 (By equation) 𝑁 = 13.76 ≈ 14 𝑠𝑡𝑎𝑔𝑒𝑠
𝑁+1

Actual Number of plates at 0.4 reflux ratio = 13.76 ≈ 14 stages


4.4.3 Feed plate location
𝑁𝐹,𝑚𝑖𝑛 𝑁𝐹
=
𝑁𝑚𝑖𝑛 𝑁
3.95 𝑁𝐹
=
6.53 13.76
Feed plate location- 𝑁𝐹 = 8.32 ≈ 9𝑡ℎ 𝑝𝑙𝑎𝑡𝑒

14
4.5 Determination of the composition of products when R=0.4
Table 2-A9 Composition Calculation at R-0.4

R 𝑹⁄ 𝑫. 𝒙𝑨𝟗 ,𝑫 𝑾. 𝒙𝑨𝟗 ,𝒘
𝑹+𝟏
∞ 1 20.09 1.61

0.4 0.286 - -

0.306 0.234 17.37 4.35

By linear interpolation,
At R= 0.4
𝑫. 𝒙𝐴9 ,𝐷 = 𝟏𝟖. 𝟑𝟗 𝑾. 𝒙𝐴9 ,𝑤 = 𝟑. 𝟑𝟏

At R= 0.4

Table 3-Actual Compositions of Distillate & Bottom

Component F.Xi,F D.Xi,D Xi,D W.Xi,W Xi,W

P5 8.1 8.1 0.094 Nil 0.000


m-xylene 1.5 1.5 0.017 Nil 0.000
o-xylene(LK) 59.0 57.8 0.672 1.2 0.024
A9 21.7 18.39 0.214 3.31 0.066
P11(HK) 15.3 0.2 0.002 15.1 0.303
A10 26.1 nil 0.000 26.1 0.523
A11 4.2 nil 0.000 4.2 0.084

15
4.6 Determination of liquid flow rate and vapor flow rates inside of the
column

D, XD

V L

F,XF

V’ L’

W,XW

Figure 4-1-Liquid/Vapor Flow Pattern of the Column

 Assumptions - Constant molar over flow

 Calculation –
For top operating section by reflux ratio

R=L/D 0.4=L/85.99  L = 34.40 𝒌𝒎𝒐𝒍/𝒉


Material balance for top operating line
V=L+D
V=85.99+34.40  V = 120.39 𝒌𝒎𝒐𝒍/𝒉
For feed plate
L’ =L +qF
L’=34.40 +135.9×0.65  L’= 122.74 𝒌𝒎𝒐𝒍/𝒉
For stripping section
L’ =V’+W
V’= 122.74 – 49.91  V’= 72.83 𝒌𝒎𝒐𝒍/𝒉

16
4.7 Determination of number of trays and compositions of each tray by
Lewis and Matheson calculation method
For feed tray
𝑊 𝐷
𝑥𝐿𝐾 [ ′ 𝑥𝐿𝐾,𝑤 + 𝑥𝐿𝐾,𝐷 ]
𝑉 𝑉
= 𝐷 𝑊
𝑥𝐻𝐾 [ 𝑥𝐻𝐾,𝐷 + ′ 𝑥𝐻𝐾,𝑤 ]
𝑉 𝑉

49.91 85.99
𝑥𝐿𝐾 𝑥𝐿𝐾 [72.83 × 0.024 + 120.39 × 0.672]
( ) ≈( ) =
𝑥𝐻𝐾 𝑖𝑛𝑡 𝑥𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦 [ 85.99 × 0.002 + 49.91 × 0.303]
120.39 72.83

0.4964
= 𝟐. 𝟑𝟕𝟒𝟎
0.2091

4.7.1 Rectifying section


1st Plate
Table 4- 1st Plate Vapor and Liquid Compositions

Component F.Xi,F D.Xi,D Yi,1 K194.7 Xi,D,194.7 K194.8 Xi,1,194.8


P5 8.1 8.1 0.094 11.029 0.009 11.045 0.009
m-xylene 1.5 1.5 0.017 1.083 0.016 1.085 0.016
o-
59 57.8 0.672
xylene(LK) 0.960 0.700 0.962 0.699
A9 21.7 18.39 0.214 0.792 0.270 0.794 0.270
P11(HK) 15.3 0.2 0.002 0.289 0.007 0.290 0.007
A10 26.1 nil 0 0.171 0.000 0.171 0.000
A11 4.2 nil 0 0.087 0.000 0.087 0.000
1.002 1.000
Temperature of 1st plate - 194.8℃
For 1st plate
𝑥 0.699 𝑥 𝑥
(𝑥 𝐿𝐾 ) = 0.007 → (𝑥 𝐿𝐾 ) = 99.857 ≥ (𝑥 𝐿𝐾 )
𝐻𝐾 1𝑠𝑡 𝐻𝐾 𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦
1𝑠𝑡

2nd Plate
𝑌𝑖,2 Values are calculated by equation;
When n=1 Top operating line equation
𝑅 𝑥𝑖,𝐷
𝑦𝑖,2 = 𝑥𝑖,1 + 𝑅 = 0.4
𝑅+1 𝑅+1
For P5,

17
0.4 0.094
𝑦𝑖,1 = × 0.009 + = 0.0697
0.4 + 1 0.4 + 1

Similarly;
Table 5-2nd Plate Vapor and Liquid Compositions

Component Yi,2 K196 Xi,D,196 K196.2 Xi,2,196.2


P5 0.070 11.235 0.006 11.267 0.006
m-xylene 0.017 1.112 0.015 1.116 0.015
o-xylene(LK) 0.680 0.985 0.690 0.989 0.687
A9 0.230 0.814 0.283 0.817 0.281
P11(HK) 0.003 0.298 0.011 0.300 0.011
A10 0.000 0.177 0.000 0.177 0.000
A11 0.000 0.090 0.000 0.091 0.000
1.005 1.001
Temperature of 2nd plate - 196.2℃
For 2nd plate
𝑥 0.687 𝑥 𝑥
(𝑥 𝐿𝐾 ) = 0.011  (𝑥 𝐿𝐾 ) = 62.45 ≥ (𝑥 𝐿𝐾 )
𝐻𝐾 2𝑛𝑑 𝐻𝐾 2𝑛𝑑 𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦

3rd Plate

Table 6-3rd Plate Vapor and Liquid Compositions

Component Yi,3 K198 Xi,D,198 K197.5 Xi,3,197.5


P5 0.051 11.55765 0.004 11.47646 0.004
m-xylene 0.016 1.156647 0.014 1.145241 0.014
o-xylene(LK) 0.682 1.025752 0.665 1.015511 0.671
A9 0.245 0.847623 0.289 0.839021 0.292
P11(HK) 0.006 0.3134 0.018 0.309616 0.018
A10 0.000 0.185709 0.000 0.183397 0.000
A11 0.000 0.095219 0.000 0.093919 0.000
0.990 1.000
Temperature of 3rd plate - 197.5 ℃
For 3rd plate
𝑥 0.671 𝑥 𝑥
(𝑥 𝐿𝐾 ) = 0.018  (𝑥 𝐿𝐾 ) = 37.28 ≥ (𝑥 𝐿𝐾 )
𝐻𝐾 3𝑟𝑑 𝐻𝐾 3𝑟𝑑 𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦

4th Plate

18
Table 7-4th Plate Vapor and Liquid Compositions

Component Yi,4 K198.5 Xi,D,198.5 K198.6 Xi,4,198.6


P5 0.038 11.639 0.003 11.656 0.003
m-xylene 0.016 1.168 0.013 1.170 0.013
o-xylene(LK) 0.679 1.036 0.655 1.038 0.654
A9 0.258 0.856 0.301 0.858 0.301
P11(HK) 0.009 0.317 0.029 0.318 0.029
A10 0.000 0.188 0.000 0.189 0.000
A11 0.000 0.097 0.000 0.097 0.000
1.002 1.000
Temperature of 4th plate - 198.6 ℃
For 4th plate
𝑥𝐿𝐾 0.654 𝑥𝐿𝐾 𝑥𝐿𝐾
( ) =  ( ) = 22.55 ≥ ( )
𝑥𝐻𝐾 4𝑡ℎ 0.029 𝑥𝐻𝐾 4𝑡ℎ 𝑥𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦

5th Plate
Table 8-5th Plate Vapor and Liquid Compositions

Component Yi,5 K200 Xi,D,200 K199.8 Xi,5,199.8


P5 0.028 11.886 0.002 11.853 0.002
m-xylene 0.015 1.203 0.012 1.198 0.012
o-xylene(LK) 0.672 1.068 0.629 1.063 0.632
A9 0.270 0.883 0.306 0.879 0.307
P11(HK) 0.015 0.329 0.045 0.327 0.046
A10 0.000 0.195 0.000 0.194 0.000
A11 0.000 0.101 0.000 0.100 0.000
0.996 1.000
Temperature of 5th plate - 199.8 ℃
For 5th plate
𝑥 0.632 𝑥 𝑥
(𝑥 𝐿𝐾 ) = 0.046  (𝑥 𝐿𝐾 ) = 13.739 < (𝑥 𝐿𝐾 )
𝐻𝐾 5𝑡ℎ 𝐻𝐾 5𝑡ℎ 𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦

6th Plate
Table 9-6th Plate Vapor and Liquid Compositions

Component Yi,6 K201 Xi,D,201 K201.1 Xi,6,201.1


P5 0.021 12.05324 0.002 12.07001 0.002
m-xylene 0.014 1.226917 0.012 1.229315 0.012
o-xylene(LK) 0.660 1.088869 0.606 1.091023 0.605
A9 0.281 0.900654 0.312 0.902464 0.311
P11(HK) 0.024 0.336872 0.071 0.337678 0.070
A10 0.000 0.200072 0.000 0.200565 0.000
A11 0.000 0.103331 0.000 0.103611 0.000
1.002 1.000

19
Temperature of 6th plate - 201.1 ℃
For 6th plate

𝑥𝐿𝐾 0.605 𝑥𝐿𝐾 𝑥𝐿𝐾


( ) =  ( ) = 8.64 ≥ ( )
𝑥𝐻𝐾 6𝑡ℎ 0.070 𝑥𝐻𝐾 6𝑡ℎ 𝑥𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦

7th Plate
Table 10-7th Plate Vapor and Liquid Compositions

Component Yi,7 K202 Xi,D,202 K202.7 Xi,7,202.7


P5 0.015 12.222 0.001 12.341 0.001
m-xylene 0.013 1.251 0.011 1.268 0.011
o-xylene(LK) 0.645 1.111 0.580 1.126 0.572
A9 0.289 0.919 0.315 0.932 0.311
P11(HK) 0.037 0.345 0.107 0.351 0.106
A10 0.000 0.205 0.000 0.209 0.000
A11 0.000 0.106 0.000 0.108 0.000
1.015 1.001
Temperature of 7th plate - 201.1 ℃
For 7th plate
𝑥𝐿𝐾 0.572 𝑥𝐿𝐾 𝑥𝐿𝐾
( ) = → ( ) = 5.66 ≥ ( )
𝑥𝐻𝐾 7𝑡ℎ 0.101 𝑥𝐻𝐾 7𝑡ℎ 𝑥𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦

8th Plate
Table 11-8th Plate Vapor and Liquid Compositions

Component Yi,8 K204 Xi,D,204 K204.8 Xi,6,204.8


P5 0.011 12.56344 0.001 12.70199 0.001
m-xylene 0.013 1.300399 0.010 1.320549 0.010
o-xylene(LK) 0.624 1.154908 0.540 1.173023 0.532
A9 0.296 0.956179 0.309 0.971416 0.304
P11(HK) 0.057 0.361704 0.157 0.368563 0.154
A10 0.000 0.215305 0.000 0.219519 0.000
A11 0.000 0.112 0.000 0.11441 0.000
1.017 1.000
Temperature of 8th plate - 204.8 ℃
For 8th plate
𝑥𝐿𝐾 0.532 𝑥𝐿𝐾 𝑥𝐿𝐾
( ) = ( ) = 3.45 ≥ ( )
𝑥𝐻𝐾 8𝑡ℎ 0.154 𝑥𝐻𝐾 8𝑡ℎ 𝑥𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦

9th Plate

20
Table 12-9th Plate Vapor and Liquid Compositions

Component Yi,9 K206 Xi,D,206 K207.4 Xi,9,207.4


P5 0.008 12.9118 0.001 13.1596 0.001
m-xylene 0.012 1.351218 0.009 1.387681 0.008
o-xylene(LK) 0.598 1.200601 0.498 1.233396 0.485
A9 0.298 0.994619 0.300 1.022219 0.292
P11(HK) 0.084 0.379041 0.223 0.39156 0.216
A10 0.000 0.225962 0.000 0.233667 0.000
A11 0.000 0.118103 0.000 0.122535 0.000
1.029 1.001
Temperature of 9th plate - 207.4 ℃
For 9th plate
𝑥𝐿𝐾 0.485 𝑥𝐿𝐾 𝑥𝐿𝐾
( ) = ( ) = 1.66 < ( )
𝑥𝐻𝐾 9𝑡ℎ 0.292 𝑥𝐻𝐾 9𝑡ℎ 𝑥𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦

Next, calculation of the number of plates and composition of each plate of the stripping section
is done.

4.7.2 Striping Section


 Plates are numbered from bottom to top for
stripping section.
 Assume the temperature for the partial reboiler as
258.5℃ (residual bubble point).
 𝑦𝑖,𝑚+1 values are the compositions of vapor leaving
the partial reboiler.

𝑦𝑖,𝑚+1 = 𝐾𝑖 . 𝑥𝑖,𝑊

 𝑥𝑖,𝑚 can be calculated by bottom operating line


equation

𝐿′ 𝑊 Figure 4-2-Stripping Section


𝑦𝑖,𝑚+1 = 𝑥𝑚 − 𝑥𝑤
𝐺′ 𝐺′
𝐺′ 𝑊
𝑥𝑚 = 𝑦𝑖,𝑚+1 + 𝑥𝑤
𝐿′ 𝐿′
1st Plate
Table 13-1st Plate Vapor and Liquid Compositions

Component Xi,W K258.5 Yi,258.5 Xi,1 K250.8 Yi,1


P5 0.000 24.594 0.000 0.000 22.557 0.000
m-xylene 0.000 3.314 0.000 0.000 2.939 0.000
o-xylene(LK) 0.024 2.974 0.072 0.052 2.635 0.138
21
A9 0.066 2.496 0.166 0.125 2.207 0.276
P11(HK) 0.303 1.119 0.339 0.324 0.970 0.314
A10 0.523 0.689 0.360 0.427 0.595 0.254
A11 0.084 0.404 0.034 0.054 0.343 0.019
0.970 1.000
Temperature of 1st plate - 250.8℃
𝑥𝐿𝐾 0.138 𝑥𝐿𝐾 𝑥𝐿𝐾
( ) =  ( ) = 0.439 < ( )
𝑥𝐻𝐾 1𝑠𝑡 0.314 𝑥𝐻𝐾 1𝑠𝑡 𝑥𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦

2nd Plate
Table 14-2nd Plate Vapor and Liquid Compositions

Component Xi,W Yi,250.8 Xi,1 K240.9 Yi,1


P5 0.000 0.000 0.000 20.10854 0.000
m-xylene 0.000 0.000 0.000 2.505881 0.000
o-xylene(LK) 0.024 0.138 0.091 2.242234 0.205
A9 0.066 0.276 0.191 1.8745 0.358
P11(HK) 0.303 0.314 0.309 0.800793 0.248
A10 0.523 0.254 0.363 0.488747 0.178
A11 0.084 0.019 0.045 0.276116 0.013
1.000 1.001
Temperature of 2nd plate - 240.9℃
For 2nd plate
𝑥𝐿𝐾 0.205 𝑥𝐿𝐾 𝑥𝐿𝐾
( ) =  ( ) = 0.8266 < ( )
𝑥𝐻𝐾 2𝑛𝑑 0.248 𝑥𝐻𝐾 2𝑛𝑑 𝑥𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦

3rd Plate
Table 15-3rd Plate Vapor and Liquid Compositions

Component Xi,W Yi,240.9 Xi,3 K234.4 Yi,3


P5 0.000 0.000 0.000 18.602 0.000
m-xylene 0.000 0.000 0.000 2.249 0.000
o-xylene(LK) 0.024 0.205 0.131 2.010 0.264
A9 0.066 0.358 0.239 1.678 0.401
P11(HK) 0.303 0.248 0.270 0.703 0.190
A10 0.523 0.178 0.318 0.427 0.136
A11 0.084 0.013 0.042 0.238 0.010
1.001 1.001
Temperature of 3rd plate - 234.4℃
For 3rd plate
𝑥𝐿𝐾 0.264 𝑥𝐿𝐾 𝑥𝐿𝐾
( ) =  ( ) = 1.3894 < ( )
𝑥𝐻𝐾 3𝑟𝑑 0.190 𝑥𝐻𝐾 3𝑟𝑑 𝑥𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦

22
4th Plate
Table 16-4th Plate Vapor and Liquid Compositions

Component Xi,W Yi,234.4 Xi,4 K230.2 Yi,4


P5 0.000 0.000 0.000 17.670 0.000
m-xylene 0.000 0.000 0.000 2.094 0.000
o-xylene(LK) 0.024 0.264 0.166 1.870 0.311
A9 0.066 0.401 0.265 1.559 0.413
P11(HK) 0.303 0.190 0.236 0.645 0.152
A10 0.523 0.136 0.293 0.391 0.115
A11 0.084 0.010 0.040 0.216 0.009
1.001 1.000
Temperature of 4th plate - 230.2℃
𝑥𝐿𝐾 0.311 𝑥𝐿𝐾 𝑥𝐿𝐾
( ) =  ( ) = 2.04 < ( )
𝑥𝐻𝐾 4𝑡ℎ 0.152 𝑥𝐻𝐾 4𝑡ℎ 𝑥𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦

5th Plate
Table 17-5th Plate Vapor and Liquid Compositions

Component Xi,W Yi,230.2 Xi,5 K230.2 Yi,5


P5 0.000 0.000 0.000 17.173 0.000
m-xylene 0.000 0.000 0.000 2.012 0.000
o-xylene(LK) 0.024 0.311 0.194 1.796 0.349
A9 0.066 0.413 0.272 1.497 0.408
P11(HK) 0.303 0.152 0.213 0.615 0.131
A10 0.523 0.115 0.281 0.372 0.104
A11 0.084 0.009 0.039 0.204 0.008
1.000 1.000
Temperature of 5th plate - 227.9℃
𝑥𝐿𝐾 0.349 𝑥𝐿𝐾 𝑥𝐿𝐾
( ) =  ( ) = 2.66 > ( )
𝑥𝐻𝐾 5𝑡ℎ 0.131 𝑥𝐻𝐾 5𝑡ℎ 𝑥𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦

Stripping section tray calculation should be stopped. Because,


𝑥𝐿𝐾 𝑥𝐿𝐾
( ) ≥( )
𝑥𝐻𝐾 5𝑡ℎ 𝑥𝐻𝐾 𝐹𝑒𝑒𝑑 𝑇𝑟𝑎𝑦

4.7.3 Number of trays


 According to the aspen plus Calculations, the feed temperature is 212.513℃.
 According to the calculation of rectifying section and stripping section,
 The 9th plate (Numbered from top to bottom) temperature is 207.4℃.
 The 5th plate (numbered from the bottom) temperature is 227.9 ℃.
 The closest value for aspen plus calculated value is 207.4 ℃. So the 9th plate from the
top is considered as the feed plate.
 Number of plates in the rectifying section including feed plate – 9 Plates
23
 Number of plates in the stripping section excluding feed plate – 4 Plates
 Total number of plates in the column - 9 + 4 = 𝟏𝟑 Plates

Figure 4-4-Aspen Plus Simulation Results

4.8 Determination of average density of vapor /liquid in rectifying and


stripping sections
Note: Molar volume values are calculated by using Aspen
Plus software.

V – Vapor flow rate of rectifying section

L - Liquid flow rate of rectifying section

V’ – Vapor flow rate of stripping section

L’ –Liquid flow rate of stripping section

Feed Plate – 9th Plate of the column

4.8.1 Rectifying Section


Figure 4-3-Liquid & Vapor Flow Through
The Column
1st Plate
Table 18-Density calculation of the vapor leaving from 1st plate of rectifying section

Molar
Volume Molar Mass Weight
Component Yi,D volume
m3 (kg/mol) kg
m3/kmol
P5 0.094 11.440 1.075 0.072 6.782
m-xylene 0.017 11.440 0.194 0.106 1.805
o-xylene(LK) 0.672 11.440 7.687 0.106 71.340
A9 0.214 11.440 2.448 0.120 25.723
P11(HK) 0.002 11.440 0.023 0.156 0.313
24
A10 0.000 11.440 0.000 0.128 0.000
A11 0.000 11.440 0.000 0.142 0.000
11.428 105.962

105.962
Density of vapor leaving from 1st plate- 11.428 = 𝟗. 𝟐𝟕 𝒌𝒈/𝒎𝟑

Table 19-Density calculation of the liquid leaving from 1st plate of rectifying section

Volume Molar Mass Weight


Component Xi,D,194.8 m3/kmol
m3 (kg/mol) kg
P5 0.009 0.218 0.002 0.072 0.614
m-xylene 0.016 0.218 0.003 0.106 1.663
o-xylene(LK) 0.699 0.218 0.152 0.106 74.192
A9 0.270 0.218 0.059 0.120 32.408
P11(HK) 0.007 0.218 0.002 0.156 1.079
A10 0.000 0.218 0.000 0.128 0.000
A11 0.000 0.218 0.000 0.142 0.000
0.217 109.956
109.956
Density of liquid leaving from 1st plate- = 𝟓𝟎𝟓. 𝟕𝟒 𝒌𝒈/𝒎𝟑
0.217

9th Plate – Feed Plate


Molar volume of the vapor mixture - 11.749 m3/kmol (By using Aspen plus)
Volume of the mixture - 11.749 m3
Weight of the mixture - 114.284 kg

Density of vapor leaving from feed plate - 114.284⁄11.749 = 9.727 𝑘𝑔/𝑚^3

8th Plate
Molar volume of the liquid mixture - 0.251 m3/kmol (By using Aspen plus)

Volume of the mixture - 0.251 m3

Weight of the mixture - 118.146kg

Density of liquid leaving from 8th plate - 118.146⁄0.251 = 470.11 𝑘𝑔/𝑚^3

4.8.2 Stripping Section


9th Plate – Feed Plate

Molar volume of the liquid mixture - 0.371 m3/kmol (By using Aspen plus)

Volume of the mixture - 0.372 m3

25
Weight of the mixture - 121.119 kg

Density of liquid leaving from feed plate - 121.119⁄0.372 = 325.86 𝑘𝑔/𝑚^3

10th Plate

Molar volume of the vapor mixture - 12.358 m3/kmol (By using Aspen plus)

Volume of the mixture - 12.358 m3

Weight of the mixture - 122.428 kg

Density of vapor leaving from 10th plate - 122.428⁄12.358 = 9.91 𝑘𝑔/𝑚^3

13th Plate

Molar volume of the liquid mixture - 0.764 m3/kmol (By using Aspen plus)

Volume of the mixture - 0.751 m3

Weight of the mixture - 133.616 kg

Density of liquid leaving from feed plate - 133.616⁄0.751 = 178.01 𝑘𝑔/𝑚^3

Reboiler

Molar volume of the Vapor mixture - 11.409 m3/kmol (By using Aspen plus)

Volume of the mixture - 11.066 m3

Weight of the mixture - 131.430 kg

Density of vapor leaving from 10th plate - 131.430⁄11.066 = 11.88 𝑘𝑔/𝑚^3


9.91 +11.88
Average Density of vapor in stripping section –𝜌𝑉 ′ = = 𝟏𝟎. 𝟗𝟎 𝒌𝒈/𝒎𝟑
2

325.86 +178.01
Average Density of liquid in stripping section - 𝜌𝐿′ = = 𝟐𝟓𝟏. 𝟗𝟒 𝒌𝒈/𝒎𝟑
2

Summary:
Table 20-Summary of density calculations

Flow streams 𝒌𝒈⁄


Average Density( )
𝒎𝟑
𝜌𝑉 9.50

𝜌𝐿 487.93

26
𝜌𝑉 ′ 10.90

𝜌𝐿′ 251.94

4.9 Determination of average molecular weights and l/V mass flow rates in
the column
Average molecular weight of feed - MWavr,feed

𝑀𝑊𝑎𝑣𝑟,𝑓𝑒𝑒𝑑 = 0.06 × 0.0722 + 0.01 × 0.1062 + 0.43 × 0.1062 + 0.16 × 0.1202 + 0.11
× 0.1563 + 0.19 × 0.1282 + 0.03 × 0.1422
MWavr,feed = 0.117 kg/mol
Similarly,
Table 21-Summary of Average molecular weights Calculations

Streams Average Molecular Weight

Feed 0.117 kg/mol

Distillate 0.106 kg/mol

Bottom 0.137 kg/mol

4.10 Determination of liquid/vapor mass flow rates


 Average molecular weight of the rectifying section –

0.117 + 0.106
𝑀𝑊𝑟𝑒𝑐𝑡𝑖𝑓𝑦𝑖𝑛𝑔 = = 0.112 𝑘𝑔/𝑚𝑜𝑙
2

 Average molecular weight of stripping section–


0.117 + 0.137
𝑀𝑊𝑠𝑡𝑟𝑖𝑝𝑝𝑖𝑛𝑔 = = 0.127 𝑘𝑔/𝑚𝑜𝑙
2
 Mass flow rates of stripping section and rectifying section can be calculated as follows.
Table 22- Summary of mass flow rates of stripping section and rectifying section

Flow rate Molecular weight Flow rates Flow rates


Flow rates
𝐾𝑚𝑜𝑙/ℎ𝑜𝑢𝑟 𝑘𝑔/𝑚𝑜𝑙 𝐾𝑔/ℎ𝑜𝑢𝑟 𝑘𝑔/𝑠

V 120.39 0.112 13483.68 3.75

L 34.40 0.112 3852.8 1.07

27
V' 72.83 0.127 9249.41 2.57

L' 122.74 0.127 15587.98 4.33

4.11 Internal column design


In here, the diameter of the rectifying and stripping section of the column, dimensions of the
column plates and the tray spacing are calculated.

4.11.1 Rectifying section


The diameter and the trays spacing of the rectifying section of the column is calculated in here.
Then, the calculated diameter should be checked for flooding. If flooding happens, the
calculated values should be change according to correct specification.

1.1.1.1 Plate Spacing


The plate spacing means the distance between two trays. The overall height of the column will
depend on the plate spacing. Usually plate spacing varies from 0.15 m to 1 m. Most columns
have 0.6 m tray spacing. Thus, the plate spacing is assumed to be 0.6 m.

Note: It should be checked if this value for plate spacing is compatible with the column
diameter, after calculating the Dc.

1.1.1.2 Liquid/vapor flow rate inside the column.

Liquid and vapor flow rates inside the rectifying section were calculated in the
previous chapter using material balance equations.

Table 23-Liquid/vapor flow rate inside the rectifying section of the column

Flow rate Flow rates Flow rates


Flow rates
𝑘𝑚𝑜𝑙/ℎ𝑜𝑢𝑟 𝑘𝑔/ℎ𝑜𝑢𝑟 𝑘𝑔/𝑠
V 120.39 13483.68 3.75
L 34.40 3852.8 1.07

28
1.1.1.3 Flooding vapor velocity (𝑼𝒇 )
Flooding vapor velocity can be calculated using the liquid-vapor flow factors 𝐹𝐿𝑉 and
tray spacing.
𝐿 𝜌 𝐿𝑊 - Liquid mass flow rate (𝑘𝑔/𝑠 )
𝐹𝐿𝑉 = 𝑉𝑊 √ 𝜌𝑉
𝑊 𝐿 𝑉𝑊 - Vapor mass flow rate (𝑘𝑔/𝑠 )
𝜌𝐿 - Average Vapor density (𝑘𝑔/𝑚3 )
𝜌𝐿 −𝜌𝑉 𝜌𝑉 - Average liquid density (𝑘𝑔/𝑚3 )
𝑈𝑓 = 𝐾1 √ 𝜌𝑉

Average Density
𝒌𝒈 3.75 9.50
𝜌𝐿 − 487.93 ⁄ 𝟑 𝐹𝐿𝑉 = √ = 0.489
𝒎 1.07 487.93
𝒌𝒈⁄
𝜌𝑉 − 9.50
𝒎𝟑

From the graph; K value is 0.056

487.93 − 9.50
𝑈𝑓 = 0.056 × √
9.50
= 0.397 𝑚/𝑠

Figure 4-5-Flooding Velocity Sieves Plates

1.1.1.4 Actual Vapor Velocity


Generally, otho-xylene columns are designed for 80% flooding at maximum feed
rate. Thus,
𝑈𝑎,𝑚𝑎𝑥 = 𝑈𝑓 × 80% = 0.397 × 0.80 = 0.318 𝑚/𝑠

29
1.1.1.5 Maximum Volumetric Vapor Flow rate
𝑉𝑤 3.75 𝑚3
𝑉𝑣 = = = 0.395
𝜌𝑣 9.50 𝑠

1.1.1.6 Net area Required


𝑉𝑣 0.395
(𝐴𝑛𝑒𝑡 ) = 𝑈 = = 1.242 𝑚2
𝑎,𝑚𝑎𝑥 0.318

As First trial down comer area is 12% of column cross sectional area.

𝐴𝑛𝑒𝑡 1.242
𝐴𝑐 = = = 1.411 𝑚2
(1 − 0.12) 1 − 0.12
1.1.1.7 Column Diameter
4×𝐴𝑐 4×1.411
(𝐷𝐶 ) - √ = √ = 1.34 𝑚
𝜋 𝜋

4.11.2 Stripping section


The diameter and the trays spacing of the stripping section of the column is calculated in here.
1.1.1.8 Plate Spacing –
Assume the plate spacing as 0.60 m.

1.1.1.9 Liquid/vapor flow rate inside the column.


Table 24-Liquid/vapor flow rate inside the Stripping section of the column

Flow rate Flow rates Flow rates


Flow rates
𝐾𝑚𝑜𝑙/ℎ𝑜𝑢𝑟 𝐾𝑔/ℎ𝑜𝑢𝑟 𝑘𝑔/𝑠
V' 72.83 9249.41 2.57
L' 122.74 15587.98 4.33

1.1.1.10 Flooding vapor velocity (𝑼𝒇 )


Flooding vapor velocity can be calculated using the liquid-vapor flow factors 𝐹𝐿′𝑉′ and
tray spacing.
𝜌𝐿′ − 251.94 𝒌𝒈⁄𝒎𝟑

𝜌𝑉 ′ − 10.90 𝒌𝒈⁄𝒎𝟑 4.33 10.90


𝐹𝐿′𝑉′ = √ = 0.350
2.57 251.94

According to the graph shown in figure 4-5; K value is 0.068

251.94 − 10.90
𝑈𝑓 = 0.068 × √ = 0.320 𝑚/𝑠
10.90
30
1.1.1.11 Actual Vapor Velocity
In the same way as for the rectifying section,
(𝑈𝑎,𝑚𝑎𝑥 ) = 𝑈𝑓 × 80% = 0.320 × 0.80 = 0.256 𝑚/𝑠

1.1.1.12 Maximum Volumetric Vapor Flow rate


In the same way as for the rectifying section,
𝑉𝑤 2.57
𝑉𝑣 = = = 0.236 𝑚3 /𝑠
𝜌𝑣 10.90

1.1.1.13 Net area Required


In the same way as for the rectifying section,
𝑉𝑣 0.236
(𝐴𝑛𝑒𝑡 ) - 𝑈 = = 0.922 𝑚2
𝑎,𝑚𝑎𝑥 0.256

As First trial, down comer area is 12% of the column cross sectional area.
𝐴𝑛𝑒𝑡 0.922
𝐴𝑐 = = = 1.048 𝑚2
(1 − 0.12) 1 − 0.12
1.1.1.14 Column Diameter
4×𝐴𝑐 4× 1.048
𝐷𝐶 = √ = √ = 1.16 𝑚
𝜋 𝜋

 Rectifying section diameter – 1.34 m


 Stripping section diameter – 1.16 m
There is a difference between rectifying section diameter and stripping section diameter. The
greater value should be taken as the column diameter. Thus, the column diameter is 1.34m.

31
4.11.3 Verification of Tray Spacing
According to the table, since tower diameter is in between 1-3m, tray spacing should be 0.60.

Figure 4-6-Recommended General Condition & Dimensions for Tray Towers

Therefore, the assumed value for tray spacing is compatible. Hence, the assumed value for tray
spacing acceptable.

4.12 Tray hydraulic design


4.12.1 Liquid flow arrangement
 The column diameter – 1.34 m
 Average liquid flow rate of the column –
1.07 + 4.33 𝑘𝑔
= 2.7 ⁄𝑠
2

 Average density of the liquid

487.93 + 251.94 𝑘𝑔
= 369.94 ⁄𝑚3
2

 Average liquid flow rate -


2.7 3
= 0.0073 𝑚 ⁄𝑠
369.94
 According to the graph and flow rate, single
pass (cross flow) flow pattern can be chosen
as liquid flow arrangement.

4.12.2 Rectifying Section Figure 4-7-Selection of Liquid Flow Arrangement


𝜋
 Column area(𝐴𝑐 ) - 4 × (1.34)2 =
𝟏. 𝟒𝟏𝟎 𝒎𝟐
 Down comer area(𝐴𝑑 ) - 𝐴𝑐 × 12% = 𝟎. 𝟏𝟔𝟗 𝒎𝟐
 Net column Area(𝐴𝑛𝑒𝑡 ) - 𝐴𝑐 − 𝐴𝑑 = 1.410 − 0.169 = 𝟏. 𝟐𝟒𝟏 𝒎𝟐
 Active area(𝐴𝑎 ) - 𝐴𝑐 − 2 𝐴𝑑 = 1.410 − 2 × 0.169 = 𝟏. 𝟎𝟕𝟐 𝒎𝟐
8
 Hole area (𝐴ℎ ) - 𝐴𝑎 × 8% = 1.072 × 100 = 𝟎. 𝟎𝟖𝟓𝟖 𝒎𝟐
32
 Hole size
The holes’ sizes are varied from 2.5 to 12 mm. 5 mm is the preferred size for
holes (diameter).

0.0858
 Number of holes - 0.005 2
= 𝟒𝟑𝟔𝟗. 𝟕𝟔 ≈ 𝟒𝟑𝟕𝟎 𝒉𝒐𝒍𝒆𝒔
𝜋×( )
2

𝐴𝑑 𝐴
 Weir length - ( ⁄𝐴 ) = 𝑑⁄𝐴 × 100 = 0.169⁄1.410 × 100 = 12%
𝑐 𝑐
By using the graph,
𝑙𝑤
= 0.77
𝐷𝑐
𝑙𝑤 = 1.34 × 0.77
𝑙𝑤 = 𝟏. 𝟎𝟑𝟐 𝒎
 Weir liquid crest
The height of the liquid crest over the weir can be
estimated using the Francis weir formulae.
2
𝐿 3
ℎ𝑜𝑤 = 750 × [ ]
𝜌𝐿 𝑙𝑤

Liquid flow rate (𝐿) − 1.07 kg/s


Average density (𝜌𝐿 ) − 487.93kg/m3 Figure 4-8-Relation between Down-Comer Area
and Weir Length
Weir length (𝑙𝑤 ) − 1.032 𝑚
2
1.07 3
ℎ𝑜𝑤 = 750 × [487.93×1.018] = 𝟏𝟐. 𝟓𝟏 𝒎𝒎

 Check for Weeping


The design should be checked for the weeping and if unsatisfactory calculation should be
repeated with small alteration.

Assume weir height as 45 mm.

33
ℎ𝑜𝑤 + ℎ𝑤 = 12.51 + 45 = 57.51 𝑚𝑚
By the Graph;
𝐾2 − 30.40
[𝐾2 − 0.9(25.4 − 𝐷ℎ ]
𝑈ℎ,𝑚𝑖𝑛 =
√𝜌𝑣

𝑈ℎ,𝑚𝑖𝑛 − Minimum vapor velocity through


the holes (based on the hole area)
𝐷ℎ − Hole diameter
𝜌𝑉 = 9.50 𝑘𝑔/𝑚3
[30.60 − 0.9(25.4 − 5]
Figure 4-9-Weep Point Correlation 𝑈ℎ,𝑚𝑖𝑛 =
√9.50
= 3.906 𝑚/𝑠
Actual minimum vapor flow rate
𝑀𝑖𝑛𝑖𝑚𝑢𝑚 𝑣𝑎𝑝𝑜𝑟 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦 0.395
𝑈𝑎,𝑚𝑖𝑛 = = = 4.2540 𝑚/𝑠
𝐴ℎ 0.0858
𝑈𝑎,𝑚𝑖𝑛 > 𝑈ℎ,𝑚𝑖𝑛
Minimum vapor velocity is greater than
the minimum vapor velocity through the
holes. Therefore, weeping doesn’t
occur.

 Check for Entrainment


The design should be checked for the
entrainment and if unsatisfactory
calculation should be repeated with
small alteration.
Vapor velocity is given by
𝑉𝑣 0.395 𝑚
𝑈𝑣 = = = 0.318
𝐴𝑛𝑒𝑡 1.241 𝑠

The percentage flooding -


𝑈𝑣 0.318
= × 100 = 80.1 %
𝑈𝑓 0.397
𝐹𝐿𝑉 = 0.489 Figure 4-10-Entrainment Correlation for Sieve Plates

By graph; 𝛹 = 0.0025 < 0.1  the value is satisfactory.


34
4.12.3 Stripping Section
𝜋
 Column area(𝐴𝑐 ) - 4 × (1.16)2 = 𝟏. 𝟎𝟓𝟕 𝒎𝟐

 Down comer area(𝐴𝑑 ) - 𝐴𝑐 × 15% = 𝟎. 𝟏𝟓𝟗 𝒎𝟐


 Net column Area(𝐴𝑛𝑒𝑡 ) - 𝐴𝑐 − 𝐴𝑑 = 1.057 − 0.159 = 𝟎. 𝟖𝟗𝟖 𝒎𝟐
 Active area(𝐴𝑎 ) - 𝐴𝑐 − 2 𝐴𝑑 = 1.410 − 2 × 0.169 = 𝟎. 𝟕𝟑𝟗 𝒎𝟐
8
 Hole area (𝐴ℎ ) - 𝐴𝑎 × 8% = 1.072 × 100 = 𝟎. 𝟎𝟓𝟗 𝒎𝟐

 Hole size
The holes’ sizes are varied from 2.5 to 12 mm. 5 mm is the preferred size for
holes (diameter).

0.059
 Number of holes - 0.005 2
= 𝟑𝟎𝟎𝟒. 𝟖𝟒 ≈ 𝟑𝟎𝟎𝟓 𝒉𝒐𝒍𝒆𝒔
𝜋×( )
2

𝐴𝑑 𝐴
 Weir length - ( ⁄𝐴 ) = 𝑑⁄𝐴 × 100 = 15%
𝑐 𝑐
By using the graph shown in figure 4-9,
𝑙𝑤
= 0.81  𝑙𝑤 = 1.16 × 0.81  𝑙𝑤 = 𝟎. 𝟗𝟒𝟎 𝒎
𝐷𝑐

 Weir liquid crest


The height of the liquid crest over the weir can be estimated using the Francis weir
formulae.
2 Liquid flow rate (𝐿) − 4.33 kg/s
𝐿 3
ℎ𝑜𝑤 = 750 × [ ] Average density (𝐿𝐿 ) − 251.94kg/m3
𝜌𝐿 𝑙𝑤
Weir length (𝐿𝐿 ) − 0.940 𝐿

2
4.33 3
ℎ𝑜𝑤 = 750 × [251.94×0.94] = 𝟓𝟐. 𝟎𝟓 𝒎𝒎

 Check for Weeping


The design should be checked for the weeping and if unsatisfactory calculation should be
repeated with small alteration.

Assume weir height as 45 mm.


ℎ𝑜𝑤 + ℎ𝑤 = 52.05 + 45 = 97.05 𝑚𝑚
By the Graph: 𝐾2 − 31
[𝐾2 − 0.9(25.4 − 𝐷ℎ ]
𝑈ℎ,𝑚𝑖𝑛 =
√𝜌𝑣 ′
35
𝜌𝑉′ = 10.90 𝑘𝑔/𝑚3
[31 − 0.9(25.4 − 5]
𝑈ℎ,𝑚𝑖𝑛 = = 3.829 𝑚/𝑠
√10.9
Actual minimum vapor flow rate
𝑀𝑖𝑛𝑖𝑚𝑢𝑚 𝑣𝑎𝑝𝑜𝑟 𝑣𝑒𝑙𝑜𝑐𝑖𝑡𝑦 0.236
𝑈𝑎,𝑚𝑖𝑛 = = = 4.00 𝑚/𝑠
𝐴ℎ 0.059

𝑈𝑎,𝑚𝑖𝑛 > 𝑈ℎ,𝑚𝑖𝑛

Minimum vapor velocity is greater than the minimum vapor velocity through the holes.
Therefore, weeping doesn’t occur.

 Check for Entrainment


The design should be checked for the entrainment and if unsatisfactory situations occur,
calculation should be repeated with small alteration.

Vapor velocity is given by,


𝑉𝑣 0.236 𝑚
𝑈𝑣 = = = 0.190
𝐴𝑛𝑒𝑡 1.241 𝑠
The percentage flooding -
𝑈𝑣 0.190
= × 100 = 59.37 %
𝑈𝑓 0.320
𝐹𝐿𝑉 = 0.350

By the graph shown in figure 4-10,


; 𝛹 = 0.0025 < 0.1  the value is satisfactory.

4.13 Height of the column


The actual height of the column depends on the overall plate efficiency of the column. Different
kind of methods are used to calculate the column efficiency. In here, O’Connell’s correlation
is used. The molar average viscosity is calculated using the ASPEN PLUS Simulation software.

4.13.1 Estimate of overall plate efficiency using o’Connell’s correlation


Equation: 𝐸𝑜 = 51 − 32.5log(𝜇𝑎 𝛼𝑎 )

where 𝜇𝑎 - the molar average liquid viscosity , 𝑚𝑁𝑠/𝑚2

𝛼𝑎 - the average relative volatility of light key.

Feed temperature – 207.4℃

36
molar average liquid viscosity - 𝜇𝑎 - 0.216 𝑚𝑁𝑠/𝑚2 (When vapor fraction = 0.5) [Aspen plus
V8.0]

Average relative volatility of light key (o-xylene)

∝𝐿𝐾,𝑎𝑣𝑒𝑟𝑎𝑔𝑒 = √∝𝐿𝐾,𝑇,𝐷,𝑑𝑒𝑤 𝑝𝑜𝑖𝑛𝑡 × ∝𝐿𝐾,𝑇,𝑅,𝑏𝑢𝑏𝑏𝑙𝑒 𝑝𝑜𝑛𝑡

∝𝐿𝐾,𝑎𝑣𝑒𝑟𝑎𝑔𝑒 = √3.319 × 2.658 = 2.97

Overall column efficiency:

𝐸𝑜 = 51 − 32.5 log(2.97 × 0.216)

= 57.265%

4.13.2 Number of actual trays required


Total No of trays actually required

𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑛𝑜 𝑜𝑓 𝑡𝑟𝑎𝑦 13
- = = 𝟐𝟐. 𝟕𝟎 ≈ 𝟐𝟑 𝒕𝒓𝒂𝒚𝒔
𝑡𝑟𝑎𝑦 𝑒𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 0.5726

No of trays in rectifying section- 9⁄0.5726 = 15.71 ≈ 16 𝑡𝑟𝑎𝑦𝑠

No of trays in rectifying section- 4⁄0.5726 = 6.98 ≈ 7 𝑡𝑟𝑎𝑦𝑠

4.13.3 Height of the column


Height of the column – no of actual trays × tray spacing

−0.60 × 23 = 𝟏𝟑. 𝟖𝟎 𝒎

37
4.14 Summary of chemical design
Table 25-Summary of Chemical Design

Parameter Section Calculated value Units


Column height - 13.80 m
Total number of trays - 23 -

No of trays in each Rectifying 16 -


section stripping 07 -
Operating Reflux ratio - 0.4 -
Feed tray location - 16th plate -
Rectifying 1.34 m
Diameter of the column
stripping 1.16 m
Plate type - Sieve type -
Rectifying 45 mm
Weir height
stripping 45 mm
Rectifying 1.032 m
Weir length
stripping 0.940 m
Rectifying 1.072 m2
Active area
stripping 0.739 m2
Rectifying 5 mm
Hole size
stripping 5 mm
Rectifying 4370 -
Number of holes
stripping 3005 -
Rectifying 0.169 m2
Downcomer area
stripping 0.159 m2
Liquid flow arrangement - Cross flow -

Reboiler - Partial -

Condenser - Total -

38
CHAPTER 5 - OVERVIEW TO DETAILED MECHANICAL DESIGN
The bottom product of the xylene splitter being distillated is a mixture of xylene, aromatics
(A9, A10, A11) and i-paraffin which is a toxic and lethal liquid. The maximum operating pressure
of the distillation column is 390kPa and the maximum operating temperature is 258℃.
Therefore, by considering the nature of the product and the operating conditions this vessel,
can be categorized as a heavy duty vessel (U-68) which is operating up to
15000psi(10342.14kPa) pressure and no limit for operating temperature. The procedure for
detailed mechanical design of the distillation column can be carried out step by step as follows.

 Determining the main geometry, main dimensions & operating conditions


 Selection of the material of fabrication based on the required properties
 Determining the welding techniques and the design allowances
 Determining the required thicknesses of various components

5.1 Main geometry of the vessel


The main geometry of the distillation column is a cylindrical shell with a two hemispherical
enclosures at the top and bottom. The diameters of the stripping and rectifying section are
different. Thus, the two cylindrical parts of those sections are joined by using a conical vessel.

5.2 Main dimensions of the vessel


Dimensions of the distillation column have been calculated and the values are as follows,

 Diameter of the rectifying section = 1.34 m


 Height of the rectifying section – 16×0.6 = 9.6 m
 Diameter of the Stripping section = 1.16 m
 Height of the stripping section – 07×0.6 = 4.2 m

5.3 Operating conditions


Operating conditions of the column have been calculated and the values are as follows
 Maximum pressure at the rectifying section - 390kPa
 Maximum temperature of the rectifying section - 222℃
 Maximum pressure at the stripping section - 340kPa
 Maximum temperature of the stripping section - 258℃

39
CHAPTER 6 - MATERIAL SELECTION FOR CONSTRUCTION
A common material is used for the construction of the distillation column including the shells,
plates, closures of rectifying and stripping sections. Also, the material is used for the
construction of supports, nuts and bolts and pipelines for product and feed.

6.1 Selection of Material


The common materials that are used to construct vessels are steels, nonferrous materials such
as aluminum and copper, specialty metals such as titanium and zirconium and nonmetallic
materials, such as, plastic and composites.

Commercially, steels can be classified into four groups namely, plain carbon steel, low alloy
steel, high alloy steel and clad steel. Plain carbon steel also can be divided as low, medium,
high and very high. Among Plain carbon steels, only law density plain carbon can be used for
process vessels. Others are usually used to fabricate nuts and bolts.

The bottom product of the xylene splitter being distillated, is a mixture of xylene, aromatics
(A9, A10, A11) and i-paraffin which are non-corrosive compounds. Thus, plain carbon steel is
suitable for the design of distillation column. Also, this distillation can be constructed by using
high alloy carbon steels. However, high alloy carbon steel is more expensive than plain carbon
steel. The non-ferrous materials are also costly than plain carbon steel. PVC, Polyolefin, Glass-
fiber reinforced plastics (GRP) are some examples for non-metallic materials that are used for
constructing pressure vessels. However, since xylene and other aromatics are highly flammable
and toxic, nonmetallic materials like plastics, PVC, glass fiber are not suitable for the column
design.

Figure 6-1-ASME Boiler & Pressure Vessel Code 2008 - DIVISION 1-- SECTION VIII;AND SECTION XII; SECTION I;
SECTION II

There are a lot of grades in plain carbon steel. Among them, most suitable grade for process
vessel designing is SA-299 (Gandy, 2007). Normally, the thickness of the shell is smaller than

40
25mm.Thus, 17th product form is selected for the design of the distillation column (Anon.,
2008).

Some properties of SA-299 are tabulated below.


Table 26- Properties of the Selected Material

Properties SA-290
Material type Carbon steel plate (< 25)
Maximum Tensile Strength (MPa) 515
Maximum Yield Strength (MPa) 290

6.2 Welding Technique


According to Table UW-12 in ASME Boiler & Pressure Vessel Code 2008 - SECTION VIII -
DIVISION 1, type of welding joint used will be the type 1, which is butt joints and spot
radiography will be used as the non-destructive testing method. Therefore, the weld joint
efficiency is taken as 0.85 for column design.

6.3 Corrosion Allowance


Corrosion allowance is the amount of material in a pipe or vessel that is available for corrosion
without affecting the pressure containing integrity. Therefore, an extra measurement is added
to the thickness of the wall. A value of 0.10-inches(2.50mm) was commonly added as the
corrosion allowance for carbon-steel. (G. A. Aaker, n.d.).

41
CHAPTER 7 - MECHANICAL DESIGN OF THE DISTILLATION
7.1 Parameter calculation
In this section, important parameters such as the design pressure, design temperature for the
stripping and rectifying sections of the distillation column and design stresses for SA-290 are
calculated.

7.1.1 Design Pressure


This section of the report contains the calculation of design pressure for the rectifying section
and stripping section separately.

7.1.1.1 Design Pressure for Rectifying Section


Atmospheric temperature – 101.235kPa

Maximum pressure at the rectifying section - 390kPa

According to Section VIII of ASME Boiler & Pressure Vessel Code 2008, this belongs to the
category where,

Pin  Pexternal

Pdesign  Pmax.operating by gauge  (10) % extra

10
𝑃𝐷𝑒𝑠𝑖𝑔𝑛 − [390 + 390 × ] = 429 𝑘𝑃𝑎
100
Absolute design pressure (𝑃𝐴𝑏𝑠𝑜𝑙𝑢𝑡𝑒 ) − 429 + 101.325 = 530.325𝐾𝑝𝑎
7.1.1.2 Design Pressure for Stripping Section
Maximum pressure at the Stripping section - 340kPa

According to Section VIII of ASME Boiler & Pressure Vessel Code 2008, this belongs to the
category where,

Pin  Pexternal

Pdesign  Pmax.operating by gauge  (10) % extra

10
𝑃𝐷𝑒𝑠𝑖𝑔𝑛 − [340 + 340 × ] = 374 𝑘𝑃𝑎
100
Absolute design pressure (𝑃𝐴𝑏𝑠𝑜𝑙𝑢𝑡𝑒 ) − 374 + 101.325 = 475.325k𝑃𝑎
7.1.2 Design Temperature
Design temperatures for both the rectifying section and the stripping section have been
calculated here.
42
7.1.2.1 Design Temperature for Rectifying section
The maximum temperature involved in the rectifying section is the feed temperature which is
222℃. Since, non-direct heating is used,

T o design  T o heating medium


T o design  T o highest temperature of body  100 C

𝑇 𝑜 𝐷𝑒𝑠𝑖𝑔𝑛 of the rectifying section = 222 + 10 = 232℃

7.1.2.2 Design Temperature for Stripping section


The maximum temperature involved in the rectifying section is the reboiler temperature which
is 258℃. Since, non-direct heating is used,

𝑇 𝑜 𝐷𝑒𝑠𝑖𝑔𝑛 of the stripping section = 258 + 10 = 268 ℃

7.1.3 Design Stress


Design Stress is calculated in terms of the maximum allowable stress at the design temperature.

𝜎𝐷𝑒𝑠𝑖𝑔𝑛,𝑅𝑒𝑐𝑡𝑖𝑓𝑦𝑖𝑛𝑔 𝑆𝑒𝑐𝑡𝑖𝑜𝑛 − 148 MPa 𝜎𝐷𝑒𝑠𝑖𝑔𝑛,𝑆𝑡𝑟𝑖𝑝𝑝𝑖𝑛𝑔 𝑆𝑒𝑐𝑡𝑖𝑜𝑛 − 148 MPa

7.2 Thickness Calculation


In order to calculate the thickness of the distillation shell, the following equation is used which
is given in UG27, Section VIII, ASME Boiler & Pressure Vessel Code 2008.

𝑷𝑫𝒆𝒔𝒊𝒈𝒏 × 𝑫
𝑡𝑎𝑐𝑡𝑢𝑎𝑙 = +𝑐
2 × 𝜑 × 𝝈𝑫𝒆𝒔𝒊𝒈𝒏

7.2.1 Rectifying section


𝑷𝑫𝒆𝒔𝒊𝒈𝒏 × 𝑫𝒊 530.325 × 1.34
𝑡𝑎𝑐𝑡𝑢𝑎𝑙 = +𝑐 = + 2.5 = 5.33 𝑚𝑚
2 × 𝜑 × 𝝈𝑫𝒆𝒔𝒊𝒈𝒏 − 𝑷𝑫𝒆𝒔𝒊𝒈𝒏 2 × 0.85 × 148 − 530.325 × 10−3

Actual wall thickness of the rectifying section is = 5.33 𝑚𝑚


Table 27-Dimeters vs thickness-Chemical Engineering Volume 6

Vessel Diameter(m) Minimum Thickness (mm)

1 5
1 to 2 7
2 to 2.5 9
2.5 to 3.0 10
3.0 to 3.5 10

43
Internal diameter of the rectifying section of column is 1.34 m.

According to the table given above, the minimum shell thickness should be about 7mm. In this
design, the calculated theoretical shell thickness is 5.33mm. Therefore, 7mm is selected as the
shell thickness of the rectifying section of the column.

However available thickness of the metal in market is 7.94mm (5/16 inch).

Mean diameter of the rectifying section – 1.34 +0.00798 – 1.348m

7.2.2 Stripping Section


𝑷𝑫𝒆𝒔𝒊𝒈𝒏 × 𝑫𝒊 475.325 × 1.16
𝑡𝑎𝑐𝑡𝑢𝑎𝑙 = +𝑐 = + 2.5 = 4.70 𝑚𝑚
2 × 𝜑 × 𝝈𝑫𝒆𝒔𝒊𝒈𝒏 − 𝑷𝑫𝒆𝒔𝒊𝒈𝒏 2 × 0.85 × 148 − 475.325 × 10−3

Actual wall thickness of the rectifying section is = 4.69 𝑚𝑚


Internal diameter of the stripping section of the column is 1.16m

According to the table-2 given above, the minimum shell thickness should be about 7mm. Our
calculated theoretical shell thickness is 4.70mm. Therefore, 7mm is selected as shell thickness
of the rectifying section of the column.

However available thickness of the metal in market is 7.94mm (5/16 inch).

Mean diameter of the stripping section (Do) – 1.16 +0.00794 – 1.168m

7.3 Design of top and bottom enclosures


In order to facilitate better stress distribution, the top and bottom enclosure are chosen as two
ASME coded type flanged and dished heads (tori-spherical head). It can be formed in a size
range from 4” (10.16cm) to 300” (762cm) diameter and in thickness up to 11/2” (13.97cm)
thick. Thus, ASEM coded tori-spherical head is more suitable.

7.3.1 Thickness and height calculation of top head


This section contains the calculation of thickness, height and other dimensions of the top
closure briefly.

7.3.1.1 Thickness of the tori-spherical head


The following equation is used to calculate the thickness of the ASEM coded tori-spherical
head.

𝑃𝐷𝑒𝑠𝑖𝑔𝑛 × 𝑅𝑐𝑟𝑜𝑤𝑛 × 0.885


𝑡𝑎𝑐𝑡𝑢𝑎𝑙 = +𝑐
𝜎𝑑𝑒𝑠𝑖𝑔𝑛 𝜑 − 0.1 × 𝑃𝑑𝑒𝑠𝑖𝑔𝑛

44
Here all symbols have their usual meanings. For the case of a tori-spherical head, crown radius
is the internal radius of the head which is equal to the outer diameter of the shell to which it is
fixed (𝑅𝑐𝑟𝑜𝑤𝑛 = 𝐷𝑜𝑢𝑡𝑒𝑟 ).

The knuckle radius of the head is equal to the 6% of the outer diameter( 𝑟𝑘𝑛𝑢𝑐𝑘𝑙𝑒 = 6% ×
𝐷𝑜𝑢𝑡𝑒𝑟 )
𝐷𝑜𝑢𝑡𝑒𝑟 = 𝐷𝑖 + 2𝑡𝑠ℎ𝑒𝑙𝑙
𝑅𝑐𝑟𝑜𝑤𝑛 = 𝐷𝑜𝑢𝑡𝑒𝑟 = 1.34 + 2 × 0.00798 = 1.356𝑚
6
𝑟𝑘𝑛𝑢𝑐𝑘𝑙𝑒 = 6% 𝐷𝑜𝑢𝑡𝑒𝑟 = × 1.356 = 0.081𝑚
100
The design thickness of a tori-spherical head is given by,

530.325 × 1.354 × 0.885


𝑡𝑎𝑐𝑡𝑢𝑎𝑙 = −3
+ 2.5 = 7.52𝑚𝑚
148 × 0.85 − 0.1 × 530.325 × 10
The actual thickness of the head  𝑡𝑎𝑐𝑡𝑢𝑎𝑙 = 7.52𝑚𝑚

However available thickness of the metal in market is 7.94mm (5/16 inch).

7.3.1.2 Checking for buckling condition


𝐷⁄ = 1.354⁄ 16925 𝑟⁄ = 0.081⁄
𝑡 = 94 = 180.053 𝐷 1.354 = 0.06
7.940 × 10−3
𝑃𝐷𝑒𝑠𝑖𝑔𝑛 530.325 × 10−3 −3
= ⁄
148 = 3.583 × 10
𝜎𝑑𝑒𝑠𝑖𝑔𝑛
2
𝑃𝐷𝑒𝑠𝑖𝑔𝑛 −3 𝑃𝐷𝑒𝑠𝑖𝑔𝑛
𝑙𝑛 ( ) = 𝑙𝑛 (3.583 × 10 ) = −6.664 (𝑙𝑛 ( )) = 44.406
𝜎𝑑𝑒𝑠𝑖𝑔𝑛 𝜎𝑑𝑒𝑠𝑖𝑔𝑛

Buckling can be checked by using the equation given below,

𝑡 2
𝑙𝑛 = −1.26177 − 4.55246 (𝑟⁄𝐷) + 28.93316 (𝑟⁄𝐷)
𝑅
2 𝑃𝐷𝑒𝑠𝑖𝑔𝑛
+ [0.66299 − 2.4709 (𝑟⁄𝐷) + 15.68299 (𝑟⁄𝐷) ] × 𝑙𝑛 ( )
𝜎𝑑𝑒𝑠𝑖𝑔𝑛
2
𝑃𝐷𝑒𝑠𝑖𝑔𝑛
2
+ [0.26879 × 10
−4
− 0.44262 (𝑟⁄𝐷) + 1.88783 (𝑟⁄𝐷) ] × (𝑙𝑛 ( ))
𝜎𝑑𝑒𝑠𝑖𝑔𝑛

𝑡
𝑙𝑛 = −1.26177 − 4.55246(0.06) + 28.93316(0.06)2
𝑅
+ [0.66299 − 2.4709(0.06) + 15.68299(0.06)2 ] × (−6.664)
−4
+ [0.26879 × 10 − 0.44262(0.06) + 1.88783(0.06)2 ] × 44.406

𝑡
𝑙𝑛 = −6.1135  𝑡⁄𝑅 = 2.21 × 10−3  𝑡 = 2.99 𝑚𝑚
𝑅
Hence a minimum thickness 2.99 mm is required to safe against buckling condition. The
calculated thickness is greater than that value. Thus,
45
The thickness of the top closure – 7.94 mm (5/16 inch).

Type -ASEM CODED TORI - SPHERICAL HEAD

7.3.2 Thickness and Height calculation of bottom closure


This section of the report contains the calculation of thickness, height and other dimensions of
the bottom closure briefly.

7.3.2.1 Thickness of the tori-spherical head


𝐷𝑜𝑢𝑡𝑒𝑟 = 𝐷𝑖 + 2𝑡𝑠ℎ𝑒𝑙𝑙
𝑅𝑐𝑟𝑜𝑤𝑛 = 𝐷𝑜𝑢𝑡𝑒𝑟 = 1.16 + 2 × 0.00798 = 1.176𝑚
6
𝑟𝑘𝑛𝑢𝑐𝑘𝑙𝑒 = 6% 𝐷𝑜𝑢𝑡𝑒𝑟 = × 1.176 = 0.071
100
The design thickness of a tori-spherical head is given by,

475.325 × 1.174 × 0.885


𝑡𝑎𝑐𝑡𝑢𝑎𝑙 = −3
+ 2.5 = 6.427 𝑚𝑚
148 × 0.85 − 0.1 × 475.325 × 10
The actual thickness of the head  𝑡𝑎𝑐𝑡𝑢𝑎𝑙 = 6.427 𝑚𝑚

However available thickness of the metal in market is 7.94 mm (5/16 inch)

7.3.2.2 Checking for buckling condition


𝐷⁄ = 1.174⁄ = 182.667 𝑟⁄ = 0.071⁄
𝑡 6.427 × 10−3 𝐷 1.176 = 0.06
𝑃𝐷𝑒𝑠𝑖𝑔𝑛 475.325 × 10−3 −3
= ⁄
148 = 3.212 × 10
𝜎𝑑𝑒𝑠𝑖𝑔𝑛
2
𝑃𝐷𝑒𝑠𝑖𝑔𝑛 −3 𝑃𝐷𝑒𝑠𝑖𝑔𝑛
𝑙𝑛 ( ) = 𝑙𝑛 (3.212 × 10 ) = −5.741 (𝑙𝑛 ( )) = 32.957
𝜎𝑑𝑒𝑠𝑖𝑔𝑛 𝜎𝑑𝑒𝑠𝑖𝑔𝑛

Buckling can be checked by using the equation given below,

𝑡 2
𝑙𝑛 = −1.26177 − 4.55246 (𝑟⁄𝐷) + 28.93316 (𝑟⁄𝐷)
𝑅
2 𝑃𝐷𝑒𝑠𝑖𝑔𝑛
+ [0.66299 − 2.4709 (𝑟⁄𝐷) + 15.68299 (𝑟⁄𝐷) ] × 𝑙𝑛 ( )
𝜎𝑑𝑒𝑠𝑖𝑔𝑛
2
2 𝑃𝐷𝑒𝑠𝑖𝑔𝑛
+ [0.26879 × 10
−4
− 0.44262 (𝑟⁄𝐷) + 1.88783 (𝑟⁄𝐷) ] × (𝑙𝑛 ( ))
𝜎𝑑𝑒𝑠𝑖𝑔𝑛

𝑡
𝑙𝑛 = −1.26177 − 4.55246(0.06) + 28.93316(0.06)2
𝑅
+ [0.66299 − 2.4709(0.06) + 15.68299(0.06)2 ] × (−5.741)
−4
+ [0.26879 × 10 − 0.44262(0.06) + 1.88783(0.06)2 ] × 32.957

𝑡
𝑙𝑛 = −5.360  𝑡⁄𝑅 = 4.699 × 10−3  𝑡 = 5.51 𝑚𝑚
𝑅

46
Hence a minimum thickness 5.51 mm is required to safe against buckling condition. The
calculated thickness is greater than that value. Thus,

The thickness of the bottom closure – 7.94 mm (5/16 inch)

Type -ASEM CODED TORI - SPHERICAL HEAD

7.4 Design of column reducer


Reducers (conical section) are used to make a gradual reduction in diameter from one
cylindrical section to another of smaller diameter. In here, reducer is designed to combine the
stripping section to the rectifying section, since the diameter of the two sections are different.

7.4.1 The thickness of the reducer


ASME Code Section VIII Division I provides the following equation for calculating the
thickness ‘t’ of conical heads subjected to an internal pressure with α as the semi-apex angle
of the cone.

Pdesign  D
t actual   corrosion allowance(c)
2 cos  design  0.6Pdesign .

Here all symbols have their usual meanings. The conical bottom is selected with an apex angle
of 250 .

530.325 ×1.348
𝑡𝑎𝑐𝑡𝑢𝑎𝑙 = + 2.5 = 5.64 mm
2×cos(25)×(148×0.85−0.6×530.325×10−3 )

Thickness of the reducer – 5.64 mm

However available thickness of the metal in market is 6.35 mm (1/4 inch)

7.4.2 Checking for reinforcement


However, it should be inspected whether additional reinforcement is required or not at the cone-
cylindrical shell junction. For that, the following procedure is followed as mentioned in Section
VIII, ASME BPVC 2008.
𝑃 530.325
Calculate the value 𝜑×𝜎𝐷𝑒𝑠𝑖𝑔𝑛 = 0.85×148×10 3 = 4.215 × 10
−3
𝑑𝑒𝑠𝑖𝑔𝑛

Compare the value of the semi apex angle with the calculated value using the following table.
Table 28-Semi-Apex Angle

𝑃𝐷𝑒𝑠𝑖𝑔𝑛
𝜑 × 𝜎𝑑𝑒𝑠𝑖𝑔𝑛
1×10-3 2×10-3 3×10-3 4×10-3 5×10-3 6×10-3

∆ 13𝑜 18𝑜 22𝑜 25𝑜 28𝑜 31𝑜


47
By interpolation, ∆=26.78 is greater than the semi-apex angle. Therefore, an additional
reinforcement is not required.
1.348m
7.4.3 Height of the reducer
The diameter of the upper section of the reducer is
HReduce
1.348m and the lower diameter should be 1. 168 m.Thus, r
1.168m
a portion of the designed cone should be cut out. The
height of the reducer, 25o

1.348 1.168
− tan(25)
(HReducer) - [ tan(25) ⁄ ] = 0.193 𝑚
2
Figure 7-1-Cross section of the Reducer

7.5 Height of the Column


 Height of the rectifying section – 9.6 m
 Excess height for rectifying section – 0.3m
 Height of the stripping section – 4.2 m
 Excess height for stripping section – 0.8m
 Height of the reducer – 0.193m
 Height of the top closure – 0.678m Height of the bottom closure – 0.597m

𝐻𝐶𝑜𝑙𝑢𝑚𝑛 – 9.6 + 0.3 + 4.2 + 0.8 + 0.193 + 0.678 + 0.597 – 𝟏𝟔. 𝟑𝟕 𝒎

7.6 Design of Openings and Reinforcements


Openings of the distillation column should be constructed in the shells and heads for product
removal, raw material introduction, top and bottom pump around, man holes and etc.
Construction of openings degrades the strength of the shell. Thus, additional reinforcements
are needed to maintain the original strength. In this design, a total of four main openings are
designed for feed inlet, top vapor outlet, reflux inlet, bottom vapor inlet and bottom liquid
outlet. According to ASME BPVC 2008, all vessels over 36-in. (900 mm) inside diameter shall
have a manhole and a circular manhole shall be not less than 16 in. (400 mm). Thus, a man
hole is constructed according to the above specification.

7.6.1 Determination of size of the Column openings


The volumetric flow rates should be known to calculate the size of the openings. The following
table depicts the solution approach to that.

48
Table 29-Volumetric Flowrate Calculations

Volumetric flowrate
Stream Density(kg/m3) Mass Flow(kg/hr)
(m3/s)
Feed In 325.86 16007.65 0.0136
Reflux In 487.93 3852.8 0.0022
Vapor Out(Top) 9.50 13483.68 0.3943
Liquid Out(Bottom) 251.94 15587.98 0.0172
Vapor in(bottom) 10.90 9249.41 0.2357

Generally, openings are not exceeding the following specification according to ASME BPVC
2008.

 For vessels 60in. (1.5m) inside diameter and less - one half the vessel diameter, but
not to exceed 20in. (0.5m)
 For vessels over 60in. (1.5m) inside diameter - one third the vessel diameter, but not
to exceed 40in. (1m).

Here, all the diameters are less than 1.5m. Thus, diameters of the openings should not be
exceeding 0.5m. If the fluid has to be pumped through the pipe, the size should be selected to
give the least annual operating cost. According to Coulson & Richardson’s Chemical
Engineering Volume 6, typical pipe velocities which can be used to estimate pipe sizes, are
given in the table below.

Table 30-Typical pipe velocities

Parameter Velocity(m/s) ∆P kPa/m


Liquid, pumped (not viscous) 1-3 0.5
Liquid, gravity flow - 0.05
Vapor and Gases 15-30 0.02
High pressure steam, >8bar 30-60 -

The calculated theoretical diameters of openings, assuming all openings are circular in shape,
are shown in the following table.

49
Table 31- Calculation of Theoretical Diameters

Maximum Area of Theoretical


Volumetric
Density Mass Allowable the Diameter of
Stream flowrate
(kg/m3) Flow(kg/hr) velocity openings the
(m3/s) 2
(m/s) (m ) opening(inch)
Feed In 325.86 16007.7 0.0136 3 0.0045 2.9961

Reflux in 487.93 3852.8 0.0022 3 0.0007 1.2012

Vapor 5.0927
9.5 13483.7 0.3943 30 0.0099
Out(Top)
Liquid 3.3625
251.94 15588 0.0172 3 0.0057
Out(Bottom)
Vapor 3.9378
10.9 9249.41 0.2357 30 0.0059
in(bottom)

However, the pipes are selected based on the NPS for carbon steel pipes. The selected pipe
dimensions are listed in the following table

Table 32- Pipe Selection

Theoretical Nominal pipe Outer Diameter


Stream
Diameter (inch) diameter (inch) (mm)
Feed In 2.9961 3½ 101.60
Reflux in 1.2012 1½ 48.26
Vapor Out(Top) 5.0927 6 168.28
Liquid Out(Bottom) 3.3625 3½ 101.60
Vapor in(bottom) 3.9378 4 114.30

The suitable pipe schedules will be selected after the calculation of the theoretical wall
thickness of the nozzles. Man holes are generally situated in the lower portion of the vessel, or
in the top head, for accessibility. According to ASME BPVC 2008, a circular manhole shall be
not less than 16 in (400 mm) and all vessels over 36 in. (900 mm) inside diameter shall have a
manhole. Thus, the diameter of the man hole is assumed as 0.5m. In this column, two manholes
are fabricated in order to increase safety concerns, since Xylene is a lethal and toxic compound.
The protruded nozzle type is chosen for all the nozzles.

7.6.2 Thickness and Reinforcements for Openings


The opening for the feed inlet is situated in the rectifying section of the column.
OD – 101.60 mm, area available in weld is neglected and theoretical thickness for the nozzle
should be calculated using,

50
𝑷𝑫𝒆𝒔𝒊𝒈𝒏 × 𝑫𝑶𝑫
𝑡𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 = +𝑐
2 × 𝜑 × 𝝈𝑫𝒆𝒔𝒊𝒈𝒏 + 𝑷𝑫𝒆𝒔𝒊𝒈𝒏

530.325 × 0.10160
𝑡𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 = + 2.5 = 2.71𝑚𝑚
2 × 0.85 × 148 + 530.325 × 10−3
However, available thickness is 3.048mm which is schedule 10s/20.

Therefore, 𝑡𝑎𝑐𝑡𝑢𝑎𝑙 = 3.048𝑚𝑚

𝐴𝑟𝑒𝑎 𝑟𝑒𝑚𝑜𝑣𝑒𝑑 ∶ 𝐴1 = (𝑑 + 2𝑐) × (𝑡𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 + 𝑐)


In here, 𝑡𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 is the calculated theoretical thickness of the shell which is 7mm. Corrosion
allowance is 2.5mm for carbon steel.

𝐷𝑚𝑒𝑎𝑛 = 𝑂𝐷 − 𝑡𝑎𝑐𝑡𝑢𝑎𝑙 = 101.60 − 3.048 = 98.55𝑚𝑚

𝐴𝑟𝑒𝑎 𝑟𝑒𝑚𝑜𝑣𝑒𝑑 ∶ 𝐴1 = (𝑑 + 2𝑐) × (𝑡𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 + 𝑐) = (98.55 + 2 × 2.5) × (5.33)


= 551.93 𝑚𝑚2
𝐸𝑥𝑐𝑒𝑠𝑠 𝑎𝑟𝑒𝑎 𝑖𝑛 𝑡ℎ𝑒 𝑠ℎ𝑒𝑙𝑙 ∶ 𝐴3 = (𝑑 + 2𝑐) × (𝑡𝑎𝑐𝑡𝑢𝑎𝑙 − 𝑡𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 − 𝑐)
𝐴3 = (98.55 + 2 × 2.5) × (7.94 − 5.33) = 270.27 𝑚𝑚2
Now, we have to assume a proper height for the nozzle. Considering the external protrusion,
H1 as 10 cm.

The external boundary limit should be calculated using the following equation,

𝐻1 = √(𝑑 + 2𝑐) × (𝑡𝑛 − 𝑐) = √(98.55 + 2 × 2.5) × (3.048 − 2.5) = 7.53 𝑚𝑚


H actual   H boundary limit 

Therefore, H1 calculated should be used in the proceeding calculations(𝐻1 = 7.53𝑚𝑚)


𝐸𝑥𝑐𝑒𝑠𝑠 𝑎𝑟𝑒𝑎 𝑖𝑛 𝑡ℎ𝑒 𝑜𝑢𝑡𝑒𝑟 𝑛𝑜𝑧𝑧𝑙𝑒: 𝐴0 = 2𝐻1 × (𝑡𝑛 − 𝑡𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 − 𝑐)
𝐴0 = 2 × 7.53 × (3.048 − 2.71) = 5.09 𝑚𝑚2
Next, excess area available in the nozzle is calculated using the equation
𝐴𝑛𝑜𝑧𝑧𝑙𝑒 = 𝐴0 = 5.09 𝑚𝑚2
𝐴2 − 𝐴𝑟𝑒𝑎 𝑜𝑓 𝑡ℎ𝑒 𝑟𝑒𝑖𝑛𝑓𝑜𝑟𝑐𝑒𝑚𝑒𝑛𝑡 ∶ 𝐴2 = 𝐴1 − 𝐴3 − 𝐴𝑛𝑜𝑧𝑧𝑙𝑒
𝐴𝑟𝑒𝑎 𝑜𝑓 𝑡ℎ𝑒 𝑟𝑒𝑖𝑛𝑓𝑜𝑟𝑐𝑒𝑚𝑒𝑛𝑡 ∶ 𝐴2
= 551.93 − 270.27 − 5.04
= 276.62 𝑚𝑚2
This area is supplied in terms of a welded
plate,
Select 𝑑𝑟 = 2 × 𝑑ℎ Figure 7-2-Welded Pad

51
𝑑𝑟 = 2 × (𝑂𝐷 − 2𝑡𝑛 ) = 2 × (101.60 − 2 × 3.048) =191.01mm

The thickness of the reinforcement : 𝑡𝑟 = 𝐴2⁄𝑑 − 𝑑 = 276.62⁄191.01 − 96.50 = 2.88 𝑚𝑚


𝑟 ℎ

Thickness of reinforcement =𝟑. 𝟗𝟏𝒎𝒎


In the same way, thickness and the schedule of openings can be calculated as follows.
Table 33-Thickness and Schedule of openings

Nominal pipe
Stream Pdesign Dod(m) Ttheoritical Tactual Schedule
diameter (inch)
Feed In 3½ 530.325 0.1016 2.714 3.048 10s/20
Reflux in 1½ 530.325 0.04826 2.602 2.769 10s/20
Vapor Out(Top) 6 530.325 0.16828 2.854 3.404 10s/10
Liquid
3½ 475.325 0.1016 2.692 3.048 10s/20
Out(Bottom)
Vapor in(bottom) 4 475.325 0.1143 2.716 3.048 10s/20
Man hole(Top) 18 530.325 0.4572 3.462 4.191 5s
Man
18 475.325 0.4572 3.362 4.191 5s
hole(Bottom)
In the same way, reinforcement area of the openings can be calculated as follows. The external
protrusion H1 is considered as 10 cm.

Table 34-Reinforcement Area Calculation

Shell and Heads Area


Excess Excess area Area of the
Dmean removed
Stream TTheor area in nozzle- reinforcement
(mm) Tactual from shell
A3(mm2) A0(mm2) -(mm2)
etical
(mm) (mm2)
(mm)
Feed In 98.55 5.33 7.94 551.93 270.27 5.0 276.62

Reflux in 45.49 5.33 7.94 269.12 131.78 1.2 136.10


Vapor Out
164.8 7.52 7.94 1277.47 71.35 11.0 1195.12
(Top)
Liquid Out
98.55 6.427 7.94 665.53 156.67 5.4 503.48
(Bottom)
Vapor in
111.2 4.7 7.94 546.38 376.66 5.3 164.42
(bottom)
Man
453.0 7.52 7.94 3444.23 192.36 40.6 3211.27
hole(Top)
Man hole
453.0 4.7 7.94 2152.64 1483.95 46.1 622.56
(Bottom)

Following same way, the thickness of the welded pad can be calculated as follows.

52
Table 35-Reinforcement Thickness Calculation

Reinforcement
Area of the
Stream Di(mm) dr Thickness-
reinforcement
tr (mm)
Feed In 276.62 2.88
96.05 192.10
Reflux in 136.10 3.17
42.99 85.98
Vapor Out(Top) 1195.12 7.36
162.38 324.75
Liquid Out(Bottom) 503.48 5.24
96.05 192.10
Vapor in(bottom) 164.42 1.51
108.75 217.50
Man hole(Top) 3211.27 7.13
450.51 901.02
Man hole(Bottom) 622.56 1.38
450.51 901.02

Three main closures have been designed in the tori spherical head for vapor outlet, as a
manhole and reflux inlet. The diameter of the man hole is higher than the diameter of the vapor
outlet. Since, too much opening may cause the head become weak, only the man hole and reflux
inlet are constructed in the head. When the column is operating, vapor outlet can be prepared
through the manhole opening by using flange to reduce diameter up to the required value.

7.7 Design of Insulation


When determining the insulation thickness required, the worst case scenario is considered.
Ambient temperature is assumed as 30℃ and maximum temperature in the column is 258℃.
So, the maximum temperature difference occurring at the worst condition is 228℃. According
to NORSOK standard, vessels of diameter 1.5m and smaller shall be insulated as piping.

Glass mineral wool is chosen as the insulation material, because higher thermal insulation
efficiency can be achieved with lighter weight (Anon., n.d.). Glass wool is non-combustible
and has the highest possible A1 fire classification according to European standards. Also, it can
be operated within -200 to 450℃.

The conductivity of glass wool is 0.065 W/m.K and density is 16 kg/m3 (Anon., 2001).
Conductivity of SA-299 at this operating conditions is found as 48 W/m.K (Gandy, 2007).
Convective heat transfer coefficient of air - 10 W/m2. K

The following parameters are calculated by using Aspen Plus Simulation. It is assumed that
the column is filled with vapor with the composition of feed input.

53
Pradtl Number(Pr) – 0.697494 Reynolds Number(Re) – 316879
Thermal conductivity(k) -0.0293 W/m. K
Nusselt number can be calculated by using Dittus-Bolter equation,
𝑁𝑢 = 0.023 × 𝑅𝑒 0.8 × 𝑃𝑟 0.4 = 0.023 × 3168790.8 × 0.6974940.4 = 501.024

𝑁𝑢 = ℎ × 1.34⁄0.0293 = 501.024

The heat transfers through the liquid mixture in the column: ℎ = 10.96 W/m2 . K
Overall heat transfer co-efficient based on the internal surface without insulation is calculated
using the following equation.

𝑟
1 1 ln( 2⁄𝑟1 ) 1 𝑟
= + 𝑟2 × + × 2⁄𝑟1
𝑈𝑢𝑛𝑖𝑛𝑠𝑢𝑙𝑎𝑡𝑒𝑑 ℎ1 𝑘𝑠 ℎ𝑎

Where 𝑟1 is the internal radius and 𝑟2 is the external radius of the shell.
𝑟1 = 1.34𝑚 𝑟2 = 1.357𝑚
1 1 ln(1.358⁄1.34) 1
= 10.96 + 1.358 × + 10 × 1.358⁄1.34
𝑈 48

Overall heat transfer coefficient; 𝑈𝑢𝑛𝑖𝑛𝑠𝑢𝑙𝑎𝑡𝑒𝑑 = 10.956 W/m2 . K


Applying heat transfer rate for a unit length of the shell
𝑄𝑈𝑛𝑖𝑛𝑠𝑢𝑙𝑎𝑡𝑒𝑑 = 𝑈 × 2𝜋𝑟2 Δ𝑇 = 10.956 × 2 × 3.14 × 1.358 × 228 = 21300 𝑊
Assuming that by applying insulation, heat loss can be prevented by 95%,

𝑄𝑖𝑛𝑠𝑢𝑙𝑎𝑡𝑒𝑑 = 21300 × 0.05 = 1065 𝑊 𝑈𝑖𝑛𝑠𝑢𝑙𝑎𝑡𝑒𝑑 = 1065⁄2 × 3.14 × 𝑟 × 228


2
𝑟 𝑟
1 1 ln( 2⁄𝑟1 ) ln( 3⁄𝑟2 ) 1 𝑟
= + 𝑟3 × + 𝑟3 × + × 3⁄𝑟1
𝑈𝐼𝑛𝑠𝑢𝑙𝑎𝑡𝑒𝑑 ℎ1 𝑘𝑠 𝑘𝑠 ℎ𝑎
𝑟
2 × 3.14 × 𝑟3 × 228 1 ln(1.358⁄1.34) ln( 3⁄1.358) 1 𝑟
= + 𝑟3 × + 𝑟3 × + × 3⁄1.34
106.5 10 48 0.065 10.96

𝑟3 = 1.4678
The insulation thickness: 𝑡𝑖𝑛𝑠𝑢𝑙𝑎𝑡𝑖𝑜𝑛 = 1.468 − 1.357 =0.111m =11.1 cm
However, the available glass wool thickness is - 12.7 cm (5 inch.)

7.8 Combined loading calculations


Distillation columns should be designed to withstand not only stresses due to pressure, but also
additional stresses exerted by dead weight, wind load, seismic activity and eccentric loads on
the vessel. A vessel must be designed for the worst case of wind or seismic loads, but need not
to be designed for both simultaneously. However, wind is the worst case in Sri Lanka. In this

54
chapter, calculations are carried out to inspect the stability of the o-xylene column for combined
loadings.

7.8.1 Stresses due to pressure


The longitudinal and circumferential stresses due to internal pressure is given by the following
equations.

𝑃𝐷𝑖 𝑃𝐷𝑖
𝜎ℎ = 𝜎𝐿 =
2𝑡 4𝑡

Here, maximum longitudinal and circumferential stresses are to be calculated. Thus, maximum
diameter is selected as the column internal diameter. Also,

Circumferential stress of the design column:

530.325 × 103 × 1.34


𝜎ℎ = = 44.75 𝑀𝑃𝑎
2 × 0.00794

530.325 × 103 × 1.34


𝜎𝐿 = = 22.375 𝑀𝑃𝑎
4 × 0.00794

Both circumferential and longitudinal stresses are way below the design stress.

7.8.2 Load due to weights of the column


Weight of the designed distillation column depends on the weight of mechanical parts, weight
of working volume mixture and the weight of insulations. The load of those weights are
calculated here.

7.8.2.1 Weight of mechanical parts


𝑘𝑔⁄
The density of the carbon steel(SA-299) is normally 7850 𝑚3 . (Gandy, 2007)
Volume can be calculated by using following equation,
2 2
𝑆ℎ𝑒𝑙𝑙 𝑉𝑜𝑙𝑢𝑚𝑒 = 2𝜋𝑙(𝐷𝑂𝐷 − 𝐷𝐼𝑛 ) × 0.25
3 3
𝑇𝑜𝑟𝑖𝑠𝑝ℎ𝑒𝑟𝑖𝑐𝑎𝑙 𝐻𝑒𝑎𝑑 𝑉𝑜𝑙𝑢𝑚𝑒 = (0.0847 × 𝐷𝐼𝐷 ) + (𝜋 × 𝐷𝐼𝐷 × 𝐻𝑓𝑙𝑎𝑛𝑔𝑒𝑑 ) (Anon., 2015)

𝑅𝑒𝑑𝑢𝑐𝑒𝑟 𝑉𝑜𝑙𝑢𝑚𝑒 = 𝜋ℎ⁄3 (𝑅𝐵𝐷


2
+ 𝑅𝐵𝐷 × 𝑟𝑇𝐷 + 𝑟𝑇𝐷 2 )

Where all symbols have their usual meanings.


Weight of the column can be calculated as follows.

55
Table 36-Column Weight Calculation

Section Volume(m3) Density(kg/m3) Weight(kg)


Rectifying Section 0.3563 7850 2797.08
Stripping Section 0.1283 7850 1006.79
Top Head 0.8383 7850 6580.66
Bottom Head 0.5507 7850 4323.00
Reducer 0.0474 7850 371.84
Plates 0.1975 7850 1550.19
Total weight 16629.54

7.8.2.2 Weight of the working volume mixture


It is assumed that the bottom closure is filled with liquid and the weight of the liquid in plates
can be neglected, compared to the weight of the column.

2𝜋𝑟 3
𝑇ℎ𝑒 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑏𝑜𝑡𝑡𝑜𝑚 𝑐𝑙𝑜𝑠𝑢𝑟𝑒 –
3

The maximum density of the mixture – 487 kg/m3

Weight of the liquid inside the column - 342.94 kg


7.8.2.3 Weight of the insulations
The density of glass wool is 16 kg/m3.
𝑇ℎ𝑒 𝑠𝑢𝑟𝑓𝑎𝑐𝑒 𝑎𝑟𝑒𝑎 𝑜𝑓 𝑡ℎ𝑒 𝑐𝑜𝑙𝑢𝑚𝑛 (𝐴𝑠 )– 𝐴𝑟𝑒𝑎 𝑜𝑓 𝑡ℎ𝑒 𝑠ℎ𝑒𝑙𝑙𝑠 𝑎𝑛𝑑 ℎ𝑒𝑎𝑑 + 𝑟𝑒𝑑𝑢𝑐𝑒𝑟
2 2
𝐷𝑡𝑜𝑝 𝑐𝑙𝑜𝑠𝑢𝑟𝑒 + 𝐷𝐵𝑜𝑡𝑡𝑜𝑚 𝑐𝑙𝑜𝑠𝑢𝑟𝑒 (𝐷𝑡𝑜𝑝−𝑠ℎ𝑒𝑙𝑙 + 𝐷𝑏𝑜𝑡𝑡𝑜𝑚−𝑠ℎ𝑒𝑙𝑙 ) (𝐷𝑡𝑜𝑝−𝑠ℎ𝑒𝑙𝑙 − 𝐷𝑏𝑜𝑡𝑡𝑜𝑚−𝑠ℎ𝑒𝑙𝑙 )2
(𝐴𝑠 ) = 𝜋 [ℎ𝐷𝑡𝑜𝑝−𝑠ℎ𝑒𝑙𝑙 + ℎ𝐷𝑏𝑜𝑡𝑡𝑜𝑚−𝑠ℎ𝑒𝑙𝑙 + + √ + ℎ2𝑟𝑒𝑑𝑢𝑐𝑒𝑟 ]
2 2 4

1.3562 + 1.1762 (1.356 + 1.176) (1.356 − 1.176)2


(𝐴𝑠 ) = 𝜋 [9.9 × 9.356 + 5.0 × 1.176 + + √ + 0.1932 ] = 𝟏𝟎𝟎. 𝟔𝟐 𝒎𝟐
2 2 4

𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑖𝑛𝑠𝑢𝑙𝑎𝑡𝑖𝑜𝑛 = 100 × 0.127 = 12.7 𝑚3


Weight of the insulation – 203.2 kg
7.8.2.4 Dead weight and load of the column
𝐷𝑒𝑎𝑑 𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑡ℎ𝑒 𝑐𝑜𝑙𝑢𝑚𝑛 – 16629.54 + 324.94 + 203.2 = 𝟏𝟕𝟏𝟓𝟕. 𝟔𝟖 𝒌𝒈
𝑊𝑒𝑖𝑔ℎ𝑡 𝑙𝑜𝑎𝑑 = 17157.68 × 9.81 = 𝟏𝟔𝟖. 𝟑 𝒌𝑵
Compressive stress due to total dead weight is given by the following equation,
𝑊 168.3 × 103
𝜎𝐷𝑒𝑎𝑑 𝑤𝑒𝑖𝑔ℎ𝑡 = = = 𝟓. 𝟕𝟕 𝑴𝑷𝒂
𝜋(𝐷𝑖 + 𝑡) × 𝑡 𝜋(1160 + 7.94) × 7.94

56
7.8.3 Load due to wind
Total force due to wind load depends on wind pressure. Wind pressure depends on wind
velocity. The height of the column is about 16m which is lower than 20m. The plant is located
in the coastal area. Therefore, wind pressure is assumed as 1.0 kN/m2. The height of the skirt
is obtained as 3m.

Load due to wind, P1 wind  k1  k2  p1  h1  Do k1and k 2  coefficien ts

𝑇 = 6.35 × 10−5 × ( 𝐻/𝐷0 )3/2 (𝑊/𝑡)1/2

𝑇 = 6.35 × 10−5 × ( 16/1.16)3/2 (4503553/0.007)1/2 = 9.27 𝑠 > 0.5

𝑃1,𝑤𝑖𝑛𝑑 = 0.7 × 2 × 1 × 16.525 × 1.176 = 27.20 𝑘𝑁

H
M wind  Pwind  where H  20 m
2
16.37 + 3
𝑀𝑤𝑖𝑛𝑑 = 27.20 × = 265.54 𝑘𝑁𝑚
2
Compressive stress due to wind is given by the following equation,
4𝑀𝑤𝑖𝑛𝑑 265.54 × 103
𝜎𝑊𝑖𝑛𝑑 = = = 7.86𝑀𝑃𝑎
𝜋𝐷𝑠𝑜 (𝐷𝑠𝑜 + 𝑡𝑠ℎ𝑒𝑙𝑙 ) × 𝑡𝑠ℎ𝑒𝑙𝑙 𝜋1160 × (1160 + 7.94) × 7.94

7.8.4 Calculation of principle stresses


Resultant axial stress of the column can be calculated by using the following equation,
𝜎𝑎𝑥𝑖𝑎𝑙 = 𝜎𝑃𝑟𝑒𝑠𝑠𝑢𝑟𝑒 − 𝜎𝐷𝑒𝑎𝑑 𝑤𝑒𝑖𝑔ℎ𝑡 ± 𝜎𝑤𝑖𝑛𝑑 (Negative sign due to downwind case)

For downwind side,


𝜎𝑎𝑥𝑖𝑎𝑙 = 𝜎𝑃𝑟𝑒𝑠𝑠𝑢𝑟𝑒 − 𝜎𝐷𝑒𝑎𝑑 𝑤𝑒𝑖𝑔ℎ𝑡 − 𝜎𝑤𝑖𝑛𝑑

𝝈𝒂𝒙𝒊𝒂𝒍,𝑫𝒐𝒘𝒏 𝒘𝒊𝒏𝒅 = 𝟐𝟐. 𝟑𝟕𝟓 − 𝟓. 𝟕𝟕 − 𝟕. 𝟖𝟔 = 𝟖. 𝟕𝟒𝟓 𝑴𝑷𝒂

For upwind side,


𝜎𝑎𝑥𝑖𝑎𝑙,𝑈𝑝𝑤𝑖𝑛𝑑 = 𝜎𝑃𝑟𝑒𝑠𝑠𝑢𝑟𝑒 − 𝜎𝐷𝑒𝑎𝑑 𝑤𝑒𝑖𝑔ℎ𝑡 + 𝜎𝑤𝑖𝑛𝑑

𝜎𝑎𝑥𝑖𝑎𝑙,𝑈𝑝𝑤𝑖𝑛𝑑 = 𝟐𝟐. 𝟑𝟕𝟓 − 𝟓. 𝟕𝟕 + 𝟕. 𝟖𝟔 = 𝟐𝟒. 𝟒𝟔𝟓 𝑴𝑷𝒂

Hoop stress of the column, is the circumferential pressure due to pressure.


𝜎ℎ𝑜𝑜𝑝 = 44.75 𝑀𝑃𝑎

Now, the three principle stresses should be found out for upwind and downwind side by using
following equations.

1 2
𝜎1 = 2 × [𝜎𝑎𝑥𝑖𝑎𝑙 + 𝜎ℎ𝑜𝑜𝑝 + √(𝜎𝑎𝑥𝑖𝑎𝑙 − 𝜎ℎ𝑜𝑜𝑝 ) + 4𝜏 2 ]

57
1 2
𝜎2 = × [𝜎𝑎𝑥𝑖𝑎𝑙 + 𝜎ℎ𝑜𝑜𝑝 − √(𝜎𝑎𝑥𝑖𝑎𝑙 − 𝜎ℎ𝑜𝑜𝑝 ) + 4𝜏 2 ]
2
1
𝜎3 = ×𝑝
2
Stress intensity distribution can be found out as follows.
Table 37-Stress intensity Values

Upwind side Downwind side


(σ1 - σ2) 20.29 (σ1 - σ2) 36.01
(σ1 – σ3) 44.22 (σ1 – σ3) 44.22
(σ2 – σ3) 23.94 (σ2 – σ3) 8.22

All the stress intensities are much lower than the design stress of SA-299 in this case which
is 148 MPa.
Therefore, the calculated thickness in previous sections is stable against combined loading.

58
7.9 Design of supports
Any vessel needs a support and the supporting members shall be arranged and /or attached to
the vessel wall in such a way as to safely withstand any kind of loadings. Different kinds of
supports are available for different types of vessels; saddle support, leg support, lug support
and skirt support. Normally, skirt support is used for tall vertical columns. It is a cylindrical
shell section that is welded either to the lower portion of the vessel shell or to the bottom head.

7.9.1 Determination of skirt wall thickness


Load on skirt depend on,
1. Internal or external pressure
2. Weight of fully equipped vessel with content
3. Wind or seismic load
As a first trial, take the skirt thickness as the same as that of the bottom section of the vessel,
7.9375 mm.

Load on skirt due to dead weight can be calculated by the following equation, where all
symbols have their usual meanings.
𝑊 168.3 × 103
𝜎𝑊𝑆 = = = 5.78 𝑁⁄𝑚𝑚2
𝜋(𝐷𝑠𝑜 + 𝑡𝑠 ) × 𝑡𝑠 3.14 × (1160 + 7.9375) × 7.9375
Load due to wind can be calculated by the following equation.
4𝑀𝑤𝑖𝑛𝑑
𝜎𝑏𝑠 = ±
𝜋(𝐷𝑠𝑜 + 𝑡𝑠 )𝐷𝑠𝑜 × 𝑡𝑠
4 × 265.54 × 103 × 103
𝜎𝑏𝑠 = ± = ±31.46𝑀𝑃𝑎
3.14 × (1160 + 7.9375) × 1160 × 7.9375
7.9.1.1 Skirt thickness calculation
Maximum compressive and tensile stresses can be calculated as follows
4𝑀𝑤𝑖𝑛𝑑
−𝜎𝑐𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒 =
𝜋(𝐷𝑠𝑜 + 𝑡𝑠 )𝐷𝑠𝑜 × 𝑡𝑠
𝑊
+
𝜋(𝐷𝑠𝑜 + 𝑡𝑠 )𝑡𝑠
−𝜎𝑐𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒 = 31.46 + 5.78 = 37.24 𝑀𝑃𝑎 t -skirt
4𝑀𝑤𝑖𝑛𝑑 𝑊
−𝜎𝑡𝑒𝑛𝑠𝑖𝑙𝑒 = 2

𝜋 × 𝐷𝑠𝑜 × 𝑡𝑠 𝜋(𝐷𝑠𝑜 + 𝑡𝑠 )𝑡𝑠
−𝜎𝑡𝑒𝑛𝑠𝑖𝑙𝑒 = 31.46 − 5.78 = 26.68 𝑀𝑃𝑎

Figure 7-3-Skirt Support

59
If 𝜎𝑡𝑒𝑛𝑠𝑖𝑙𝑒 < 𝜎𝑑𝑒𝑠𝑖𝑔𝑛 𝜑 then the used thickness is okay for the skirt.

Taking 𝜑 = 0.85 for a welded steel plate ,


𝜎𝑑𝑒𝑠𝑖𝑔𝑛 𝜑 = 148 × 0.85 = 125.8 𝑀𝑃𝑎

t 
Allowable compressive stress :  compressive  0.125E   sin 
D
Young's modulus of carbon steel is normally 200 GPa (29,000,000 psi).

𝜎𝑐𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒 < 0.125 × 200000 × 7.9375⁄1160 37.24 < 171.06 𝑀𝑃𝑎

Therefore, assumed theoretical thickness of the skirt (7.9375𝑚𝑚) is acceptable.


7.9.2 Design of Bearing plate and Bolt
The loads carried by the skirt are transmitted to the foundation slab by the skirt bearing plate
(base ring). There are three types of bearing plates namely, double ring stiffened by gussets,
rolled angle and plain flange ring. Commonly, rolled angle and plain flange ring are used for
small vessels.

Therefore, doubled ring stiffened by gussets is designed for the skirt of the distillation column.
The procedure in the book of chemical engineering and design is used for this design.

Assume that the skirt support height is 3m.

Take the skirt bottom dia. as 1.7 m,

3
𝑆𝑘𝑖𝑟𝑡 𝑏𝑎𝑠𝑒 𝑎𝑛𝑔𝑙𝑒 = 𝑡𝑎𝑛−1 ( ) = 84.850
1
(1.7 − 1.16)
2
Highest stresses will occur at the top of the skirt; where the values will be close to those
calculated for the cylindrical skirt. Sin 80.9= 0.987, so this term has a little effect on the design
criteria.

Scheiman gives the following guide rules that can be used for the selection of the anchor bolts:

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


 Minimum number of bolts 8.
 Use multiples of 4 bolts.
 Bolt pitch should not be less than 600 mm (2ft).
It is assumed that the number of bolts is 8.
The bolt area required is given by following equation;

60
1 4𝑀𝑠
𝐴𝑏 = [ − 𝑊]
𝑁𝑏 × 𝑓𝑏 𝐷𝑏
Where
Ab - area of one bolt at the root of the thread, mm2
Nb - Number of bolts,
fb - Maximum allowable bolt stress; typical design value 125 N/mm2 (18,000 psi),
Ms - Bending (overturning) moment at the base(Nm)
W- Weight of the vessel, N,
Db - Bolt circle diameter, m.

16.525+3
Bending moment at base of skirt; 𝑀𝑤𝑖𝑛𝑑 = 27.20 × = 265.54 𝑘𝑁𝑚
2

1 4𝑀𝑠 1 4 × 265.54 × 103


𝐴𝑏 = [ − 𝑊] = [ − 168.3 × 103 ] = 456.5 𝑚𝑚2
𝑁𝑏 × 𝑓𝑏 𝐷𝑏 8 × 125 1.7
M30 bolts (BS 4190:1967) root area= 2030 mm2 is selected for the design.

For safe design of the bearing plate, 𝜎𝑑𝑒𝑠𝑖𝑔𝑛 < 𝜎𝑓𝑜𝑢𝑛𝑑𝑎𝑡𝑖𝑜𝑛

4𝑀𝑤𝑖𝑛𝑑 𝑊
𝜎𝑐𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒 = 2 ×𝐿 + 𝜋𝐷 , Where all symbols have usual meanings.
𝜋×𝐷𝑠𝑜 𝑠 𝑠𝑜 𝐿𝑠

𝜎𝑓𝑜𝑢𝑛𝑑𝑎𝑡𝑖𝑜𝑛 is taken as 5 MPa which is a common value.

4𝑀𝑤𝑖𝑛𝑑 𝑊 4 × 265.54 × 103 168.3 × 103


5 × 103 𝐿𝑏 = 2
+ = + −→ 𝐿𝑠 = 29.64 𝑚𝑚
𝜋 × 𝐷𝑠𝑜 𝜋𝐷𝑠𝑜 3.14 × 1.72 3.14 × 1.7

However, actual length of bearing plate is 76mm;

𝑨𝒄𝒕𝒖𝒂𝒍 𝒘𝒊𝒅𝒕𝒉 𝐛𝐞𝐚𝐫𝐢𝐧𝐠 𝐩𝐥𝐚𝐭𝐞

𝑳𝒂𝒄𝒕𝒖𝒂𝒍 + 𝒕𝒔 + 𝟓𝟎 𝒎𝒎 = 𝟕𝟔 + 𝟕. 𝟗𝟑𝟕𝟓 + 𝟓𝟎 = 𝟏𝟑𝟑. 𝟗𝟑𝟕𝟓 𝒎𝒎

Actual bearing pressure on concrete foundation:

148.2 × 103
𝑓𝑐′ = = 1.10 𝑁/𝑚𝑚2
210 × 103

61
7.10 Description of Fabrication
Carbon steel type SA-299 is used for the fabrication of the main components of the o-xylene
distillation column. The insulation of the column is done by using glass mineral wool.
Considering the thicknesses of carbon steel SA-299 metal plates available in the market and
the requirements in the vessel, it is decided to use 6.35mm thick plates for reducer and 7.94
mm thick plates for the shell and heads. The ends, reducers and two part of shell will have to
be fabricated separately and then welded together.

Fabrication process of column consists of several steps and cutting, crimping, rolling and
welding are the main steps of fabricating shells and reducer. Modern methods for cutting are
based either on CNC (computer numerical control) laser cutting or multi tool CNC punch
pressing. Crimping is the next step after cutting the plate which sets the correct radius on the
ends of the plates. Crimping eliminates the waste of excess material. So, Crimping is a crucial
step prior to rolling. Then the plates are heated. Heated plates are rolled to the proper radius
using rollers. It is preferable if the diameter of the rolled sheets is measured and verified to be
correct before going for welding. In the welding steps, rolled plates can be welded using the
common fusion and resistance techniques, however special care should be taken to prevent
“hot cracking”. Double V grooved butt joint which is a category A type weld, is used for
welding of shells and reducers.

The top and bottom hemispherical closures are formed by forging and heat treatment of the
carbon steel plates. First, the plates are subjected to bumping to form the head dish by hydraulic
press and pressing dish. Next the plate is spanned to form knuckle section by flanging machine.
After some further treatments are done according to the requirement, closures, shells and
reducer are assembled and welded using category B, double V grooved butt joint. The skirt
support of the vessel is attached bottom closure by using a single full fillet lap joint with plug
weld. All nozzles are welded to the main shell using category D fillet welds.

62
7.11 Mechanical Drawings
Table 38-List of Drawings

Description Drawing Number


Detail Drawing - Top closure 01
Detail Drawing – Bottom Enclosure 02
Detail Drawing – Skirt Support 03
Detail Drawing - Shell and Reducer 04
Production Drawing – Distillation Column 05
Detail Drawing – Sieve Plate 06

63
CHAPTER 8 - CONTROL, PIPING, INSTRUMENTATION &
OTHER ASPECTS
In this chapter, selection of suitable pipes, valves, pumps and other instruments are done for
the designed distillation column.

8.1 Selection of Pipes


Normally, Pipes are used to convey liquids and gases (vapor). Pipes are generally specified by
nominal diameter and wall thickness. The material to be used to design the pipes is depending
on the requirement of the pipe. In here, Pipes are required for following purposes.

 Transportation of feed in to distillation column


 Transportation of top vapor in to condenser and condenser drum
 Transportation of portion of condensed liquid back to column as reflux
 Transportation of remaining condensed liquid as the top product
 Transportation of bottom liquid to reboiler and reboiled vapor in to the column
 Transportation of bottom liquid as the bottom product
However, carbon steel SA-299 is used to manufacture pipe lines. Pipe lines are designed based
on the maximum allowable velocities and corrosion. Further, the size and thickness of the pipes
are selected based on nominal standard pipe diameters and thickness. The designed pipe
diameters are shown in the Table 01.

Table 39-Designed Pipe Diameters

Theoretical Nominal pipe Outer Diameter


Stream
Diameter (inch) diameter (inch) (mm)
Feed In 2.9961 3½ 101.60
Reflux in 1.2012 1½ 48.26
Vapor Out(Top) 5.0927 6 168.28
Liquid Out(Bottom) 3.3625 3½ 101.60
Vapor in(bottom) 3.9378 4 114.30

8.2 Selection of Valves


Industrial valves are devices that regulate, control or direct the flow of any liquid/vapor
medium passing through it. Their functions include automatic control of valve position, safety,
diagnosis and process control. Since this distillation column is related to petrochemical
industry, it is very important to pay attention on the safety as well as control.
64
In petro chemical industry, various types of valves are used; shut-off valves, flow control
valves, pressure control valves and non-return valves. The requirements of valves for the
distillation column are as follows,

 Shut off valves for overhead condenser in/out


 Shut off valves for reflux pump in/out
 Shut off valves for bottom pumps in/out
 Shut off valve for drain line of reflux drum
 Pressure relief valve for vent line in top of column.
 Pressure relief valve for reflux drum
 Shut off valves of trim cooler and reboiler
 Control valve for reflux in and top product out
 Control valve for trim cooler cooling water in
 Control valve for bottom product out
 Control valve for fuel in of the furnace
 Control valve for reboiler steam in

8.2.1 Selection of shut off valve


A valve used for shut offing a fluid line should be able to give a positive seal in the closed
position. At their opening condition, a minimum resistance to flow should be maintained.
Normally, gate, plug and ball valves are used as shutoff valves. Among them, plug valves can
be used for a wide range of applications including high temperature/pressure operations and
hazardous processes. Plug valve is shaped like a cylinder or cone that can be rotated inside
valve body. Typically, eccentric plug valve is used for transfer petrochemical materials and
thus that type is used as the shut off valve in this design.

Figure 8-1-Side View of an Eccentric Plug Valve(Partially open)

65
8.2.2 Selection of pressure relief valve
Pressure relief valves are used for ensuring the safety of the equipment against internal over
pressure. In here, pressure relief valve is designed for the distillation column to maintain its top
pressure below safety level. Pressure relief valves are available in two general types: spring
operated type and rupture device. Again spring operated type is categorized in to two;
conventional and balanced bellow type. Conventional type is widely used when handling
hazardous material because it doesn’t release those material to atmosphere. Since xylene is
toxic and combustible gas, API 520 type spring conventional type is selected as the pressure
relief valve.

Figure 8-2-API 520-Conventional


safety relief valve

8.2.3 Selection of flow control valve


Flow-control valves are used to control the rate of flow of a fluid through a pipe line. Those
valves should be capable of giving smooth control over the full range of flow, from fully open
to closed.

Most widely used flow control valves are globe valve and butterfly. Normally, butterfly valve
is used to control gas and vapor. Automatic control valves are basically globe valves with
special trim designing. Therefore, globe valve is selected as liquid flow controller and butterfly
valves are selected as steam and vapor flow controller in this system. Tea pattern globe valves
are the most common body type and wafer style butter fly valves are also commonly used.

Normally, compressed air is used as a medium to control valves in petrochemical plants


because electrical signal may cause hazards. Thus, pneumatic control valves are selected for
automatic control valves.

66
Figure 8-4-Wafer Type Butterfly Valve Figure 8-3-Tee Pattern Globe Valve

8.3 Selection of pumps and strainers


Distillation column operates as an internal pressure vessel. The pressure inside the column is
maintained by vaporizing a fraction of the bottom product using a furnace. As a result, no
pumping is required to maintain the pressure inside column.

Normally, centrifugal pumps are required to pump reflux back to the distillation column. Also,
Pumping is used to transfer the bottom product to A9 column, as well as to maintain the pressure
inside the column. Y strainers are required for each pump to remove unwanted solids from
liquid. Typically, mesh inside the y-strainer is cleaned manually in the maintenance. In
petrochemical industry, carbon steel y-strainers are used because they have excellent resistance
to mechanical or thermal shock. It can also be used for higher pressure applications because of
their great strength (pagina, 2016). Therefore, carbon steel y strainers are selected.

Figure 8-5-Carbon steel Y strainer

67
8.4 Instrumentation
Different types of instruments are required to maintain the operation of distillation column
properly. In petrochemical industry, it is very crucial to obtain an accurate and reliable
measurements, because it needs to maximize the production rate while maintaining the safety
level. Also, issues in distillation process could lead to costly shutdowns. Some of common
parameters measured in a distillation system are given below.

 Temperature
 Pressure
 Liquid level
 Flow rates

8.4.1 Pressure measurement


Distillation columns are normally operated with a differential pressure at top and bottom. This
difference of the pressure is caused by the flow of vapor in the column. Also, difference of the
pressure has to be minimized because it’s essential to operate distillation column in constant
pressure condition to prevent column from flooding and weeping, and to maintain stability of
downstream. Therefore, pressure measurements are very important to maintain the operation
safe while obtaining maximum products rate.

The pressure at the top of the column is normally high. Therefore, it is required to obtain a
pressure reading at the top of column to maintain operation safely. If the pressure at top is
higher than required value, more cooling load is needed. Based on these requirements, a
pressure sensor should be located at the top vapor-out pipe line to measure the top column
pressure. For that, a diaphragm type pressure sensor is used.

Pressure indicators are also vital to ensure the safe operation


of the system. Therefore, pressure indicators are used at the
reflux drum and bottom of the column. Also, Pressure
indicators are installed at the suction and discharge of all
centrifugal pumps that are used in the process, for
predictive maintenance and troubleshooting. Diaphragm
pressure gauges are selected to indicate the pressure.

Figure 8-6-Diaphragm Pressure Gauge

68
8.4.2 Temperature Measurement
As well as pressure measurements, temperature measurements are also crucial, because
controlling temperature is used as a substitute to product composition analysis. It is an easy
and inexpensive than controlling product composition (Kister, 1990). The change in control
temperature represents a corresponding variation in the concentration of key component in the
product. As an example, a rise in the top section control temperature represents a rise in the
concentration of the heavy key component in the top product. Then, the purity of the top
product couldn’t be achieved.

Normally, temperature measurements are taken in top stage, bottom stage and feed flow of a
distillation system. Product purity can be achieved by controlling these temperatures. Thus,
temperature sensors are installed in these location. Several factors should be considered when
selecting a temperature sensor. Some of them are operating temperature range, sensitivity,
precision, reliability and accuracy.

The most common type of temperature sensors used in petrochemical industry are
thermocouples and resistance thermometers (resistance temperature detectors-RTDs).
Thermocouples are low cost and they are used in locations that need a more durable sensor.
Although resistance thermometers are more sensitive and accuracy is high (Anon., 2010). Since
xylene is toxic and hazardous gas, resistance thermometer is selected as the sensor. Platinum,
Nickel and Copper are the most commonly used sensing elements using in RTDs. Among them,
Platinum is considered the best as it has the widest temperature range (-200-800℃) (John,
2011). Also, it is widely used in petrochemical industry. Therefore, platinum resistance
temperature detectors are selected for the installment.

Figure 8-7-Platinum Resistance temperature Detector

69
8.4.3 Level measurement
Distillation is placed high requirements on level measurements. Usually accumulation of
condensate in the reflux drum and column is controlled by manipulating top and bottom
product flow. Besides traditional technologies like differential pressure level meters, radar,
magnetostrictive, and magnetic float are also used extensively in petrochemical industry.

Among them, radar level meter is selected for the installment. It is an electronic non contacting
device which can measure level continuously. Maintenance cost is low, but initial cost may be
high. However, it is more suitable, because xylene is toxic and flammable.

8.4.4 Flow measurement


Flow measurements are also taken as pressure, temperature and level measurements, because
it is important to make it clear how much oil chemicals are transported in each pipe to control
process properly. In here, liquid and vapor are transported through pipes. Therefore, flow
measuring equipment should be capable with measuring both liquid and vapor flow.

Orifice plate flow meters which can be used to measure both liquid and vapor flow rates are
used in this case due to their applicability over a broad range and relatively low cost. Therefore,
orifice plate flowmeters are installed in here.

70
8.5 Process Control Aspects
Generally, distillation column control system should achieve the following main three
objectives.

 Set stable conditions for column operation


 Regulate conditions in the column so that the product always meet the required
specifications
 Achieve the above objectives most efficiently (minimize energy consumption,
maximizing product recovery)

To achieve these three objectives, it is essential to control variables such as pressure,


temperature, level and flowrates. Different control strategies have been implemented and
various control structures have been developed depending on the requirements.

8.5.1 Pressure control in the column


In order to control column pressure, some mechanism is required to vary the heat transfer rate
in condenser. The possible mechanisms are given below.

Media side- In here, valve at the cooling water inlet of the cooling water condenser or speed
of the fan of the air cooled condenser can be controlled. Both control and process issues are
arisen.

Process side – The most common approach is flooded condenser. In here, a part of the
condensate is retained within the condenser in order to reduce the effective surface area for
heat transfer.

In most distillation columns, the pressure is controlled through the heat removal in the
condenser. Also, air - cooled condensers are difficult to operate as flooded condensers (Kister,
1990). Therefore, the method of pressure controlled through heat removal is selected to control
the process. In here, the condensation rate in condenser must be increased with the increase of
the pressure. To increase the condensate rate, the rate of heat removal in the condenser must
be increased. Therefore, the cooling water flow to the condenser must be increased. Some
issues are arisen when controlling condenser cooling water flow rate. The main reason is the
fouling in cooling water condenser. So it is required to design carefully to avoid these issues.

The cooling water control valve is usually located on the return, but it can also be located on
the supply line. From the perspective of control performance, it makes no difference. The

71
control valve affects the condensation rate in the condenser in exactly the same manner when
located on the supply as when located on the return.

8.5.2 Controlling the overhead and bottom product


The composition of the overhead product is more important in here, because it depends on the
purity of o-xylene. Therefore, it is desirable to maintain a constant temperature profile
throughout the column. This is done by controlling the feed, reflux and reboiling vapor flows.

The temperature in the upper section of the column is maintained by using the reflux flow. The
reflux flow rate must be increased with the increment of the top column temperature. When
increasing the reflux rate, the reflux ratio is increased. However, reflux ratio should be
maintained constant. It is done by regulating the top product outlet. Also, the level of the reflux
drum will be reduced when increasing the reflux rate to maintain the top temperature of the
column. Then, cavitation may be happened in overhead pump system. Pump cavitation is the
formation and subsequent collapse or implosion of vapor bubbles in a pump. Therefore, the
level of the reflux drum should be maintained properly. This is done by controlling top product
outlet.

PC

Condenser V-1

PT

LC
TC

TT
LT

Reflux Drum

V-2 V-3

Figure 8-8-Distillation column overhead control system

The middle temperature of the column is kept constant by maintaining feed temperature
constant. The feed flow rate is not always constant. Therefore, the feed temperature is
controlled by controlling heat load of the furnace coil. It is controlled by manipulating the oil
TT
feed TCrate to the column.
LC

LT
V-4
72

LC

Furnance
TT
TC

LC

LT
V-4

TT
LC

TC
Furnance
V-6

Pump

V-5
Figure 8-9-distillation column bottom control system

The column bottom temperature can be maintained by using the reboiler vapor flowrate. In
here, furnace is used instead of the reboiler. The heated vapor outlet from the furnace is used
to maintain the column bottom temperature. The heat load required to vaporize bottom liquid
in the furnace is supplied by burning oil. Therefore, the amount of oil supplied to the furnace
is required to be controlled properly. This is done by obtaining a temperature measurement at
the pipeline of the vapor flow from the furnace to the column.

As the top reflux drum, the liquid level of the column is required to be controlled to maintain
the proper functioning of the pumps. Therefore, the bottom product outlet rate is manipulated
to control the liquid level of the column.

73
8.6 PI Diagram

PT PC

PI TI
PI PI

6''

V-12 Cooling water In


V-13
02
V-40
V-08 V-11
C-01 V-10
FM-02

V-09
Safety Relief V-39 V-14 V-15

TT

V-07

TC C-02
Cooling water Out

DWC-01 Reflux In
23 06
1½'' Vent Out
V-16
RD-01
TC
O-xylene column TT
PI
V-18 V-19 V-20 PI LT
Feed

01
V-21
FM-01
V-26
Y-01 V-17
F-01 P-01
V-22 V-23 PI
PI
PI
PI
Drain Out

TI
Furnace oil Feed PI
Y-02
V-01 3½'' 07 V-25 PI
V-24 V-26 P-02 PI LC

TC
TI
PI
07
TT V-27 V-28 V-29
V-41 V-42 V-43 Top Product Out
01 3½''
TT
05 FM-03
4'' V-30
V-44
LT LC
PI
TI

TC PI
TI PI
PI TI
PI PI
F-02 PI
03
V-32 V-33
04
V-06 V-36 V-37 V-38 Bottom Product
3½'' Y-03 3½'' FM-04
P-03 Out
V-04
V-02 PI
PI V-34
PI
Furnace oil Feed Drain Out PI

3½ '' V-31 V-35

V-05 Y-04
P-04

DWC-01 C-01 RD-01

OTHO XYLENE COLUMN OVERHEAD CONDENSER- WIND FANS REFLUX DRUM


OP. AVG. PRESSURE – 340 kPA OP. AVG. PRESSURE – 390 kPA OP. AVG. PRESSURE – 390 kPA
OP. AVG. TEMPERATURE – 222 0C
NO. PLATES – 23 C-01
FEED PLATE – 7th (FROM BOTTOM)
COOLING WATER CONDENSER
OP. AVG. PRESSURE – 340 kPA

STREAM ID 1 2 3 4 5 6 7 REFERENCE DRAWING

MOLE FRACTION LIQUID 0.6 0 1 1 0 1 1 Title NO DWG NO


o
TEMPERATURE ( C) 212 194.8 194.8 30 250.8 194.7 30
MOLECULAR WEIGHT(g) 117 106 137 137 137 106 106
PRESSURE(kPA) 340 390 290 - - 390 -
RATE(kg/hr) 15943.62 12874.18 16406.91 6825.25 9581.66 3755.81 9118.37
3
DENSITY(kg/m ) 470.11 9.27 178.01 178.01 11.88 505.74 505.74
BUILT BY- W.M.H.E.Wijesinghe
MOLAR COMPOSITION
DATE -21/01/2017
P5 581.34 581.34 0.00 0.00 0.00 0.00 581.34
(Company Name)
M-Xylene 162.72 217.27 3.48 3.48 0.00 58.03 159.24
O-Xylene 6260.43 8690.81 681.06 124.38 556.68 2554.76 6136.05
P & I DIAGRAM
A9 2610.47 3328.30 1853.18 399.99 1453.19 1117.82 2210.48
P11 2383.86 56.45 6211.79 2352.60 3859.20 25.19 31.26 O-xylene Column
A10 3346.73 0.00 6707.21 3346.73 3360.48 0.00 0.00 SHEET
DRAWING NUMBER REV
01 of 01
A11 598.07 0.00 950.19 598.07 352.12 0.00 0.00

74
CHAPTER 9 - COLUMN OPERATING PROCEDURE
The purpose of the distillation column is to separate otho xylene from mixed aromatics with
xylene. Xylene is a very toxic and flammable gas. Therefore, it is essential to operate the
distillation column safely. So it is very important to identify the startup and shutdown
procedure of the distillation column.

9.1 Startup procedure of a distillation column


General column startup procedure is discussed here. It usually consists with following steps.

1. Commissioning – In this operation, it is cleared that the system of undesirable material


and tested it for introducing chemicals.
2. Final elimination of undesirable material
3. Bringing the column to its normal operating pressure
4. Column heating and cooling
5. Introducing feed
6. Starting up heating and cooling sources
7. Bringing the column to the desired operating rates.

9.2 Shutdown procedure of a distillation column


Similarly, Column shutdown also consists of the following steps.

1. Reducing column rates


2. Shutting down heating and cooling source
3. Stopping feed
4. Draining liquid
5. Cooling or heating medium
6. Bringing the column to atmospheric pressure
7. Eliminating undesirable material
8. Preparing the column for opening to atmosphere
The above two sequences of steps are used for startup and shutdown operations.

9.3 Emergency shutdown procedure of a distillation column


It is very important to identify emergency shutdown procedure, since xylene is flammable and
toxic liquid. It consists several steps.
1. Shut off oil line of the furnace using the oil control valve.
2. Switch off the feed pump. Shut off the oil line to the feed preheater.

75
3. Turn on the cooling water to the distillate product cooler if it is not already on.
4. open the distillate product manual control valve fully.
5. Turn on the cooling water to the bottoms product cooler if it is not already on.
6. If it is not intended to go to the restart operation, the remaining normal shutdown
procedures should be continued.

9.4 Useful Startup and shutdown lines


Besides the "normal" piping for continuous operation, column piping often contains lines
whose primary purpose is to minimize material loss or speed up startups and shutdowns. These
lines are not normally used during column normal operation, but they can be extremely useful
at times of startup or shutdown.

Some of more common useful lines at startup and shutdown are given below.

1. Pressuring up lines- These lines are used to be pressured up with the desirable materials
prior to starting up. Designed distillation column is operated as pressure distillation.
Therefore, the column needs to be bought close to its normal operating pressure prior
to liquid feed. That is done to avoid the brittle failure of the column. At shutdown, all
liquid should be drain out of the column before de-pressuring. It is more suitable to
pressured up with a liquid mixture or gas of similar volatility, rather than inert gas.
2. Column bypass lines- These lines are more essential if the column is in a compressor
train and may be sensitive to surging.
3. Line for recycling top/bottom products to feed tank- These pipe lines are useful for
minimizing the amount of off-spec materials produced.
4. Lines for circulating liquid- These lines are useful when liquid circulation is performed
at startup.
5. Line for introducing feed at the reboiler inlet sump- These lines are useful for avoiding
excessive temperature at the column bottom.

9.5 Troubleshooting of distillation column


In this section general distillation operation problems and possible causes are discussed.

9.5.1 Flooding
Flooding is accumulation of liquid in the distillation tower. When a distillation column floods,
tray efficiency diminishes, separation deteriorates, and products go off-spec. It can be
recognized by following symptoms.

76
1. Excessive column pressure drop – In general, the pressure drop per tray greater than 50
to 60% of the tray spacing in the relevant column section indicate flooding (Kister,
1990).
2. Sharp rise in column pressure drop - This is more sensitive flooding indicator than
excessive column pressure drop
3. Reduction in bottoms flow rate - it is good indicator of flooding in columns which are
relatively short.
4. Rapid rise of entrainment from column top tray
5. Loss of separation

The primary tool for flooding point determination is measuring pressure drop across various
column sections. Also gamma ray scanning technique is a technique widely used for flooding
detection in petrochemical industry. Flooding can be eliminated by using following techniques.

1. Variating distillation column pressure


2. Changing preheating/precooling condition
3. Unloading the column-reducing plant rates
4. Improving stability

9.5.2 Foaming
Foaming in a distillation column is the expansion of liquid that provides high interfacial liquid-
vapor contact. It can be recognized by following symptoms (Kister, 1990).
1. Premature flooding and massive entrainment
2. Flood data are non-reproducible
3. Additional point of inflection on a downcomer gamma ray scan.
The more reliable technique is done for testing foaming is ‘an armored level glass technique’,
which is capable of duplicating plant condition of temperature, pressure and composition.
Inject inhibitors is the simplest technique used widely, but the inhibitor should be chosen and
injected correctly. The main issue of using foaming inhibitors is expensive downstream
filtration, because it is required to remove them. It is a more expensive process and activated
carbon is widely used to remove.

77
CHAPTER 10 - SAFETY ASPECT
Safety is crucial in manufacturing processes. The ultimate goal in safety is having zero
accidents, preventing injuries and losses in work time. Therefore, it is very important to
properly identify the risks and implement good safety practices to achieve above goals in any
process. In o-xylene distillation column, the safety aspects are discussed under following
headings.

1. Personal protection
2. Fire measures
3. Accidental release measure
4. Handling and storage

10.1 Personnel protection


The main raw material used in this distillation unit is o-xylene. According to material data
sheet, o-xylene is identified as hazardous in case of skin contact (irritant, permeator), eye
contact (irritant), ingestion and inhalation. Therefore, personal protective equipment should be
provided to the employees. Following personal protective equipment are generally used.

 Protective gloves
 Safety goggles
 Appropriate cloth with safety shoes
 Vapor respirators

In additionally, emergency eye wash and shower stations should be located. Since xylene is a
toxic gas, emergency respirators should be provided.

10.1.1 First aid measures


 Eye contact – Immediately flush eyes with running water for at least 15 minutes,
keeping eyelids open. Get medical attention
 Skin Contact - In case of contact, immediately flush skin with plenty of water. Cover
the irritated skin with an emollient. Remove contaminated clothing and shoes.
Thoroughly wash and clean cloths/shoes before reuse. Get medical attention.
 Inhalation: If inhaled o-xylene gas, remove to fresh air. If not breathing, give artificial
respiration. If breathing is difficult, give oxygen. Get medical attention.

78
 Ingestion: Don’t induce vomiting without any advice of medical officer. Never give
anything by mouth to an unconscious person. If large quantities of this material are
swallowed, call a physician immediately.

10.2 Fire measures


When considering the unit of o-xylene separation distillation column, the overhead product is
99.9%(w/w) purified o-xylene. According to the MSDS available, o-xylene is classified as

Flammability of the Product : Flammable.

Auto-Ignition Temperature : 463°C

Flash Points (closed cup) : 17°C

Flammable Limits : Lower- 0.9% /Upper- 6.7%

Fire Hazards in Presence of Various Substances : Highly flammable in presence of open


flames and sparks, of heat.

Therefore, it is very important to eliminate the presence of ignition sources such as welding
sparks while doing maintenance and constructions, electrical wirings and equipment which
cause sparks, static charges due to friction force and hot surfaces.

In addition, firefighting equipment should be installed to face any case of fire occurred. Also,
Fire trainings and drills should be conducted from time to time to train the workers.
Additionally, fire and smoke detection alarms systems should be installed and maintained
properly.

10.3 Accidental release measure


According to the MSDs, following measures are summarized for o-xylene.
Small spill: Absorb with an inert material and put the spilled material in an appropriate waste
disposal.

Large spill: o-xylene is a toxic flammable liquid and it is very slightly soluble in water.
Therefore, it should be kept away from source of ignition. It can be absorbed with dry earth,
sand or other non-combustible material. Don’t take water inside container. Do not touch spilled
material. Prevent entry into sewers, basements or confined areas; dike if needed. Call for
assistance on disposal. Be careful that the product is not present at a concentration level above
TLV. Check TLV on the MSDS and with local authorities

79
10.4 Handling and Storage
Precautions: Keep locked up. Keep away from heat and sources of ignition. Ground all
equipment containing material. Do not ingest. Do not breathe gas/fumes/ vapor/spray. Wear
suitable protective clothing. In case of insufficient ventilation, wear suitable respiratory
equipment. If ingested, seek medical advice immediately and show the container or the label.
Avoid contact with skin and eyes. Keep away from incompatibles such as oxidizing agents,
acids.

Storage: Store in a segregated and approved area. Keep container in a cool, well-ventilated
area. Keep container tightly closed and sealed until ready for use. Avoid all possible sources
of ignition (spark or flame)

10.5 HAZOP Study Applied to the Distillation Column


In here, distillation process is used to separation of o-xylene. It is a thermal separation and
energy is mainly obtained by burning oil in furnace. This distillation system contains specific
units such as column, reflux drum, condenser, furnace and pumps. This unit can cause different
problems in the operation.
The Problems that may represent risks to equipment or personnel can be easily identified and
evaluated by using hazard analysis. A HAZOP (s hazard and operability study) survey is one
of the most common and widely accepted methods of systematic qualitative hazard analysis

80
Table 40-HAZOP Study of the Distillation Column

Project Name: Production of p-xylene Date: 2017/01/23


Process : Separation of o-xylene
Section: Distillation column

Process Guide
Study Node Possible causes Passible consequences Action required
parameter Word
Feed flow Flow NO  Shutoff valve fully closed  Column dry out  Install low level alarm
 Blockage in feed pipe  No operation  Regular done maintenance
 Leakage in feed pipe  Damage to sensors and of pumps, valves and pipes
 Feed Pump failure internals.  Install filters
 Failure of controller  Make bypass
 Emergency shutdown
Less  Partially closed of shutoff  Changes in product quality  Install law level alarm
valve  Colum dry out  Regular done maintenance
 Failure of controller of pumps, valves and pipes
 Leakage or blockage  Make bypass
 Feed Pump failure  Emergency shutdown
More  Failure of controller  Flooding in the column  Install high level alarm
 Failure of feed pump  Changes in product quality  Regular done maintenance
controller  Temperature decrease
 Rise in bottom flowrate
Distillation Pressure Low  Vapour line leakage  Weeping  Install pressure indicators
Column  Pressure relief valve  Low efficiency of  Install low level alarm
malfunctioning operation  Regularly done maintenance
81
 Reflux/feed line controller  Change of product quality
failure
 Furnace failure
High  Vapour pressure high  Low efficiency of product  Install pressure relief valve
 Pressure indicator failure separation  Install high pressure alarm
 Controller failure  Rupture the column
 Product loss
Temperature Low  Furnace failure(fouling)  Pressure change  Install temperature indicator
 Loss of heating(leakages)  Loss of products  Upgrade isolations
 Ineffective isolation  Change of product quality  Attention to heat input and
 Reflux flow controller  Ineffective product output (reflux, vapour and
failure separation feed in)
 Properly done maintenances
and operations
 Install low level alarm

High  Furnace controller failure  Separation can’t be done  Install pressure indicator
 Cooling water condenser or  Loss of product  Instruct operation procedure
trim fan failure  Change of product quality  Attention of heat input and
 Reflux controller failure  Column flooding output
 Heating medium is leak to  Phase effect  Install high level alarm
the process  Pressure change system
Level Low  Inadequate feed/reflux flow  Column dry out  Regular monitoring the
 Increase the bottom  Bottom Pump failure control systems
temperature  Excessive foaming  Properly done maintain ace
 Column pressure increase  Process failure  Install low level alarm

82
High  Uncontrolled feed/reflux  Weeping inside the  Regularly done
flow column maintenances
 Reduce the bottom  Change of product quality  Install high level alarm
temperature  Failure of separation
 Block or controller failure in
bottom pipe lines
 Pump failure

83
CHAPTER 11 - ECONOMICS ASPECTS
In this section, a rough estimate of the total capital cost investment required for the vessel is
done. The accuracy of an estimate of the capital cost of a distillation column depends on the
amount of detail available, accuracy of the cost data available and the time spent on preparing
the estimate. The total capital cost of a distillation column is the sum of the costs for condenser,
reboiler, tower and trays and miscellaneous cost including controlling, piping, pumps and etc.
In here, a rough estimation of total capital cost is done neglecting control, piping and pumps
capital costs.

Following criteria given in equilibrium stage separation book, Phillip C. Wankat is used to
estimate the capital cost for the design (Wankat, 1988).

11.1 Capital cost of the shell


(1.34 + 1.16)⁄
The average diameter of the column - 2 = 1.25 𝑚 =4.10ft

The total height of the column – 16.37m - 53.71ft

The number of sieve trays – 23

The maximum design pressure – 540Kpa(absolute) -76.98 psig

According to following graphs,

The cost of the shell having 4.1ft diameter 25-tray column at 76psig is $ 35000 and for 50tray
column, the cost is $90000. A linear interpolation for 23 stages gives, the cost of the column is
$ 30600. An alternative interpolation is also used,

𝑁𝑜 𝑜𝑓 𝑡𝑟𝑎𝑦𝑠 𝑠𝑖𝑧𝑒 𝐴 𝑒𝑥𝑝𝑜𝑛𝑒𝑛𝑡


𝐶𝑜𝑠𝑡 𝑠𝑖𝑧𝑒 𝐴 = (𝑐𝑜𝑠𝑡 25𝑡𝑟𝑎𝑦𝑠) × ( )
25

Exponent can be calculated using following equation,

𝐶𝑜𝑠𝑡 𝑜𝑓 50 𝑡𝑟𝑎𝑦𝑠
ln( ) ln(90000)
𝑐𝑜𝑠𝑡 𝑜𝑓 25 𝑡𝑟𝑎𝑦𝑠 35000 = 1.3626
𝐸𝑥𝑝𝑜𝑛𝑒𝑛𝑡 = =
50
ln( ⁄25) ln(50⁄25)

𝟐𝟑
𝑪𝒐𝒔𝒕 𝒔𝒊𝒛𝒆 𝑨 = 𝟑𝟓𝟎𝟎𝟎 × ( )𝟏.𝟑𝟔𝟐𝟔 = $ 𝟑𝟏𝟐𝟒𝟏
𝟐𝟓

To be conservative, higher value is selected for the cost of the column, $ 31241.

84
Figure 11-2-50 trays -Cost of sieve tray distillation Figure 11-2-25 trays -Cost of sieve tray distillation columns

11.2 Capital cost of the sieve trays


Tray, tower casing, reboiler and condenser cost can be calculated by using following equation
given in the table below.
𝑑𝑖𝑎𝑚𝑒𝑡𝑒𝑟, 𝑓𝑡⁄ 4.10
The sieve tray cost - $ 151 × ( 3) = 151 × 3 =$ 206
Total sieve tray cost - 𝑪𝒐𝒔𝒕 𝒐𝒇 𝒂 𝒑𝒍𝒂𝒕𝒆 × 𝑵𝒐 𝒐𝒇 𝒑𝒍𝒂𝒕𝒆𝒔 = 206×23 = $ 4738

Figure 11-3-Cost equations for Distillation Equipment

85
11.3 Capital cost of the condenser
Area of the condenser –
Mass flowrate - 12874.18 kg/hr
Vapor input temperature - 258℃ liquid out temperature - 40℃
Average heat capacities and latent heat is calculated using aspen plus software.
CpVapour – 2.05 kJ/kgK Cpliquid -2.19 kJ/kgK latent heat – 3470 kJ/kg
The heat load of the condenser –
𝑄 = 12874.18 × (2.05 × (258 − 160) + 2.19 × (160 − 40) + 3470) = 50643𝑀𝐽/hr
Cooling water –
input temperature - 30℃ liquid out temperature - 50℃
Assume overall heat transfer coefficient as 1000 W/m2C and all the vapor is condensed using
a cooling water condenser.
LMTD – 65.24℃
50643
( )×106
Area of the condenser – 3600
= 215𝑚2 = 2314.24𝑓𝑡 2
1000×65.24
𝟎.𝟒𝟖
𝒂𝒓𝒆𝒂, 𝒇𝒕𝟐⁄ 𝟎.𝟒𝟖
Condenser cost - $ 𝟒𝟎𝟖𝟎 × ( 𝟓𝟎) = 𝟒𝟎𝟖𝟎 × (𝟐𝟑𝟏𝟒. 𝟐𝟒⁄𝟓𝟎) = $ 𝟐𝟓𝟕𝟎𝟖

11.4 Capital cost of the Process furnace


In here, a process furnace is used to supply heat load required to heat up the feed in and the
bottom feed in of the column. The cost of the furnace is estimated using the criteria given in
the book of Conceptual Design of Chemical Processes, James Merrill Douglas (Douglas, 1988).

Distillation Feed in - 30℃ Distillation feed out - 222℃

The average heat capacity – (2.285 + 1.759)/2= 2.02 kJ/kgK

The heat load required to heat up feed in – Qfeed= 15943.62 ×2.02× (222-30) = 6183.5 MJ/hr

Reboiler feed in - 258℃ Reboiler out - 258℃

Latent heat of bottom product - 3380 kJ/kg

The heat load required to reboil – Qreboil-9581.66×3380 = 32384 MJ/hr

The total heat load required – 38567.5 MJ/hr = 36554936.78 BTU/hr =36.55×106 BTU/hr

86
Tube Material: A214

(Electric-resistance-welded
carbon steel heat exchanger
and condenser tubes)

Design Pressure: 500 psig


Design Temperature: 750 °F

Figure 11-4-Process Furnace (Loh & Lyons , 2002)

By using graph,
𝑃𝑢𝑟𝑐ℎ𝑎𝑠𝑒𝑑 𝑐𝑜𝑠𝑡, $ = $ 400000
𝐹𝑐 = 𝐹𝑑 + 𝐹𝑚 + 𝐹𝑝 = 1 + 0 + 0 = 1

𝐶𝑎𝑝𝑖𝑡𝑎𝑙 𝑐𝑜𝑠𝑡, $ = (𝑃𝑢𝑟𝑐ℎ𝑎𝑠𝑒𝑑 𝑐𝑜𝑠𝑡, $) × (1.27 + 𝐹𝑐 ) = $ 400000 × 1.27 = $ 508000

Figure 11-5-Correction Factors Fc for process furnace

87
11.5 Total capital cost of the distillation system
Table 41-Total Capital Cost Calculation

Equipment Capital cost


Distillation Column $ 31241
Sieve plates $ 4738
Condenser $ 25708
Furnace $508000
Total Capital Cost $ 569687

Therefore, the total cost required for the design, construction, installation and auxiliaries of
the o-xylene distillation column is $ 569687.

88
CONCLUSION
Ortho-xylene is a commercial isomer of xylene. It is a hydrocarbon based on benzene, with
two methyl substituents bonded to adjacent carbon atom. 90% of o-xylene global production
is used to manufacture phthalic anhydride (PAN), an aromatic anhydride acid used to produce
plasticizers (Such as PVC). o-xylene is also used as a solvent in solvent based paints and used
for lubricating oil additives, herbicide and bactericides production. Therefore, o-xylene should
be separated from mixed xyene and other heavy hydrocarbons. In here, the target purity of the
o-xylene is 99%. Distillation separation is the most suitable method. So, it is used here to
separate o-xylene.

The designed distillation column consists with 23plates. The dimensions of both stripping and
rectifying section are calculated in here to obtain a maximum yield. The piping and instruments
also designed according to the correct specifications. Classical feedback control structure is
used to control the flow, temperature, pressure and level. Detailed drawing of P & I diagram,
and drawing of each equipment are attached with the report. All safety aspects, startups,
shutdowns and emergency shutdown procedures are discussed in detail. Economic aspects are
being considered and the total capital cost investment is found as 85.818 million LKR.

In here, classical feedback control structure is used, but modified control structures are now
available. Therefore it is more suitable to use those kind of modified control structures. The
design of the furnace cost is higher than others. Therefore, it is more suitable to used existing
furance by doing modifications. Also, The heat integration system of the distillation column is
not discussed here,but it also important topic like others. Because, Operating cost and capital
cost of the process are depend on heat integration systems.

89
REFERENCES

1. Anon., 2001. THERMAL INSULATION HANDBOOK. LYTTELTON: Thermal


Insulation Association of Southern Africa.
2. Anon., 2010. National Instruments. [Online]
Available at:
http://digital.ni.com/public.nsf/allkb/C50FA55B3B2F85D9862572D00083350E
[Accessed 23 January 2017].
3. Anon., 2015. TORISPHERICAL HEAD VOLUME. [Online]
Available at: www.ksecal.com/torispherical-head-volume.php
[Accessed 05 01 2017].
4. Anon., n.d. Is glass wool better than rock wool?. [Online]
Available at:
http://www.knaufinsulation.ee/sites/ee.knaufinsulation.net/files/Rock_Vs_Glass.pdf
[Accessed 04 01 2017].
5. Chuang, K. T. & Nandakumar, K., 2000. Tray Columns: Design. [Online]
Available at: http://razifar.com/cariboost_files/Tray_20Columns_20Design.pdf
[Accessed 10 12 2012].
6. Douglas, J. M., 1988. Conceptual design of chemical processes. In: Appendix E-Cost
Data. s.l.:McGraw-Hill,, pp. 569-580.
7. G. A. Aaker, J. P., n.d. [Online]
Available at: http://www.engineering-experts.com/definition-of-corrosion-
allowance.pdf
[Accessed 30 12 2016].
8. Gandy, D., 2007. Carbon Steel Handbook. Kalamazoo: ELECTRIC POWER
RESEARCH INSTITUTE .
9. Jaya, A., 2011. Distillation Column Selection and Sizing. [Online]
Available at:
http://kolmetz.com/pdf/EDG/ENGINEERING%20DESIGN%20GUIDELINES%20-
%20distillation%20column%20-%20Rev%2003%20web.pdf
[Accessed 08 12 2016].
10. John, 2011. Resistance Temperature Detector (RTD). [Online]
Available at: http://www.instrumentationtoday.com/resistance-temperature-detector-
rtd/2011/09/
[Accessed 23 January 2017].
11. Kister, H. Z., 1990. Distillation Operation. New York: Mc Graw Hill.
12. Loh , H. P. & Lyons , J., 2002. Process Equipment Cost Estimation, Pittsburgh:
National Energy Technology Center .

90
13. Naik, S. et al., n.d. DISTILLATION COLUMNS. [Online]
Available at:
http://encyclopedia.che.engin.umich.edu/Pages/SeparationsChemical/DistillationColu
mns/DistillationColumns.html
[Accessed 08 12 2016].
14. pagina, D., 2016. Y-Strainer. [Online]
Available at: http://www.lenntech.com/systems/sediment/y/y-strainer.htm
[Accessed 22 01 2017].
15. Sandhyarani, N., 2016. The Various Types of Distillation That are Worth Knowing.
[Online]
Available at: http://www.buzzle.com/articles/types-of-distillation.html
[Accessed 09 12 2016].
16. Sinnott, R., 2005. Coulson & Richardson’s Chemical Engineering Design. 4th ed.
s.l.:s.n.
17. Sloley, A., 2012. Select the Right Reboiler. [Online]
Available at: http://www.chemicalprocessing.com/articles/2012/select-the-right-
reboiler/
[Accessed 10 12 2016].
18. Wankat, P. C., 1988. Equilibrium Staged Separation. Indiana: Prentice Hall.
19. WU, S., ZHAO, Y., FENG, X. & CHU, K. H., 2011. Simulation and Optimization of
an O-xylene Columns. Advanced Materials Research, Volume 236-238, pp. 67-71.

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