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Hashan Eranda
University of Moratuwa
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All content following this page was uploaded by Hashan Eranda on 05 March 2017.
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.
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
vii
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.
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
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.
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.
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.
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
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.
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.
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
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.
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.
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
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,
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)
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|
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
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 - -
By linear interpolation,
At R= 0.4
𝑫. 𝒙𝐴9 ,𝐷 = 𝟏𝟖. 𝟑𝟗 𝑾. 𝒙𝐴9 ,𝑤 = 𝟑. 𝟑𝟏
At R= 0.4
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
Calculation –
For top operating section by reflux ratio
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
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
3rd Plate
4th Plate
18
Table 7-4th Plate Vapor and Liquid Compositions
5th Plate
Table 8-5th Plate Vapor and Liquid Compositions
6th Plate
Table 9-6th Plate Vapor and Liquid Compositions
19
Temperature of 6th plate - 201.1 ℃
For 6th plate
7th Plate
Table 10-7th Plate Vapor and Liquid Compositions
8th Plate
Table 11-8th Plate Vapor and Liquid Compositions
9th Plate
20
Table 12-9th Plate Vapor and Liquid Compositions
Next, calculation of the number of plates and composition of each plate of the stripping section
is done.
𝑦𝑖,𝑚+1 = 𝐾𝑖 . 𝑥𝑖,𝑊
2nd Plate
Table 14-2nd Plate Vapor and Liquid Compositions
3rd Plate
Table 15-3rd Plate Vapor and Liquid Compositions
22
4th Plate
Table 16-4th Plate Vapor and Liquid Compositions
5th Plate
Table 17-5th Plate Vapor and Liquid Compositions
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
8th Plate
Molar volume of the liquid mixture - 0.251 m3/kmol (By using Aspen plus)
Molar volume of the liquid mixture - 0.371 m3/kmol (By using Aspen plus)
25
Weight of the mixture - 121.119 kg
10th Plate
Molar volume of the vapor mixture - 12.358 m3/kmol (By using Aspen plus)
13th Plate
Molar volume of the liquid mixture - 0.764 m3/kmol (By using Aspen plus)
Reboiler
Molar volume of the Vapor mixture - 11.409 m3/kmol (By using Aspen plus)
325.86 +178.01
Average Density of liquid in stripping section - 𝜌𝐿′ = = 𝟐𝟓𝟏. 𝟗𝟒 𝒌𝒈/𝒎𝟑
2
Summary:
Table 20-Summary of density calculations
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
0.117 + 0.106
𝑀𝑊𝑟𝑒𝑐𝑡𝑖𝑓𝑦𝑖𝑛𝑔 = = 0.112 𝑘𝑔/𝑚𝑜𝑙
2
27
V' 72.83 0.127 9249.41 2.57
Note: It should be checked if this value for plate spacing is compatible with the column
diameter, after calculating the Dc.
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
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
487.93 − 9.50
𝑈𝑓 = 0.056 × √
9.50
= 0.397 𝑚/𝑠
29
1.1.1.5 Maximum Volumetric Vapor Flow rate
𝑉𝑤 3.75 𝑚3
𝑉𝑣 = = = 0.395
𝜌𝑣 9.50 𝑠
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
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
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
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.
Therefore, the assumed value for tray spacing is compatible. Hence, the assumed value for tray
spacing acceptable.
487.93 + 251.94 𝑘𝑔
= 369.94 ⁄𝑚3
2
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
33
ℎ𝑜𝑤 + ℎ𝑤 = 12.51 + 45 = 57.51 𝑚𝑚
By the Graph;
𝐾2 − 30.40
[𝐾2 − 0.9(25.4 − 𝐷ℎ ]
𝑈ℎ,𝑚𝑖𝑛 =
√𝜌𝑣
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
2
4.33 3
ℎ𝑜𝑤 = 750 × [251.94×0.94] = 𝟓𝟐. 𝟎𝟓 𝒎𝒎
Minimum vapor velocity is greater than the minimum vapor velocity through the holes.
Therefore, weeping doesn’t occur.
36
molar average liquid viscosity - 𝜇𝑎 - 0.216 𝑚𝑁𝑠/𝑚2 (When vapor fraction = 0.5) [Aspen plus
V8.0]
= 57.265%
𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑛𝑜 𝑜𝑓 𝑡𝑟𝑎𝑦 13
- = = 𝟐𝟐. 𝟕𝟎 ≈ 𝟐𝟑 𝒕𝒓𝒂𝒚𝒔
𝑡𝑟𝑎𝑦 𝑒𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 0.5726
−0.60 × 23 = 𝟏𝟑. 𝟖𝟎 𝒎
37
4.14 Summary of chemical design
Table 25-Summary of Chemical Design
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.
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.
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).
Properties SA-290
Material type Carbon steel plate (< 25)
Maximum Tensile Strength (MPa) 515
Maximum Yield Strength (MPa) 290
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.
According to Section VIII of ASME Boiler & Pressure Vessel Code 2008, this belongs to the
category where,
Pin Pexternal
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
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,
𝑷𝑫𝒆𝒔𝒊𝒈𝒏 × 𝑫
𝑡𝑎𝑐𝑡𝑢𝑎𝑙 = +𝑐
2 × 𝜑 × 𝝈𝑫𝒆𝒔𝒊𝒈𝒏
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.
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.
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,
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).
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,
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 )
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
1.348 1.168
− tan(25)
(HReducer) - [ tan(25) ⁄ ] = 0.193 𝑚
2
Figure 7-1-Cross section of the Reducer
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.
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
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
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.
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.
The external boundary limit should be calculated using the following equation,
51
𝑑𝑟 = 2 × (𝑂𝐷 − 2𝑡𝑛 ) = 2 × (101.60 − 2 × 3.048) =191.01mm
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.
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.
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
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.)
54
chapter, calculations are carried out to inspect the stability of the o-xylene column for combined
loadings.
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,
Both circumferential and longitudinal stresses are way below the design stress.
55
Table 36-Column Weight Calculation
2𝜋𝑟 3
𝑇ℎ𝑒 𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑏𝑜𝑡𝑡𝑜𝑚 𝑐𝑙𝑜𝑠𝑢𝑟𝑒 –
3
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.
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
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
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.
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
59
If 𝜎𝑡𝑒𝑛𝑠𝑖𝑙𝑒 < 𝜎𝑑𝑒𝑠𝑖𝑔𝑛 𝜑 then the used thickness is okay for the skirt.
t
Allowable compressive stress : compressive 0.125E sin
D
Young's modulus of carbon steel is normally 200 GPa (29,000,000 psi).
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.
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:
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
4𝑀𝑤𝑖𝑛𝑑 𝑊
𝜎𝑐𝑜𝑚𝑝𝑟𝑒𝑠𝑠𝑖𝑣𝑒 = 2 ×𝐿 + 𝜋𝐷 , Where all symbols have usual meanings.
𝜋×𝐷𝑠𝑜 𝑠 𝑠𝑜 𝐿𝑠
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
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.
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.
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.
66
Figure 8-4-Wafer Type Butterfly Valve Figure 8-3-Tee Pattern Globe Valve
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.
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
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.
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.
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.
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.
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.
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
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-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
V-05 Y-04
P-04
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.
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.
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.
9.5.1 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.
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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.
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
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.
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.
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.
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)
80
Table 40-HAZOP Study of the 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).
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,
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
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
The heat load required to heat up feed in – Qfeed= 15943.62 ×2.02× (222-30) = 6183.5 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)
By using graph,
𝑃𝑢𝑟𝑐ℎ𝑎𝑠𝑒𝑑 𝑐𝑜𝑠𝑡, $ = $ 400000
𝐹𝑐 = 𝐹𝑑 + 𝐹𝑚 + 𝐹𝑝 = 1 + 0 + 0 = 1
87
11.5 Total capital cost of the distillation system
Table 41-Total Capital Cost Calculation
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
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.
91