CE 3003 Advanced Process Design - Individual Project: Executive Summary

CE 3003 Advanced Process Design Individual Project
EXECUTIVE SUMMARY:
The main objective of this project was to carry out a design on the Propane
distillation column for a process that produces 1,3 Butadiene. The raw materials
used are Butane, Oxygen and Water and the process capacity is 100 000 tonnes
per annum nominal. In the previous work it was stated that the plant is located
in China. The main location of the plant is in the capital city of the Gansu
Provence, Lanzhou. This was decided as the location over other provinces due to
the excellent transport links and the availability of raw materials and cheap
labour. The close proximity to suppliers, customers and skilled labour all make
Lanzhou the ideal location for the plant to be located.
The design of the distillation column consists of the packed type. The distillation
is a multi-component distillation involving separation of Propane from the other
components at very high pressure. The number of theoretical stages chosen was
16 stages based on a reflux ratio of 0.608. The column diameter calculated was
0.61 at maximum pressure gradient possible for distillation columns and 0.66m
for minimum pressure gradient, which was then scaled up to 0.65m. This was a
reasonable decision as it may be helpful when the plant capacity increases. The
column has a height of 8m. Feed location for the arrangement of packing is at
stage 3 from the top of the column. Pall rings constructed out of stainless steel
with a size of 25mm is used for packing. The vessel thickness of the column is
around 5mm, constructed out of stainless steel also to avoid corrosion.
A preliminary design on the condenser for this distillation column was also
carried out. The type of condenser is a fixed plate with a 1 shell and 1 tube pass.
The tubes are stainless steel, 119 in number, 2.44m in length, and with a square
pitch arrangement. The overall heat transfer coefficient was also calculated as
486.026W/m2C. The pressure drop on the tube side was 7.306 N/m2 (almost
negligible) as only one tube pass is used with a very short length. The pressure
drop on the shell side was 46.64 N/m2
The next section details on the Piping and Instrumentation over the column. The
control system used for better efficiency of the units is also featured in the same
Richie Gandhi Page 69

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P and ID.. The control mainly used for this, is the cascade control for the
temperature and product composition, also in the varying of the bottom product
flow rate to control the level at the bottom of the column. The variables
controlled are the top and bottom temperatures including product composition
and the reflux drum and also the level at the base of the column.
There were two group tasks performed in this term along with the individual
design. The first group task performed was the HAZOP on the feed line of the
propane distillation column. The aim of the HAZOP was to evaluate the selected
process line and identify the possible deviations which could result into a hazard;
the possible causes to the deviations, consequences and actions needed to
avoid the consequences were also discussed. An improvised P and ID was then
produced after Hazop was done. The Hazop was done with Dr. Titiloye as the
Study Leader. The deviations discussed include no flow, less flow, less
temperature due to weather conditions, more temperature likely to occur as a
result of external fire and extra phase in an event of poor separation, presence
of heat transfer fluids, presence of off gases, corrosion inside the pipe catalyst
pellets in the pipe and excess residue due which leads ultimately to
contamination.
The second group work is the economic appraisal, which was useful in
concluding that if this project were to be operational; the payback period would
be two years which would leave 13 years of net profit. So, from a financial
aspect, the project was found to be very viable and attractive.
Both the group works are attached in the Appendix VI and VII

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Contents
1.0 Project Brief:....................................................................................................5
1.1 Introduction to the product:.........................................................................5
1.2 Production:...................................................................................................6
[4]
1.3 Location ....................................................................................................7
2.0 Project Plan and Objectives:..........................................................................10
2.1Technical Objectives:...................................................................................10
2.2 Personal Objectives:...................................................................................12
2.3 Schedule....................................................................................................13
2.3.1Project Schedule...................................................................................13
3 The Revised Process:........................................................................................15
4 The Chemical Design:.......................................................................................17
4.1 Calculations:...............................................................................................20
4.1.1 Reflux ratio and the number of Theoretical Stages..............................21
4.1.2 Determination of the Diameter of the Column:....................................28
4.1.3Feed Location:.......................................................................................31
4.2 Choice of Plates and Packing:....................................................................33
4.2.1 Types of Packing:..................................................................................34
4.3 Column Internals [21][22]:...............................................................................43
5.0 CONDENSER:.................................................................................................48
5.1 Energy Balance Over the condenser:.........................................................49
5.2 Shell Side Coefficient:................................................................................54
5.3 Tube Side Coefficient:.................................................................................55
5.4 Overall Heat transfer Coefficient U;...........................................................56
5.5 Shell side Pressure Drop:............................................................................59

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5.6Tube Side Pressure Drop:............................................................................63

6.0 REBOILER:.....................................................................................................65
6.1 Heat Duty over the Reboiler:......................................................................66
6.2 Choice of type of reboiler used with the Propane Distillation:[28]................67
7.0 Overall Energy Balance over the Distillation Column:...................................68
8.0 Piping and Instrumentation Diagram.............................................................69
8.1 Control Loop...............................................................................................72
8.2 Control Systems over the Distillation Column:...........................................73
9.0 Hazard and Operability Studies HAZOP.........................................................76
10.0 Conclusion:..................................................................................................77
11.0 References:.................................................................................................78
12.0 APPENDIX:...................................................................................................81
Appendix I........................................................................................................81
Appendix II.......................................................................................................81
Appendix III......................................................................................................81
Appendix IV......................................................................................................81
Appendix V.......................................................................................................81
Appendix VI......................................................................................................81
Appendix VII.....................................................................................................81

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1.0 Project Brief:
1.1 Introduction to the product:
Butadiene is a simple conjugated diene. It is

an important industrial chemical used as
a monomer in the production of synthetic
rubber. Butadiene at most of the times
refers to 1,3-butadiene. 1,2-butadiene,
which is a cumulated diene is an isomer
which is difficult to prepare and has no
industrial significance.[1]
1, 3 Butadiene (CH2=CH-CH=CH2), is a colourless gas with mild aromatic odour.

Butadiene is soluble in alcohol and ether, insoluble in water and polymerizes
readily, particularly if oxygen is present. It is non-corrosive and has a molecular
formula of 54.09. Its boiling point is -4.4C and its vapour pressure is 1,790 mm
Hg (239kPa) at 20C. It is easily liquefied, with a density of 0.6211 g/ml at 20C. It
is soluble with ethanol, diethyl ester, and organic solvents and very slightly
soluble in water. 1, 3 Butadiene has a flash point of -76C and can slowly be
dimerised and may form peroxides upon exposure to air. Because 1, 3 Butadiene
is a highly volatile gas, it is expected to partition in the atmosphere and then
[1]
undergo rapid destruction by photo-initiated reactions.
A table of properties can be seen in Appendix I section (a)
In 1863, a French chemist isolated a previously unknown hydrocarbon from

the pyrolysis of amyl alcohol.[1] This hydrocarbon was identified as butadiene in
1886, after Henry Edward Armstrong isolated it from amongst the pyrolysis
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products of petroleum.[1] In 1910, the Russian chemist Sergei

Lebedev polymerized butadiene, and obtained a material with rubber-like
properties. This polymer discovered was too soft to replace the natural rubber in
many of its uses, especially automobile tires.
The butadiene industry originated during the World War II. Many of the
belligerent nations realized that in the event of war, they could be cut off from
rubber plantations controlled by the British Empire, and sought to remove their
dependence on natural rubber.
In 1929,Eduard Tschunker and Walter Bock, working for IG Farben in Germany,

made a copolymer of styrene and butadiene that could be used in
automobile tires. Worldwide production quickly ensued, with butadiene being
produced from grain alcohol in the Soviet Union and the United States and
from coal-derived acetylene in Germany.[1]
Butadiene is the raw material used [2] in the making of various synthetic rubbers
and polymer resins as well as a few chemical intermediates.
It is mainly used to make styrene butadiene rubber (SBR) which is used to make
automobile tyres. It is also used in adhesives, sealants, coatings and rubber
article such as shoe soles. SBR is has a high molecular weight, as it has
excellent resistance to abrasion, it is widely used in the automobile tyre industry.
Various other uses of butadiene are detailed in the table attached in Appendix I
Section (b).

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Figure 2: Chart Showing Various Uses of different forms of 1,3

Butadienehttp://www.sriconsulting.com/WP/Public/Reports/pie_charts/B
utadiene.gif
1.2 Production:
Butadiene is produced commercially by three main processes:[3]
Steam Cracking of Paraffinic Hydrocarbons: In this process, butadiene is a
co-product in the manufacture of ethylene (the ethylene co-product
process).
Catalytic Dehydrogenation of n-Butane and n-Butene (the Houdry process).
Oxidative Dehydrogenation of n-Butene (the Oxo-D or O-X-D process).
Each of these processes produces a stream commonly referred to as crude
butadiene that is rich in 1,3-butadiene.
In the United States, western Europe, and Japan, butadiene is produced as a by-
product of the steam cracking process which is used to produce ethylene and
other olefins. The quantity of butadiene produced depends on the hydrocarbons
used as feed. Light feeds, such as ethane, give primarily ethylene when cracked,
but heavier hydrocarbons favour the formation of heavier olefins, butadiene,
and aromatic hydrocarbons.
Butadiene can also be produced by the catalytic dehydrogenation of normal

butane. The first commercial plant, producing 65,000 tons per year of butadiene,
began operations in 1957 in Houston, Texas.

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In the previous project it was decided that Oxydehydrogenation Process would

be employed to produce butadiene for the plant to be built in China, which uses
Butene as the main raw material. Due to the easy availability of Butane from the
nearby industries, it was decided to integrate the process, where butane was
first decided to be catalytically dehydrogenated to Butnene and the O-X-O D
Process follows after that. The specification was not clearly illustrated in the
project earlier, and hence its now detailed further in this project.
1.3 Location [4]
Since 2002, the Global Butadiene industry has maintained relatively fast growth
especially in Asia due to its variety of uses. The global annual butadiene output
increased from 8.08 million tons in 2002 to 10.15 million tons in 2007, with an
average annual growth rate of 4.68%.
China is one of the fastest developing Asian countries in the world. Along with
the rapid development of china butadiene industry, the national output of
butadiene increased from 725,000 tons in 2001 to 1.36 million tons in 2007, with
an average annual growth of 9.4%. Even after increase in production, China has
to import huge quantities of butadiene from different countries. Korea is the
biggest supplier of butadiene to china.
Figure 3 : graph to show Production Capacity and Output of Butadiene

in China, 2001-2008 (Unit: 10,000
tons)http://www.researchinchina.com/UpLoads/Article/2008112601.gif

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It was decided that the best place locate the butadiene plant in China which can
satisfy the demands of its market in near future is in Lanzhou, the capital of the
Gansu province which is in north western china.
Figure 4: Map of Gansu Province in China

i
http://janetong.com/image_gallery/data/agansubest.jpg
While deciding the plant location several factors were taken into consideration:
Productivity - Since 1949 Lanzhou has been transformed from the capital of
a poverty-stricken province into the centre of a major industrial area. The GDP
per capita of Lanzhou was 25,566 Yuan (RMB) (US$3,681) in 2008, ranked no.
134 among 659 Chinese cities.
River - Lanzhou is situated at the upper course of the Yellow River. The river can
provide water to the plant as the process requires large quantities of water for
scrubbing and cooling. Also the river provides hydropower to the industries and
cities in Gansu. A large multipurpose dam has been built in the Liujia Gorge on
the Yellow River above Lanzhou. The river also helps in transportation.
Natural Resources - Lanzhou has many natural resources which include coal,
gold, silver, nickel, manganese, clay and dolomite. The Coal is obtained from
Qinghai which provides thermal power. The catalyst for our process is nickel
which will be cheaper to buy and will be available in large quantities.

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Cheap Labour - Due to the presence of the Yellow river the site is a residential
area for more than 3.3 million people. Cheap labour is available for the plant.
There are many top ranked universities in this province which means qualified
staff will be available at the site.
Industrial area - Gansu has one of the largest oil refineries in the country and
Lanzhou itself is the centre of the province's petrochemical industry. The main
industries include rubber, petrochemical, oil refinery and machinery industry.
Butane which is the raw material for our process is readily available and also
Butadiene (product) can be sold to the neighbouring industries. Also, the
machinery parts will be available from the neighbouring industries which will
reduce the cost of transportation and energy and time.
Transportation - Lanzhou is very well interconnected to various cities and

provinces through highways, railways and airlines. There are 3 major national
highways namely China National Highways 212,213 and312, connecting
Lanzhou to different provinces of the country. Transportation is cheap and easy.
The Lanzhou Sustainable Urban Transport Project in China aims at improving the
transport infrastructure and urban road networks. The total Asian Development
Bank contribution is estimated at US$150 million. This project is under planning
and is expected to get its approval by 11 th Dec; 2010.This will greatly enhance
the transportation of our product to different provinces when our plant is ready
for production.
2.0 Project Plan and Objectives:

The Second part of this project aims at carrying out a design study on a selected
process section for the production of 100 000 tonnes per year of 1, 3 Butadiene
from Butane for a plant to be built in China.
Project Supervisor: Dr. James Titiloye
Project Author: Richie Gandhi

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The process development project aims to give third year Chemical Engineering
students a chance to experience what working on a project in an industry might
be like. Working in groups, they must cover all the major areas involved in
designing a process. The main process unit which has been discussed in this
project is a Distillation Column which separates Propane from 1,3 butadiene.
Within this task other objectives have been set to ensure that the goal is met
which are outlined below:
2.1Technical Objectives:
Chemical engineering design to achieve the following outcomes is to be

done
Understanding solving a complex engineering design problem
Design a distillation column according to the engineering standards
To design a distillation column to meet the desired criteria
Gain an understanding of chemical engineering unit operations
Description of a control system for the distillation column for best possible
results is to be done
To study concepts of process control including principles of feedback
and feed forward, apply these concepts to the design of
instrumentation and control system for a distillation column.
Propose a control system which will execute the desires of the process
functionality
Piping and Instrumentation Diagram for the distillation column is

obligatory
Exhibit an understanding of engineering codes, standards and
regulations
Develop skills through use of computer software such as Microsoft Visio
Carry out a group study on the HAZOP for any one of the individual
selected processes to achieve the following outcomes
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To be able to investigate how the chemical plant might deviate from the
design intent
To be able to identify scenarios that would lead to the release of
hazardous and flammable materials to the environment and also to
determine whether a particular deviation would result into an hazard
Work effectively in a team to achieve the project goal
Economic appraisal (group work) for the full process on production of 1,3
Butadiene in order to gain the following outcomes
Work effectively in the group to enhance team work skills
To estimate the costs and benefits of production of products using the
desired process route
To study the economic feasibility of the production of products
Written report preparation based on the selected design to achieve the following
Assemble and use relevant background information
Provide Complete Referencing
Appendices containing lengthy derivations, calculations, large drawing,
computer printouts etc.

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2.2 Personal Objectives:

Understanding how chemical process work: Upon completion of this
project, a better understanding of the Butadiene process will be gained.
Also technical skills in carrying out a detailed distillation column design
study will be improved, which will help towards future projects as a
chemical engineer.
Enhance organisational skills and keeping to deadlines: The tasks would

be scheduled at regular meeting with the supervisor where the deadlines
will be decided which have to be met for a successful project.
To utilize our initiative: Many decision making processes will be used in the
undertaking a couple sections of this project. Each member will need to
use their initiative to come to a sensible and reasonable conclusion, which
will benefit the entire group.
Develop Communication Skills: Communication skills are enhanced both

by meetings with the supervisor and the group meetings. This would
provide and individual a platform to build his confidence and propose his
ideas.
Enhance Team-working Skills: HAZOP and Economic Appraisal have to be

carried out as a group. The group members are required to co-operate
with each other, share and listen to ideas and take constructive criticism
from group members. This will encourage each member to provide advice
and feedback.
Professional report writing: At the end of our project I wish to able to

deliver a professionally laid out report.

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2.3 Schedule
To support me in achieving these objectives a schedule has been devised to plan
the project and ensure that all required tasks are undertaken, within the time
period set for the study to be completed. This can be seen below. A Gantt chart
is also attached for assistance in the Section 3(b) in the Appendix II. This is the
revised Gantt Chat according to with the schedule has actually been carried out.
A Gantt chart which was made earlier to aid in maintain time is attached in
Section 3(a) in the Appendix II
2.3.1Project Schedule
Serial
No. Objective Start End
Date Date
Get feedback on
1 report/presentation and mass and
energy balance from Dr. Titiloye 19/01/1 22/01/1
Submit project plan. 0 0
2 Tutor meeting and discussing the

topic. 25/01/1
Gathering relevant information 0 29/01/1
from 1st term project 0
3 Discuss findings with tutor

Put together a list of all the 01/02/1 07/02/1
equations required to design a 0 0
Distillation Column for the process
Start Designing the Distillation
Column in the Butadiene
production process.

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4 Calculating diameter and size of 08/02/1 19/02/1

Distillation Column along with the 0 0
flow though them thereby
completing the design
Review the mass balance and 22/02/1 5/03/10
calculating other dimensions 0
5 Piping and instrumentation 1/03/09 10/03/1

diagram 0
Control and instrumentation
research
Calculating cost and profit
6 HAZOP 10/03/1 19/03/1

0 0
7 Calculating cost and profit 01/03/1 15/03/1

Economic appraisal 0 0
8 Completing referencing 25/01/1 17/03/1

Executive summary 0 0
13/03/1 17/03/1
0 0
9 Ensuring completion of all section 20/03/1 21/03/1

Submit report 0 0
Review with tutor
Make changes
10 Proof read 22/03/0 26/03/0

Submit report 9 9

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To complete the objectives of the project various sources would be utilised for
research work. The main source of information used will be university library,
Birmingham city library, Aston Universitys access to online journals, internet
and contacting companies in relation to scope of the project. Discussions would
be carried out with Dr. Titiloye to check the track of the work and to ensure
correct research is carried out.
3 The Revised Process:
[3]
Phillips OXO-Process
The n-butene, steam and air react at 590-650C on a fixed bed heterogeneous
catalyst (probably a ferrite (iron or iron alloy) with Zn, Mn or Mg). Addition of
steam controls the selectivity. With butane conversions between 75-80%, the
butadiene selectivity reaches
roughly 88-92%.
Magnesium ferrite
C4H8 + O2 C4H6 + H2O..................................(1)
1 bar / 590-650C
It is a one step process, where Butene gets oxidised straight away, without the
need of butane dehydrogenation. Since our plant is close to an oil refinery plant,
where butane can be obtained at a cheaper price in abundance, a decision to
integrate the conversion of Butane to Butene in our process was made. This
reaction would take place in the first reactor and then the produced butene is
fed into the second reactor for further processing. The catalytic
dehydrogenation of Butane to Butene is not a part of our OXO process
which we had considered in the previous report.[3] The same method
was carried out in the first project, but it was not stated clearly stated
in literature.
Tubular Rector
C4H10 + O2 C4H8 + H2O.................................(2)
1Atms/5900C
Cromina-Alumina

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Equation (1) gives 100% completion; higher conversions at lower temperatures

are possible with fewer side reactions and improved yields. It is also easier to
remove the hydrogen as it is now present as water vapor and can be condensed
out. It is an exothermic reaction; heat input to the reactor is thus eliminated as
heat is recovered to generate high pressure steam. By feeding stream and air to
the reactor it is possible to carry out continuous in-situ catalyst regeneration.
The steam also absorbs some heat released by a small amount of hydrocarbon
oxidation and has a beneficial effect on butene selectivity to butadiene. In
general, the equipment used is smaller and utilities usage is reduced for a given
throughout compared with the conventional dehydrogenation process. A typical
flow goes from the feed stream, with a composition of butene feedstock, 90% n-
butene, 5% butane, 2% of small amounts of Hydrocarbon and 1% Butadiene. Air
is compressed and mixed with steam before heating in a furnace at 480-590C.
This mixture is then blended with butenes and passed over the oxidative
dehydrogenation catalyst bed in the reactor. Three reactors are used in parallel
(multitubular reactor) with a fixed bed of mixed oxide catalysts, feeding into a
single stream recovery and purification train. The products from the reactor are
cooled. Heat is recovered from reactor effluent with water sprays and can be
used to generate process stream. After quenching, Stream is cooled to about
400C, by direct contact with cold water. Cooling the stream causes
condensation, the condensate being removed by a simple phase separation.
Washing and scrubbing occurs in order to remove all water-soluble impurities,
the C4 fraction is recovered in an oil absorption section. The mineral oil absorber
has the ability to absorb the hydrocarbon components of the stream, in this case
the butadiene whilst rejecting gases such as nitrogen, carbon dioxide. The fat oil
is stripped and crude butadiene is transferred to the final purification step. The
product is then obtained from the tailing column which is then fed into the
recovery unit. Small amounts of oxygenated compounds are also produced and
these are separated and taken to a waste disposal unit. Water sprays are used
to reduce fouling in the plant.
The advantages for this process are that the catalyst life is long which lasts for
around 1000 hours. The capital costs compared to the other oxidative

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dehydrogenation process routes are more favorable because of the low steam
requirements for the mixture and the relatively high concentration of butadiene
leaving the reactor. Reactors are set up to de-coke the catalyst and restore its
activity, and to allow more effluent output of butadiene. At high temperatures
(up to 6000C), oxygen acts to oxidatively regenerate the catalyst. Also there are
a class of metal Vanadate catalysts that are newly being used, which has highly
selectivity and high conversions and the formation of oxygenated by-products is
suppressed. The feedstock raw materials are inexpensive in the United States; a
major factor causing this is the trend towards greater usage of feedstock such as
natural gas liquids (ethane, propane). However, there is a growing shortage of
these raw materials, encouraging the use of heavy feedstock such as ethylene.
During this process, various by products are produced. These by-products must
be removed to produce butadiene, so it can be polymerised. One major by
product is vinyl acetylene, which is a highly unsaturated compound, a poison for
the catalysts that polymerise butadiene. Therefore there is a need to produce a
purification process by providing a stream with distillation steps. This allows the
process to be energy-conserving and simple.
A revised Flow Sheet is attached in Appendix III. A compressor is added after the
extractive distillation column, in the new flow sheet that increases the pressure
of the process before it can be sent to the Propane Distillation Column for further
purification.
I assume the mass balance to be correct as it was based on many assumptions
which were acceptable. A Copy of the Mass Balance done in the previous project
is attached in Appendix IV.
4 The Chemical Design:

The design chosen for this project is a continuous distillation column. The
separation of the liquid mixture by distillation depends on differences in volatility
between the components. The separation becomes easier if the differences in
the volatilities between the components are massive. Figure 5 shows a basic
distillation column. The liquid mixture is heated up and routed into the
distillation column. The feed when enters the column flows down. Heat is

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vaporise the volatile components is provided by the reboiler. The components

with lower boiling points vaporise and rise to the top of the distillation column.
Vapour flows up and the liquid flows counter currently down the column. These
two phase come in contact with each other on a surface which can be trays or
packing. The composition of the vapour above the liquid differs from the liquid
composition. The vapour is then separated and condensed into a liquid; it
becomes richer in the lower boiling component(s) of the original mixture.
Part of the condensate from the condenser is returned to the top of the column
which provides liquid flow above the feed point and part of the liquid from the
base of the column is vaporised in the reboiler and returned to provide vapour
[5]
floe rate.
Figure 5: Basic Distillation Column

http://wpcontent.answers.com/wikipedia/commons/e/e0/Distillation_Col
umn.png
The highlighted distillation column in the flow sheet in Appendix III is the
Propane/Butadiene distillation column which is considered to be designed. The

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main objective of this unit is to get rid of propane from the process. The
distillation is a multi-component distillation thereby it involves more than two
components. It operates at very high pressure of 13.5 bars and consists of three
streams. The feed enters the distillation column at a temperature of about 350C.
On distillation, the Propane vapour leaves the top of the column to the
condenser and collected in the reflux drum. Partial amounts of 1,3 Butadiene is
also lost at the top of the column. The bottom product majorly comprises of 1, 3-
Butadiene, 1, 2-Butadiene and Pentane.
The table below shows the preliminary Mass Balance over the Distillation
Column
Table 1 (a): FEED:
Kmols/hr Kmols
Components Flow rate (kg/h) fraction
Propane 424.23 9.64 0.04
1,3 butadiene 11904.76 220.46 0.91
1,2 butadiene 500.00 9.26 0.038
Pentane 138.84 1.93 0.008
Total 12967.83 241.29 1
Table 1 (b): Distillate:

Components Flow rate (kg/h) Kmols/hr Kmols fraction
Propane 424.23 9.64 0.687
1,3 Butadiene 237.6 4.4 0.313
Total 661.83 14.04 1
Table 1 (c): Bottom:

Components Flow rate (kg/h) Kmols/hr Kmols fraction
1,3 Butadiene 11667.16 216.06 0.951
1,2 Butadiene 500.00 9.26 0.041
Pentane 138.84 1.93 0.0085
Total 12306.00 227.25 1

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The boiling points of the feed components at 1 atmospheric pressure are as

below:
Propane: 42.09 C
1,3 Butadiene: -4.4 C
1,2 Butadiene: 10.8 C
Pentane: 36.1 C
Looking at the temperature differences it can be said that the components can
be separated easily by reducing the temperatures but since in tangible
situations, it is very expensive to reduce down the temperatures in the plant for
continuous process we have to increase the pressure inside the unit to separate
it at reasonable costs. This is done by using compressors or pumps before the
feed is fed into the unit.
It is assumed that the distillate is at a temperature of 400C which is a reasonable
assumption as chilled water can be used to cool down the components in the
distillate. Taking this as our basis we can calculate the pressure and temperature
for rest of our unit using Antoines Equation. Detailed calculations are attached
in Appendix V; Section (a)
4.1 Calculations:
Basis: 1hr
Units: 1 Kg
Propane boiling point: 40C/313K @ 13.5 bars
Specifications

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Feed condition: Cold Liquid under pressure

Feed inlet temperature @35C/308K
Temperature of Top of distillation column @ 45C/318K
Temperature of Bottom of distillation column @ 95C/368K
Therefore column Temperature will be taken as the average @ 70C/343K
The detail distillation design was performed by using the main steps below
- Determination of reflux ratio and number of stages required for the
distillation
- Calculation of the column diameter and determining the type of column to
be used, Packed or trays
- Column design in detail
4.1.1 Reflux ratio and the number of Theoretical Stages

The vapour reaching the top of the column is totally condensed and the resulting
liquid is divided into two parts. One part, L (reflux), is returned to the column
and the other part, D (distillate), is withdrawn as product. The reflux ratio is the
[6]
ratio of L to D, that is R = L/D.
Smaller values of reflux ratios means less the number of theoretical stages in
the distillation column increases, which reduces the energy costs as most of the
vapour is condensed as distillate and only partial amounts of reflux is sent back
to the column.
The minimum reflux ratio and the infinite reflux ratio place a constraint on the
range of separation operation. Any reflux ratio between Rmin and Total R will
produce the desired separation, with the corresponding number of theoretical
stages varying from infinity at Rmin to the minimum number (Nmin at Total R). The
relationship between R and N is shown in the Figure below. The choice of reflux
[7]
ratio to use is governed by cost considerations

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Figure 6: Generalised graph between number of theoretical stages V/S

Reflux Ratio
http://www.separationprocesses.com/Distillation/DT_Chp04n.htm
Calculations:
[8]
The minimum reflux ratio is calculated by using Underwood method.
A x fA B x fB C x fC D x fD
+ + + =1q .(1)
A B C D
A x dA B x dB C x dC D x dD
+ + + =1+ R (2)
A B C D min
Since the minimum reflux is calculated for a distillation column which consists of
four components, four variables are used in the above equation. For a multi-
component mixture to be split into two streams (distillate and bottoms) by
distillation, it is common to specify the separation in terms of two key
components of the mixture. Hence in this way multi components can be
reduced to equivalent binary systems.
Light Key: Most Volatile component in the Bottom Product

Heavy Key: Least Volatile component in the Top Product. [8]
Hence, from the table 1 (b) and (c);
Heavy Key (HK) 1,3 Butadiene

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Light Key (LK) 1,3 Butadiene

This will cause a problem in the calculation, since both the HK and LK are the
same component therefore an unreasonable reflux ratio will be obtained.
Therefore to trounce this problem, a small amount of Propane was added to the
bottom product, making Propane the LK.
I assume that 99% mole of propane and 2% mole of 1,3 Butadiene is now in the
Distillate and the remaining are the bottom product.
Revised Balance over the distillation column is as follows:
Table 2 (a); FEED
Feed
Componen Flow rate Kmols/hr Kmol
ts (kg/h) Fraction
Propane 424.23 9.64 0.04
1,3 220.46 0.91
butadiene 11904.76
1,2 9.26 0.04
butadiene 500.00
Pentane 138.84 1.93 0.01
Total 12967.83 241.29 1
Table (b); Distillate and Bottoms

Distillate Bottoms
Componen Kmols/hr Kmol Kmols/hr Kmol
ts Fraction Fraction
Propane 9.544 0.684 0.096 0.0005
1,3 4.41 0.316 216.05 0.95
butadiene
1,2 - - 9.26 0.041
butadiene
Pentane - - 1.93 0.0085
Total 13.954 1 227.336 1
Therefore new key components are:

HK 1,3 Butadiene
LK Propane

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The next step is to find the relative volatilities of each component with respect
to the HK which in this case is 1, 3 Butadiene. The calculations are attached in
the Appendix V, Section (b) and are tabulated below:
Table 3:
Components
Propane =2.724
1,3 Butadiene = 1
1,2 Butadiene = .66
Pentane = .31
Using the UNDERWOOD EQUATION:

Propane x fPropane 1,3Butadiene x f 1,3 Butadiene 1,2 Butadiene x f 1,2Butadiene Pentane x fPentane
+ + + =1q
Propane 1,3Butadiene 1,3Butadiene Pentane
Where q 1 as the feed is cold liquid @ 35C.
Calculation of feed condition q[9]:
Heat
q= vapourside 1 mol of feed .(3)
molar latent h eat of t h e feed
Therefore,
mc p T + m H vapuorisation
q= ( 4)
m H vapuorisation
Table 4: Latent Heat of the Components inside the Column [9]

Components Latent Relative Calculation Latent Heat
Heat in Molecular in KJ/Kmol
KJ/Kg Mass
Propane 229.93 44 229.93*44 10116.92
1,3 335.55 54 335.55*54 18119.7
Butadiene
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1,2 387.38 54 387.38*54 20918.52

Butadiene
Pentane 333.24 72 333.24*72 23993.28
Latent Heat = (10116.92* 0.04) + (18119.7* 0.91) + (20918.52* 0.038) +

(23993.28* 0.008)
Latent Heat = 17880.454 J/mol or KJ/Kmol
[9]
Table 5: Specific Heat of the Components inside the Column
Components Specific Heat
in KJ/KmolK
Propane 81.84
1,3 138.78
Butadiene
1,2 136.08
Butadiene
Pentane 182.88
Specific Heat to Vaporize the 1 mol of feed = mcpT + mHvapuorisation

=> {[(81.84*0.04) + (138.78*0.91) + (136.08*0.038) + (182.88* 0.008)] * (70-
35)] } + 17880.454 J/mol
Specific heat to Vaporise 1 mol of feed to 70oC = 4766.79 J/mol + 17880.454
J/mol
Therefore, Specific Heat = 22647.244 J/mol
22647.224
q= =1 .267
17880.454
q = 1.267
Using the above value of q in the Underwood Equation (1), is obtained;
2.7240.04 10.91 0.660.04 0.310.01

+ + + =11.267
2.724 1 0.66 .31

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Therefore; by using excel spread sheet:

= 2.67; which is acceptable as the value for should lie between the values
obtained for relative volatility of heavy key and light key.
Next, proceed to calculate Rmin.
Propane x fPropane 1,3Butadiene x f 1,3 Butadiene

+ =1+ R
Propane 1,3Butadiene min
2.7240.04 10.91
+ =1+ R
2.7242.67 12.67 min
Rmin +1=1.468, therefore Rmin = 0.468.

Reflux ratio is generally between 1.1 -1.5 times the minimum reflux ratio based
on practical values but there is no relationship between Rmin and the optimum
value.[8]
R = 1.1*0.468= 0.515
[11]
To find the number of theoretical stages using FENSKE EQUATION
x LK x HK
log
x HK d x LK w
N m= ..(5)
log LK
0.684 0.95
log
0.316 d 0.0005 w
N m= = 8.30(approximately 8)
log 2.724
Therefore,
R 0.515
= =0 . 34 ... ..(6)
R+ 1 0.515+1
R min 0.468
= =0 . 319 .(7)
R min+1 0.468+1

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From CHART Erbar-maddox correlation in the figure below we have,
Graph 1: Ebbar Maddox Correlation
Nm
=0.4 .. ...(8)
N
8
=0.4
N
N= 20 theoretical stages
Table 6: Number of theoretical stages at different Reflux Ratios
R R/R+1 Nm/N N
1.1*0.468 = 0.34
0.515 0.4 20
1.2*0.468 = 0.36
0.562 0.42 19
1.3*0.468 = 0.39
0.608 0.49 16
1.4*0.468 = 0.4 0.53 15

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0.655
1.5*0.468 = 0.41
0.702 0.55 15
1.6*0.468 = 0.43
0.749 0.58 14
From the above observations it is clear that increasing the reflux ratio reduces
the number of stages. But it is seen that increasing the minimum reflux ratios by
1.4 to 1.5 does not changes the number of theoretical stages.
There are two options available to decide which reflux ratios could be used in
our design. Either a line can be drwan from the origin of the graph as shown
below which means that the best available technique is a mid way between the
number of stages and the reflux ratio or this can be debated on the basis of
economic costs.
Figure 8: Selection of Reflux ratio and the number of stages

http://www.separationprocesses.com/Distillation/DT_Chp04n.htm
The increase in the reflux ratio reduces the number of stages in a distillation
column. But energy costs shoot up which has to be considered as well. Since the
Distillation column is almost running for (350 days* 15 years) approximately, it
is not a good option to run the column at high reflux ratios. But if very low reflux
ratios are opted, the metal costs to build the column go up. The reflux ratio
chosen for the process is 1.3 Rmin. I have decided to use a reflux ratio of 0.608
which requires reasonable costs and the number of stages are also acceptable. [8]

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If the Feed is assumed to enter the column at its boiling point there is a huge
difference in the reflux ratios
4.1.2 Determination of the Diameter of the Column:
FAIR CORELLATION (1961)[10] is used to calculate the diameter of the column. To

find the diameter, velocity of the fluids has to be calculated. The calculations are
detailed below:
Internal Traffic [11]:

L =RD ; 0.608*661.83 = 402.39kg/hr
L = L + qF ; 402.39+(1.267*12967.83) = 16832.63 kg/hr
V = L+D ; 402.39+661.83 = 1063.22 kg/hr
V = V (1-q)F ; 1063.22 (1-1.267)* 12967.83= 4525.63 kg/hr
FLV = L/G (V/L)0.5 [18]
where;
L = Liquid mass flow rate, kg/s
G = Vapour mass flow rate, kg/s
Vapour density, kg/m3 = V
Liquid density, kg/m3 = L
The calculation of L and v (see section (C) of Appendix V)
L = 599.69 Kg/m3 and v = 30.324 kg/m3
The Flooding correlation is calculated at both the sides of the column because it
can be a stepped column.
Therefore, the flooding correlation above the feed
0.5
L v
F LV = ( ) ..(9)
G L
402.39 30.324 0.5

F LV = ( ) =0.085
1063.22 599.69
Using the CHART flooding velocity, sieve plates, in Graph 2 and taking a
generalized plate spacing of 0.6m:

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Graph 2: Flooding Velocity Sieve plates
K1 (top) = 0.1
The velocity can now be calculated by;
( L V ) 0.5
u f =K 1(top)[ ] .(10)
V
Hence,
0.5
(599.6930.324)
u f =0.1[ ] =0. 4333 m/ sec
30.324
Taking percentage flood @ 80% based on good design considerations, therefore

velocity @ flooding:
uf (top) = 0.8*0.4333 => 0.34664 m/sec

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Maximum Volumetric Flow Rate:
1063.22 Kg/h r
Top= =9 . 74103 m3 / sec
(30.324 Kg/m33600 sec /hr )
Net Area Required

Volumetric Flow Rate
A= .( 11)
Velocity
3 3
9.7910 m /sec
A= =0 . 028 m2
0.34664 m/sec
Allowing 10% for down comer and 10% for support rings;
There total area = 0.028*1.1*1.1 = 0.034 m2
Hence column diameter above the feed point;
d=
A4

=

0.0344

=0 . 21m
Similarly for the lower section of the column;
16832.63 30.324 0.5

F LV = ( ) =0.84
4525.63 599.69
Using the CHART flooding velocity, sieve plates in Graph 2; taking a generalized
plate spacing of 0.6m:
K1 (bottom) = 5*10-2
The velocity can now be calculated by;
(599.6930.324) 0.5
u f =0.05[ ] =0 .21665 m/sec
30.324

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Taking percentage flood @ 80% based on good design considerations, therefore

velocity @ flooding:
uf (bottom) = 0.8*0.21665 => 0.17332 m/sec
Maximum Volumetric Flow Rate:
4525.63 Kg/hr 3
Bottom= =0 . 041 m /sec
(30.324 Kg/m 33600 sec/ h r)
Net Area Required

3
0.041m / sec
A= =0 . 237 m2
0.17332 m/sec
Allowing 10% for down comer and 10% for support rings;
There total area = 0.237*1.1*1.1 = 0.288 m2
Hence column diameter below the feed point;
d=
A4

=

0.2924

=0. 61 m
4.1.3Feed Location:
The number of stages is greatly affected by the subsequent position of the feed
into the column. The feed should enter the column at a point that matches best
with the composition of the feed. It is always a wise decision to provide two or
three feed point nozzles around the predicted feed point which will account for
the changes in the feed compositions after the start up.
The propane Distillation column is operating under high pressure. Hence, the
feed is either compressed or pumped into the column. It can be made to
compress to a slightly higher pressure into the feed pipe, approximately 14 bars,

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so that when it enters the column which is slightly at a lower pressure than the
pipe, some of the propane from the components will immediately expand and
undergo a partial flash vaporisation resulting in vapour liquid separation as it
enters the distillation column.
4.1.3 Calculation of the Feed Position:
Krickbride(1994)[13] can a practical equation to calculate the feed point location
[ ]
B
x 2
Nr D fHK x bLK
log =0.206 log (12)
Ns x fLK x dHK
Where,
Nr = number of stages above the feed, including any partial condenser
Ns = number of stages below the feed, including the reboiler
B = Molar Flow Bottom Product
D = Molar Flow Top Product
XfHK = concentration of the heavy key in the feed
XfLK = concentration of the light key in the feed
XbLK = concentration of the light key in the bottom product
XdHK = concentration of the heavy key in the Distillate
Therefore, by substituting the values in the above equation;
[ ]
277.336
0.91
Nr 13.954 0.0005 2
log =0.206 log
Ns 0.04 0.316
Nr
log =0.607
Ns

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Nr
=0.2472
Ns
This can also be rewritten as;

N r =0.2472 N s
......................(A)
Since the total number of stages being used is 16,

Therefore;
N r + N s=16 ..( B)
Substitution the value of Nr from Equation (A) in equation (B),

We get, Ns = 12.8 ( 13) which means, there are 13 stages below the feed
position which includes the reboiler as well.
Since, the feed location is almost at the top of the column leaving 3 stages, the
design of a stepped column is pointless. It is made with an overall diameter of
0.6m.
4.2 Choice of Plates and Packing:
The calculated value for the distillation column is approximately 0.6 m. The
choice between packing and trays was made on the basis of advantages and
disadvantages of each type, and it is concluded that a PACKING would be best
[14]
for such small diameters. This decision was made because:
Plate columns are generally designed to handle wider range of vapour and
liquid flow rates than packed columns. Since the gas flow rates in the top
of the column is minor, plate installation would not be a good idea.
Packed columns are not suitable for very low liquid flow rates.
The pressure drop per equilibrium stage (HETP) is lower for packing than
plates. Since, the column is operated at high pressures; it would be a
better option to choose packed column rather than plates to avoid
complications.

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Packing should always be considered for smaller diameters, generally for

column diameters >0.9m as it is very expensive and difficult to install
plates in such columns.
After the decision is made, the design over the packed column has to be done.
[14]
This includes the following procedures:
The type and packing size has to selected corresponding to the diameter
of the column
Determining the height of the column required for the desired separation
Calculation of the column diameter (capacity), to handle the liquid and
vapour flow rates.
Selection of column internal features like; packing support, liquid
distributor, redistributors.
4.2.1 Types of Packing:
[14]
A packing should always fulfil the following requirements:
Provide a large interfacial area between the gas and the liquid.
Should have an open structure for low resistance to gas flow.
Should provide consistent liquid distribution on the packing surface
Promote unvarying vapour gas flow across the column cross section
Hence, keeping the above requirements into consideration, the packing is

broadly classified as
Structured Packing: These are packing with standard geometry made of
wire mesh or perforated metal sheets which are folded and arranged
together. Some metal structured packing commonly used in distillation
columns are shown in the figure 10. They have low height of equivalent
theoretical plates (HETP) and low pressure drops. They are generally used
in difficult separations which require many stages, like separating isotopes
or in high vacuumed distillation columns. Using structured packing can
also used to increase the capacity and reduce the reflux ratio
requirements.

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Figure 10: Structured Packing

http://img.alibaba.com/photo/50678452/Ceramic_Metal_Plastic_Str
uctured_Packing.jpg
Random Packing: These are variously shaped in rings, saddles etc, and
are dumped into the distillation column to take up a random shape. These
structures can be made up of plastics, ceramics and metals. The various
types of random packing are shown in figure 11 below. The packing
manufacturers should be consulted for details for many special types of
packing that are available for special applications.

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Figure 11: Various kind of random packing

http://img.alibaba.com/photo/50553772/Ceramic_Random_Packing.jpg
Raschig rings are the oldest types of random packing whose length is equal to
the diameter. These are cheaper compared to any of the random packing
structures but not as efficient as others.
These were then modified to Pall rings which have openings made by folding
strips of the surface into the ring. This increases the liquid distribution by
increasing the surface area.
Other types of random packing are, Berl Saddle Ceramic, Intalox Saddle
Ceramic, Metal Hypac and Super Intalox Ceramics.
Selection of Packing:
Type and Material [15]:

From the above information it would be cheaper to use Random Packing with
Metallic (Carbon-Steel) Pall Rings. This is because the column is operating at
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high pressures and has a very small diameter. Also the components inside the
column are non-corrosive. It would require too much effort and capital to install
structured packing inside the column which would separate the same amount of
propane. Also Ceramic pall rings can be considered, but they are more
expensive than the metallic ones.
Figure 12: Metallic Pall rings

http://www.pall-
ring.com/images/product/Chempack_metal_pall_ring_02.jpg
Packing Size [15]:

The largest size of packing suitable for any size of column should not exceed
more than 50mm. This is because the larger packing sizes would cause flooding
due to poor liquid distribution. Very small sizes are also available but are much
more expensive than the larger ones.
The sizes recommended for different column diameters are:
Table 7: Packing size depending on the Column Diameter
Column Diameter Packing Size
< 0.3m < 25mm (1inch)
0.3 m to 0.9m 25mm to 38mm (1inch to 1.5
inches)
> 0.9m 50mm to 75mm (2 inch to 3 inches)
Hence, for the Propane distillation column Metallic Pall rings with a size of
25mm is used.

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Column Diameter (capacity)[16]:

A distillation column is always designed to operate at height economical
pressure drop. This ensures good liquid and gas distribution. For random packing
the pressure drop normally does not exceed more than 80mm of H 2O/m of the
packing column.
A distillation columns design values for pressure gradients are between 40 -80
[17]
mm Hg/m packing. These values are almost halved when the liquid starts to
foam. The proposed design has a diameter of 0.61m with trays. Since random
packing is now considered a new diameter has to be calculated.
Pressure gradient over the enriching section using column diameter as 0.61m
A generalised pressure gradient/flooding correlation graph can be seen in Graph

3 below:
Graph 3: Graph to determine the Flooding Line

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Values for x and y axis can be calculated and the flooding line can be plotted
in the figure above.
X axis :
L
G g
L
(13)
Where,
L = Liquid Rate per Area
G= Gas Rate per Area
Since the area remains same; the ratio can just be taken as the normal flow
rates of vapours and liquids.
Hence;
X axis :

16832.22 30.524
4525.63 599.69
=0 . 839
Now,
2 0.2
G F p L
Y axis: (14)
v Lg
Where,
Fp = Wet Packing Factor; Appendix V; section (d)
= Ratio; (density of water/Density of Liquid inside the column)
L = Liquid Viscosity of 1,3 butadiene is considered in the calculations, as major
fraction of the liquid comprises of 1,3 Butadiene
g = Gravitational constant
Hence;
4525.634
36000.612

21601000
0.250.2
599.69

Y axis:

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From the Graph 3; the flooding line is calculated at 6, which is 81 mm

Hg/meter. This result is acceptable since the pressure gradient calculated
above, 6mm Hg, it is concluded that the system is expected to run at very
extreme pressure gradients.
The values of pressure gradients for the lower range over the distillation column
can be used to calculate a new diameter. Any of the values between the two
ranges can be used for the design.
From the same graph above a new value of Y is plotted at 40mmHg/m is now
calculated.
Hence the Flooding line would be,
40 mm Hg
=2.9 3 ..(15)
13.6 mm Hg
As 13.6 mm Hg is the specific gravity of mercury.

Y axis in now 0.015.
Again using Equation on the Y axis in Graph 3; a new gas flow rate per area is
calculated which would give the new diameter.

0.01530.324599.699.81
G= =3 . 64
1601000 0.2
0.25
599.69
Since,
V
G=
A
Therefore,
V 4525.63 2
New Area ( A )= = =0 . 345 m ..(16)
G 36003.64
Since the gas flow rate per area in decreased; the diameter has to be increased.

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Hence,
D=
A4

=

0.3454

=0.662m 0 .66 m
Since, the change in diameter is not drastic the packing used can still be
suitable for this diameter. The capacity of the column can be anything between
0.61m 0.66m depending on the flooding line.
Hence, it has been concluded that the capacity will be 0.65m; which can also be
helpful when the production capacity of the plant increases. The flooding like
can be changed accordingly.
Packed Bed Height:[18]

The heights of equivalent equilibrium stage or HTEP is the height of a single
packing which gives the same amount of separation as an equilibrium stage in a
trayed column. The HTEP is for a specific type of packing is usually constant and
is independent of the physical properties of the components. This provides good
liquid distribution and does not let the pressure drop fall below 17mm H 2O/m of
the packing height.
Table 8: The recommended HETPs for Pall rings

Size of the Pall Ring in mm HETP in m
25mm 0.4m 0.5m
38mm 0.6m 0.75m
50mm 0.75m 1.0
Hence, HETP for the propane distillation column is 0.5m as the size for pall rings
used is 25mm.
This means, one stage is 0.5m since there are 16 stages calculated earlier, total
height of the column = 0.5*16 = 8m
Flooding is prevented due to the tall height of the column.
Since the feed stream is put after 3 stages; the position of the feed stream is
(0.5m*3 stages) 1.5 m at the top and the length below it is 6.5 m.

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Choice of material used for construction:

The column is decided to be made up of stainless steel (18Cr/8Ni, Ti stabilised)
(321). Steel is a very strong metal with high ductility and high malleability which
can withstand high stress. Since the column has to with stand high pressures
and high temperatures, poor choice of material should not be used. Also the
column is very tall. Also stainless steel does not corrode. It is more expensive
than carbon steel, but it one time investment is affordable. Also the column is
required for purification purposes; hence any corroded metal in the product
would not be appreciated.
Thickness of the metal:

It is assumed that the column is cylindrical in shape. The welds are fully radio-
graphed. This column is operating at very high pressure of 13.5 bars. Hence, a
pressure has to be designed in such a way that the column resists the increase
in pressure due to equipment failure.
Internal pressure is designed at 10% above operating pressure.
= (13.5 1)* 1.1 => 13.75 bars (1.375N/mm2)
The thickness of the cylindrical section of the column can be calculated by a

formula from British standards PD 5500:
Pid i
e= .(17)
( 2 s ) P i
Where,
Pi = Internal pressure
s = Design Stress for stainless steel @ 1000C; Appendix V; section (e)
e = minimum thickness of the material
Hence,

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1.3750.651000
e= =2.99 mm 3 mm
( 2150 )1.375
Allow 1mm for corrosion;

Hence the thickness of the cylindrical section should be 4mm.
The thickness of the Domed Section of the column can be calculated by:
A standard dished head (torisphere) is

assumed;
Crown Radius, Rc = Di = 0.65 m
Knuckle radius = 6%of Rc = 0.039m
C s=
1
4( ) ( )
R 1
3+ c = 3+
Rk 4
0.65
0.039
=1. 77
A head of this size would be formed by pressing: no joints, hence, J = 1
Pi Rc C s
e= (18)
2 fJ + Pi (C s0.2)
Substituting, correct values in the above equation;
1.3750.6510001.77
e= =5 . 24 mm
(21501)+1.375(1.770.2)

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A tank diameter of less than 15m should have a minimum allowable thickness of
[16]
5mm . The thickness obtained from calculation would hold the weight of
content in the vessel, but would not stand depression or dent. Therefore, a 5mm
minimum allowable thickness was given for any vessel less than 1m because
this can withstand depression. Hence, the results obtained are acceptable.
Diameter and Thickness of the Pipes:

It is decided to use Pipes made of Stainless Less because they have high tensile
strength and are ductile. These twp parameters are matter much as the system
is operating at high pressures. The diameter is calculated by equation 19 [20] and
the thickness is calculated from equation 20[20]
For Stainless steel;
d ,optimum =260 G0.52 .37 .(19)
The thickness of the pipe; t

P do
t= (20)
20 d + P
The Feed Pipe:

0.52
12967.83
d ,optimum =260( ) 599.69.37 =47 . 48 mm
3600
And;
13.547.48
t= =0 .22 mm
(20145)+13.5
Pipe to the Condenser:

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1063.22
3600

d ,optimum =260
And,
13.539.02
t= =0 .18 mm
(20145)+13.5
Pipe to the Reboiler:

16832.63 0.52
d ,optimum =260( ) 599.69.37 =54 . 38 mm
3600
And,
13.554.38
t= =0 .252 mm
(20145)+13.5
4.3 Column Internals [21][22]:

The internal packing in a packed distillation column should be designed
carefully, to ensure better performance.
Generally, the standard fittings are developed by the packing manufacturers and
its uses are specified. Some of the typical designs are discussed as follows.

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Packing Support: The support

plate carries the weight of the
random structures inside the
column. A poorly designed of the
support plates causes flooding
or very high pressure drops
inside the column. A simple Grid
or a perforated plate support
can be used. The only
disadvantage with such kind of
support systems is that the
liquid and the gas have to vie
through the same openings.
Hence, wide spaced grids are used to avoid this problem and increase the flow
area. The larger sizes packing are dumped into the column first if wider grids are
used, which support the smaller random packing. (As shown in Figure 13)
The best design for packing

support is the gas injection
type of support. The gas inlets
are provided above the level
where the liquid flows from the
bed. The problem of local flooding
and high pressure drops is solved
with the application of these
support rings. These supports are
available in a variety of sizes and materials, like plastics, ceramics and metals.
Figure 14; shows design for the gas injection supports and Figure 15 shows the
Principle of gas injection packing support

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Liquid Distributors:
Uniform flow of liquid throughout

the column and good initial liquid
distribution is a very essential
factor for good performance of a
column. A central open feed pipe
or a pipe with a spray nozzle is
best suited for proper distribution
of liquid in small diameter
columns. But for larger
diameters, more elaborate
designs are required. The two
most common type of distributors
used are orifice type and weir type.
The orifice type has holes in the plate which allows passage for the liquid and it
has short stand pipes, through which the gas flows. Sizing of gas pipes are
compulsory as it provides sufficient area for the gas flow without letting the
pressure to drop significantly. The holes should be of an appropriate size, neither
too small nor too big so that at lowest liquid flow rate, there should be a level of
liquid always present on the plate and at highest flow rates, the liquid distributor
does not over flows. Figure 16 shows the C.S and the T.S of an orifice distributor.

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In the Weir types the liquid flows over the notched weirs in the gas stand-pipes.
These stand an upper grade over the orifice type in handling wider range of
liquid flow rates. The column designed uses Orifice type of distributor. A pipe
manifold distributor shown in figure 17 is used when the liquid is fed to the
column under pressure and the flow rate is reasonably constant. The distribution
pipes and orifices are accurately sized for equal uniform distribution.
Orifice
type is exploited in the propane distillation column.
Liquid Redistributors:
The main purposes of

redistributors are to collect
liquid that has moved to the
column walls and redistribute
it evenly over the packing also
redistributors will even out
any maldistribution that has
occurred within the packing.
A full distributor shown in figure 18 combines the function of packing support

and liquid distributor.

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The maximum bed height that should be used without liquid redistribution lies
solely on the type of packing and the process. The wall-wiper type is mainly
used in small columns of less than 0.6m in diameter. This operates in a
mechanism were a ring collects liquid from the column wall and redirects it into
the centre packing.
Hold Down Plates:

Fluidisation of the top layer of
packing can occurs due to high gas
flow rates or surging effects due to
mis-operation. The ceramic packing
crushes during such circumstances
but the metal and plastic packing can
be wafted out of the column. Bed-
Limiters are used for plastic and
metal packing to prevent to prevent
expansion of bed at higher pressure
drops.
These are similar to Hold Down plates. Such plates should have smaller grids to
retain the packing but not too small to restrict the fluid flow.
Installing Packing:
The column is filled with water and the packing is dumped into the water
ensuring the level of water always being above the packing at all times. Metal
and Ceramic packing are generally deserted into the column WET. This
ensures random distribution and prevents any damage to the packing.
In case of DRY packing the packing should be lowered into the columns in
buckets or other containers.
Concept Drawing:
The Concept Drawing Details the application of column internals more in detail.
Bit-Map is used to create the column showing every possible detail and
dimension. The non calculated values are assumed to British standards.

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5.0 CONDENSER:
Condensers are units similar to heat exchangers, which are used to condense
the vapours to their liquid state. Condensers vary in size ranging from hand
handled units to large industrial scale units.
For condensers used in distillation columns, the process fluid generally flows
through the shell side and the cooling fluid is made to flow through the tube
side. The two fluids never come in contact with each other. The diagram below
shoes a one tube pass condenser.
Figure 20: One pass tube side condenser

http://upload.wikimedia.org/wikipedia/commons/c/cd/Straight-
tube_heat_exchanger_1-pass.PNG
Four condenser configurations are possible:[23]

Horizontal, with condensation in the shell, and the cooling medium in the
tubes
Horizontal, with condensation in tubes
Vertical, with condensation in shell
Vertical, with condensation in the tubes

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Horizontal shell side and vertical tube side is widely used as condensers. The
other two are usually used in arrangements for heaters and vaporisers using
steam as the heating medium.
Assumptions:
It is assumed that a horizontal shell side condenser is used to cool the
propane vapours.
It is a complete condenser. Hence all the vapours are cooled down.
There is one shell and one tube pass inside the condenser and the flow is
counter current.
Since the top product mainly comprises of the propane, the physical
properties of propane are used for all the calculations.
The cooling fluid chosen is chilled water that enters the tube side at 150C
and leaves at 450C.
The tube layout for this particular design is arranged in a squared pitch.
Basis: 1 hour
Flow rate entering the condenser; V
V = L+D; 402.39 + 661.83 = 1063.22 kg/hr
5.1 Energy Balance Over the condenser:

Q = (Vapour flow rate * latent heat of vaporisation of methanol) + mCpT
Q=mL +mC p T .(21)
mL due to phase change, since it is a complete condenser where phase

change occurs; and
mCpT due to increase in the energy per degree rise in temperature.
Vapour Flow Rate;

Kg
1
hr
m=1063.22 =0.295 Kg /s
3600 s
Latent heat of Vaporisation of Propane (1,3 Butadiene is ignored as it would not

bring a vast difference)= L = 322.76 kJ/Kg
Therefore,

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mL=0.295 kg /s322.76 kJ / Kg= 95 . 214 KJ /s95. 214 KW
661.83 Kg
1.75 KJ
sec
mC p T = 10 K =3.22 KJ /sec
KgK
Overall Q=95.214 KW +3.22 KW =98 . 434 KW
Since the Heat lost by the condenser is calculated the flow rate of water
required can also be calculated as relevant from the following formula;
Q=(mC p T )1=( mC p T )2 (22)
It is assumed earlier that the chilled water enters the condenser @ 15 0C and
leaves @ 450C. Hence T = 300C
Hence,
X Kg
4.2 KJ
sec
(mC p T )1=98.434 KW = 30 K=0 .781 Kg/sec
KgK
Water flows at a flow rate of 0.781Kg/sec inside the tubes.

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Figure 21: My Diagram for better understanding of TLM
From the diagram above it now becomes easier to TLM. The Log mean
temperature difference is given by:
( T t OUT )(T OUT t )
T LM = ..(23)
T t
ln ( OUT )
T OUT t
Where,
TLM = log mean temperature
TIN = inlet temperature of process fluid
TOUT = outlet temperature of process fluid
tIN = inlet temperature of cooling water
tOUT = outlet temperature of cooling water
( 4540 )(3515)
T LM = =10.820 C
4540
ln ( )
3515
To begin with the design, we assume an approximate overall coefficient. This is

done in aid with Graph 4; where the fluid in the process side are classified as
Paraffin and the fluid in the service side is taken as River, Well or Sea Water.
Hence, the assumed overall coefficient = 600 W/m2 0C

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Graph 4: Overall Coefficients (join process side to the service side and
read U values from the centre line)
Trial Area:
Q=UA T LM (24)
Where,
Q= Heat Transfer per unit Time
U= Heat Transfer Coefficient
A= Area
TLM = Log Mean Temperature difference
Q 98.4341000W
A= = =15 .16 m 2
U T LM 600 W /m2 K10.82 K

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Layout and Tube Size[24]:
Usually the plant standards require tubes of:

The outer diameter is 20mm
The inner diameter is 16 mm
The length is taken to be 2.44 m (8 ft)
The tubes are made of arbitrary brass.
The arrangement is a squared pattern.
Hence, the surface area can now be calculated from the above data specified.
Surface Area ( A ) =dl=3.14201032.44
Surface Area ( A ) =0 .1533 m2
Therefore,
Total Trial Area
Number of tubes=
Suraface Area of one tube
15.16 m2
Number of tubes= =99 tubes
0.1533 m2
Since there is slight condensation occurring, hence the number of tubes

calculated is so less.
Since, it was decided to use a Square Pitch;

Pt =1.25d o =1.2520 mm= 25 mm
Tube Bundle Diameter; Db

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Nt
K1

Db=d o
Where,
Nt = number of tubes
K1 and n = constants obtained from table 9[25]
Do = Outer diameter
Table 9: K and n constants for square arrangements:
Square pitch, Pt = 1.25 do
Number of 1 2 4 6
Passes
K1 0.215 0.156 0.158 0.0402
n1 2.207 2.291 2.263 2.617
Hence,
99
0.215

Db=20
Number of tubes in the centre row:
Db
Tubest h e centre row = ..(26)
Pt
321.91 mm
Tubest h e centre row = =12 . 87 tubes 13 tubes
25 mm
We take it as 12 tubes as the number of tubes should be even and divisible by 4

as the arrangement is a square pitch.

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5.2 Shell Side Coefficient:

The Tube Wall temperature, Tw can be estimated if the condensing coefficient is
assumed. The value for the condensing coefficient is assumed to be
1500W/m0C
Mean temperature:
35+45
S h ell side= =400 C
2
15+40
Tube side= =27.5 0 C
2
( 40T w ) 1500=( 4027.5 ) 600
Hence, the wall temperature is 350C.

Table 10: Physical Properties of Propane @ 350C[26]
Liquid Density (L) @ 350C 514.13 Kg/m3
Liquid Viscosity (L) @ 350C 0.11321 centi-poise
Liquid Thermal Conductivity (kL) @ 0.095W/m K
350C
Vapour Density @ 40 0C mean vapour temperature (V) = 28.6 Kg/m3

[27]
Using Kerns Method , the mean transfer coefficient for the tube bundle is
given by:
hc

Where,
Wc
h=
L Nt
Wc = Flow rate of the distillate in Kg/sec

L = Length of the tubes
Nt = Number of tubes

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2
N r= number of tubest h e centre row ..(28)
3
2
N r= 12=8
3
Hence,
0.295 3
h= =1 . 2210 Kg/m sec
2.4499
Substituting the values in the Kerns Equation:
hc

hc

The value obtained is close enough to the value assumed (1500W/m 2K), hence
the estimated Tw is acceptable.
5.3 Tube Side Coefficient:
Eagle and Ferguson (1930) adapted a much reliable formula for the heat transfer
coefficient for water used in the tube side. This is stated as below:
0.8
4200(1.35+0.02 t)u t
hi= 0.2
(29)
di
Where,
hi = inside coefficient for water

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t = mean water temperature

ut = water velocity
di = tube inside diameter
ut can be calculated from the internal diameter of the tube

Tube Cross- Sectional Area;
2
(.016) 99 2
( A )= =0. 0199 m
4
Density of water at 27.50C (mean water temperature in the tubes) = 995.65

Kg/m3
Tube Side Velocity, ut

m
ut = ..(30)
A L
0.781
ut = =0. 0394 m/ sec
995.650.0199
Hence, substituting the values of velocity, the heat transfer coefficient of water
inside the tube is;
4200(1.35+0.0227.5)0.03940.8
hi = 0.2
=1375. 49 W / m2 0 C
(.016)
5.4 Overall Heat transfer Coefficient U;

do do do
d o ln ( ) 1 1
1 1 1 di di di
= + + + + (31)
U h o hod 2 kw hid hi
Where,
20
U = the overall coefficient based on the outside area of the tube, W/m C
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20
ho = outside fluid film coefficient, W/m C
20
hi = inside fluid film coefficient, W/m C
20
hod = outside dirt coefficient; fouling factor, W/m C
20
hid = inside dirt coefficient; fouling factor, W/m C
kw = thermal conductivity of the tube wall material, W/m0C
di = tube inside diameter, m
do = tube outside diameter, m
Fouling Factors: As neither of the fluid is heavily fouling, the dirt coefficient at
2 0
both the sides has been assumed to be 6000 W/m C and kw is assumed to be
50 W/m0C
Substituting all the values in the equation 31;
20 20 20
(20103 ) ln ( ) 1 1
1 1 1 16 16 16
= + + + +
U 1646.979 6000 250 6000 1375.49
1
=1.9354103
U
Hence, Overall Heat transfer coefficient;
U=516 . 689 W /m2 0 C
The value obtained is significantly lower than the assumed value of 600 W/m2 0C
The calculation has to be repeated using different values of Overall heat transfer
coefficient by trial and error method; and the closest possible answer firms up
the final design.
The calculations are redone with a new value of 500 W/m2 0C

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Q 98.4341000 W 2
A= = =18 .19 m
U T LM 500 W /m2 K10.82 K
3
Surface Area ( A ) =dl=3.142010 2.44
Surface Area ( A ) =0 .1533 m 2
Hence, the number of tubes now changes,
Total Trial Area 18.19 m2

Number of tubes= = =119 tubes
Suraface Areaof one tube 0.1533 m2
Tube Bundle Diameter; Db
Nt
K1

119
0.215

Db=d o
Db 349.899
Tubest h e centre row = = =14 tubes
Pt 25
Shell Side Coefficient:

As already known,
hc


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Where,
0.295
h= =1. 009103 Kg/m sec
2.44119
And
2 2
N r = number of tubest h e centre row= 14 9tubes
3 3
Therefore, substituting the values of h and Nr in equation 32
hc

hc

Tube Side Coefficient:
Again using Eagle and Fergusons (1930) formula tube side coefficient is
calculated. But the velocity of the water in the tubes changes;
New Cross sectional Area

2
(.016) 119
( A )= =0 .0239 m2
4
Hence, the tube velocity,
0.781
ut = =0. 033 m/sec
995.650.0239

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Hence, the new calculated value for the Tube Side Coefficient;
4200(1.35+0.0227.5)0.0330.8
hi = 0.2
=1220 . 06 W /m2 0 C
(.016)
Overall Heat transfer Coefficient;

20 20 20
(20103 ) ln ( ) 1 1
1 1 1 16 16 16
= + + + +
U 1630.35 6000 250 6000 1220.06
1
=2.0575103
U
Hence, Overall Heat transfer coefficient;
U=486 . 026 W /m2 0 C
The results are satisfactory. The values obtained are close enough to the values
assumed hence, the design is confirmed.
5.5 Shell side Pressure Drop:
Specifications:
Pull through Floating head is used, no close clearance is required.

35% cut of the Baffle Spacing
A condenser has wider baffle spacing, lB Ds
Pressure Drop is given by;

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j f Ds
L
de
u s2
lb .14
Ps =8 ( ) .(32)
2 w
Where,
Jf = Friction factor
L = Length of the tubes
Lb = baffle Spacing
All the unknowns are calculated below.
Shell internal Diameter; Ds
D s=D b+ clearance
Clearance is = 89mm estimated from the graph 5
Graph 5: Shell- Bundle Clearance

Hence,
Ds=349.899mm+ 89 mm=438 .899 mm

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Cross Sectional Area As for the hypothetical row of tubes at the Shell Equator
( pt d 0) D s l B
As= (33)
pt
Where,
Pt = Tube Pitch
Ds = shell inside diameter
LB = baffle spacing
( 2520 ) 438.899438.899106
As= =0 . 039 m2
25
Shell Side mass Velocity Gs

Ws
G s= .(34)
As
Where,
Ws = Fluid Flow Rate on the shell side in kg/sec
0.295 2
G s= =7 . 56 Kg/m sec
0.039
Linear Velocity us
G s 7.56
us = = =0. 26 m/sec
29.16
Shell Side Equivalent Diameter; de

The equivalent diameter for a square pitch arrangement is given by;

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2 2
pt d o
4( )
4 1.27 2 2
de=
do
=
do
( pt 0.785 d 0 ) (35)
1.27
de= ( 25 20.785 202 )=19 . 8 mm
20
Friction Factor; jf
Friction factor is estimated from a graph in FIG; which is a correlation between
Reynoldss number and baffle cut.
Hence,
G sd e 7.5619.8103
Re = = =18 , 711
v 0.008103
Graph 6: Shell side Friction Factor; Segmental Baffles
From the graph Friction Factor is determined to be 4.8 *10-2

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Substituting all the above calculated values in the pressure drop equation;
2
84.810 438.899
2.44
19.8
29.160.262
0.438899 .14
Ps = ( )
2 w
Ignoring the viscosity correlation;

Ps =46 . 64 N /m 2
The Pressure drop is negligible; hence more sophistication calculation is not

justified.
5.6Tube Side Pressure Drop:
The pressure Drop on the Tube side is given by,
ut2
[ j L
]
m
Pt =N p 8 f
di w ( ) +2.5
2
(36)
The viscosity correlation is neglected;

Jf ; Friction Factor is given by a graph 7
Where,
u td i
Reynoldsnumber R e = (37)

Hence,
0.03316103995.65
Re = =876 . 172
0.6 103

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Graph 7: Tube side Friction Factor

Hence from the graph below,
Jf = 9*10-3
Substituting the values in the pressure drop equation;
891032.44 995.65 0.0332

Pt =1[ + 2.5]
16103 2
2
Pt =7 . 306 N /m
The pressure drop is almost negligible due to the following reasons:

The flow is laminar as Re < 2000
The velocity of the cooling water is very low
Only one tube pass is used, hence there is a straight pipe through which
the pipe flows.

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6.0 REBOILER:
Reboilers are used with the distillation column to vaporise a fraction of the
bottom product.
[28]
There are three different kind of reboilers used:
Forced Circulation; where the fluid is pumped through the exchanger. The
vapour formed is separated and sent back to the bottom of the distillation
column and rest is removed.
Figure 22: Forced Circulation Reboiler

http://upload.wikimedia.org/wikipedia/commons/a/a7/ForcedCircul
ation.png
Thermosyphon, unlike forced circulation it has natural circulation. The
liquid circulation is maintained by the difference in densities of the two-
phase mixtures of vapour and liquid. These kinds of Reboilers can have
vaporisation on the tube side; when they are vertically placed or the
vaporisation occurs on the shell side, when placed horizontally.
Figure 23: Thermosyphon

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http://upload.wikimedia.org/wikipedia/commons/5/57/Thermosyph
on_Reboiler.png
Kettle Reboilers, also called submerged bundle reboilers; where boiling
takes place on the tubes immersed in a pool of liquid. The liquid does not
circulate through the heat exchanger. These are the most expensive kind
of Reboilers.
Figure 24: Kettle Reboiler

http://www.spiraxsarco.com/images/resources/steam-engineering-
tutorials/2/13/Fig_2_13_5.gif
6.1 Heat Duty over the Reboiler:

Q=V ' H vapourisation .(38)
In the above equation, the H (Heat of Vaporisation) is considered only for 1, 3

Butadiene as major fraction of the component entering the Reboiler comprises
of 1, 3 Butadiene. Minor fractions of propane, pentane and 1, 2 Butadiene is
ignored. This would not affect the result drastically as the Heat of vaporisation of
the other components somewhere lies in the same range.
Hence,
Assuming; that the bottom product is liquid at boiling point which enters the
Reboiler at 368K.

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4525.63 Kg
1 hr
hr
335.55 KJ
3600 sec
Q= =421 . 826 KW
Kg
Amount of Steam Required:
Heat obtained by the process fluid is the heat lost by the steam entering the
Reboiler.
Hence the Q remains same. Assuming steam entering the Reboiler at 2.6 bars,
Hence, H for steam at 2.6 bars = 2177.42 KJ/Kg
Q 421.826 KW
S= = =0 .194 Kg/ sec
H
vapourisation
2177.42 KJ /kg
6.2 Choice of type of reboiler used with the Propane Distillation:

[28]
The choice of the kind of reboiler used with a distillation column solely depends
on the following:
The viscosity and the propensity to fouling of the process fluid
The operating pressure
The headroom available to layout the equipment.
After careful judgement, it is concluded that a Horizontal Thermosyphon

Reboiler would be used with this distillation column, since the horizontal
reboilers require less headroom. These are most economical type of reboilers for
most application and are not suitable for high viscous fluids. The fluids in the
column have very low viscosity.
Also these reboilers are suitable for high temperatures and high pressure which
fulfil the demands for this unit.
The only disadvantage with this kind of reboiler is that a hydrostatic head is
required for the thermosyphon effect which requires elevation of the column

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base. This problem can be overcome by using supporters at the distillation

column is not huge.
7.0 Overall Energy Balance over the Distillation Column:
The Energy Balance over the column could not be calculated in the first part of
the assignment as the Reflux Ratios were unknown.
The Heat Duty over the Condenser and the Reboiler is calculated. It is
summarised in the table below.
Units Energy Required Energy Released
Condenser - 98.434 KW
Reboiler - 421.826KW -
Total -323.392 KW
The Negative Sign shows that the Energy is required to run the unit.

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8.0 Piping and Instrumentation Diagram

The Piping and Instrument diagram (P and ID) shows the engineering details of
the equipment, instruments, piping, valves and fittings and their arrangements
which is not detailed in the process Flow sheet. It should include the following.
[29] [30]
All process equipment identified by an equipment number. The equipment

should be drawn roughly in proportion, and the location of nozzles shown.
All pipes, identified by a line number. The pipe size and material of
construction should be shown. The material can be included as part of the
line identification number.
All valves control and block valves, with an identification number. The type
and size should be shown. The type may be shown by the symbol used for
the valve or included in the code used for the valve number.
Pumps identified by a suitable code number.
All control loops and instruments, with an identification number.
For simple processes, the utility (service) lines can be shown on the P and I
diagram. For complex processes, separate diagrams should be used to
show the service lines, so the information can be shown clearly, without
cluttering up the diagram.
Since the Process of Butadiene production is very complex which includes many
units, the P and ID is only done over the Propane Distillation Column which is
attached in Appendix, 6 (issue number 002) The basic units and symbols used in
the P and ID are briefly described below:
Control Valves [31]: The parameters such as temperature, pressure, flow and
level are controlled by the control valve. Control Valves can be manual or
automatic which are partially or fully open or closed. The action of the
control valves are in response to the signals received from their respective
controllers that compare the set-point to the process variables.

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Figure25: Detailed Diagram of a Control Valve

http://www.isa.org/Images/InTech/2005/April/20050415-3.gif
Gate Valve [32]

: These valves are opens by lifting a round or rectangular
wedge out of the path of the fluid. Gate valves are used when a straight-
line flow of fluid and minimum restriction is desired. These valves should
never be used as control valves unless those are specifically designed for
it. Typical gate valves are designed to be fully opened or closed. There is
very low frictional loss when the valve is fully open due to negligible
obstruction. Gate valves are present before and after every control valve
and pump which offers effortless maintenance during equipment failure.
Figure 26: Detailed diagram of a Gate Valve

http://www.spiraxsarco.com/images/resources/steam-engineering-
tutorials/12/1/fig_12_1_1.gif
Transmitters: These are sensors which monitor the changes in the process
variables and simultaneously send signals to the controller.

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They are named as FT (flow Transmitter), PT (Pressure Transmitter), TT

(Temperature Transmitter) and LT (Level Transmitter) respectively. They are
Locally Mounted which means that the controller and the display are
located in the plant where the sensing instrument is placed.
Drain Valve: As the name suggests, these valves are used to drain the
components from the unit or pipelines. These are generally closed and are
in operation usually during site or unit maintenance.
Relief Valve: The relief valve is a type of valve used to control or limit
the pressure in a system or vessel which can build up by a process upset,
instrument or equipment failure, or fire. The pressure is relieved by
allowing the pressurised fluid to flow from an auxiliary passage out of the
system. Since the distillation Column taken into consideration is operating
under high pressures, a relief valve can act as a precautionary measure
which would help to get rid out the extra pressure built up into the unit. It
is built on the reflux drum, as building it over the column can lose its
components in the vapour phase that is released. As it is the last stage the
purified butadiene cannot be afforded to be wasted.
Pneumatic Lines: The signals transmitted from a controller to the valve are
generally shown by pneumatic lines on a P and ID.

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Electric Lines: The dotted lines show the transmission of electric signal in
the P and ID. The electric signal is send by the transmitter to the
controller.
High and Low Level Alarms: Alarms alert the operators of serious and
potentially hazardous deviations in the process conditions. Key
instruments are fitted with switches. If there is a delay or lack of response
by the operator a hazardous situation can occur in a short span of time.
Often drills are practiced to overcome such catastrophic situations. When
this system turns on, a trip system automatically comes into action which
includes, shutting down of pumps, closing valves, operating emergency
systems etc.
8.1 Control Loop

A chemical plant is composed of several processing units; these cannot be
treated as simple systems working independently. They are integrated to form a
systematic, rational and controlled process. This process must then satisfy
many requirements in order to achieve its objective of converting raw material
to the desired products. Control systems are employed to successfully satisfy
the requirements of safety, product specifications, taking into account,
operational constraints, plant economics and environmental regulations. The
control system is composed of an arrangement of equipment such as
temperature / pressure indicators, pneumatic valves, process controllers linked
with computers (CPU). The requirements of control are stated below:[33]
Safety [33]

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A principal prerequisite of the plant is to operate safely for the well being of
plant stakeholders and to continue satisfying the economic goal. To achieve
this, temperature, pressures, flow rates etc need to be controlled within
allowable limits.
Operational Constraints [33]
Different process equipment have variable process constraints i.e. tanks should
not overfill, distillation columns should not be flooded and centrifugal pumps
must maintain a certain net positive suction head, these need to be considered
when determining the control system.
Environmental Constraints [33]
Involves ensuring discharges are within acceptable limits e.g. as prescribed
under IPC.
Economics [33]
Plant operating conditions need to be controlled to ensure that the plant is
operating at its optimum, thus ensuring maximum profitability.
Although control is essential, it is known in industry that trying to tightly control
absolutely every stream in the process is very costly and unrealistic and can
result in total inflexibility and even destabilisation of the plant, (control loops
may start to interfere with each others actions). Similarly measurement
sensors and control valves are expensive, so unnecessary measurement is a loss
of money. Therefore these factors will need to be taken into account when
deciding upon the control.
8.2 Control Systems over the Distillation Column:
Various control measures have been taken into account to meet the objectives
of the plant such as safety, operation, environmental constraints and economics.
Sensors have been installed at various process lines and equipments to make
the operator aware of the situation with the equipment and the process. The
sensors transfer signals to the controller which then send back commands to the
respective valves to carry out the action.
Control system of the process will be explained as we go along the PID from left
to right.[34][35]
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FC 1: the feed pipe is installed with a flow controller, which helps to control the
flow throughout the pipe. The flow rate is received as input to the FT-1, which
then sends output signals to the flow controller FC, which then sends on
information to the automated control valve CV-1. This ensures a steady state
and control flow rate of feed to the distillation column.
PC 1: The distillation column is operating under high pressures. The pressure is
a very crucial variable and has to be controlled to avoid flooding. The pressure is
read by a pressure gauge and this input is received by a PT1 which sends signal
to the PC 1 which then forwards the information to the control valve on the
condenser. The condenser would reduce the flow rate of water if the pressure
drops; this intern increases the temperature of the distillate entering the reflux
drum as desired heat exchange was not possible; which increases the pressure
back into the column. The reverse action is carried out if the pressure inside the
column increases. There is a relief valve on the reflux drum which also operates
when the pressure inside the column increases drastically.
LC 1: For desired separation to take place, it is important to maintain the ratio of

the distillate to the reflux Liquid. Hence it is vital to maintain the level in the
reflux drum. The level is read by a level indicator which sends the information to
the LT 1 which further forwards the signal to the control valve on the pipe back
to the condenser. If the level in the drum falls, the controller sends signal to
close the valve which results in maintaining the level in the drum.
TC 1 and FC 2: The temperature should be well maintained inside the column

to provide vaporisation of the volatile fluids for desired separation. Heat is
provided by the steam flow in the reboiler. Hence a controller valve is installed
on the pipe which carries steam to the reboiler. This controller receives signal
from the flow transmitter (FT2) or the temperature transmitter (TT1). If the
temperature inside the column reduces, the controller sends signal to the
control valve to open slightly. This increases the flow rate of steam into the
reboiler increasing the temperature of the column.

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LC 2: Flooding is a problem commonly faced by distillation columns if the

design is poor. Sometimes blockage in the support systems inside the column
can cause obstruction to the passage of the liquid and the gases. This can
increase the level in the column resulting in spillage of the valuable product. A
level controller is installed in the pipe leaving the column at the bottom. This
control valve receives signals from the level controller which gets its input from
the level transmitter. If the level in the column falls down, the valve closes
slightly to maintain the level and prevent it from becoming dry. Also when the
level falls down too low or rises to high, the alarms blow up which would alert
the operators to take serious actions immediately like evacuating the plant or
shutting all the valves and stopping the flow rates.
Indicators:
There are three main indicators used in the P and ID. These are mainly to
provide information of the operating conditions. There are two sample indicators
SI (1-1) and SI (1-2), which provide information about the purity of the fluids
entering and leaving the column.
Since, the columns top temperature is different from the bottom one, two
temperature indicators are required.
A combination of automated valves, flow and temperature indicators along with

controllers are used to control the process. Investment in these instruments and
the control system is required and is necessary. The control system along with
the PID is then checked by senior manager and engineers over a HAZOP
meeting. Changes are made to the control and the PID before the system is
installed, in such a way money is saved and at the same time safety of the
operator is ensured.
Since Hazop was carried out on this section of the process, there were certain
changes made from the previously designed control loop system. Issue 001 in
Appendix VI shows the draft copy of the previously designed P and ID which was
then improvised to Issue 002

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9.0 Hazard and Operability Studies HAZOP

HAZOP is a procedure for critical, systematic examination of the operability of a
process. Procedure of a Hazop involves taking a full description of a process,
generally using a PID, and systematically questioning every part of it. This helps
to establish deviations from the design intent. When the deviations are identified
assessments are made on the consequences of the deviation and the required
action which should be taken to prevent or control the hazard from taking place.
The analysis of Hazop is carried out in a structured way by following the
guidlines attached; it completely relies on the realising and imagination to
discover the credible causes of the deviations by the Hazop team. In practise
many of the causes will be very obvious such as pump failure. But putting a
Hazop meeting encourages highlighting many causes which might be obvious in
first consideration. In this way the study is carried out and becomes more
rigorous and encourages the involvement of all the team members. The result of
the Hazop there is a good chance of identifying and recording relevant actions to
be taken against failures and problems which have not been experienced before.
More over a documented file of Hazop is required by legislation to confirm that

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preventive measures had been taken to ensure the safe working condition of the
operators and the environment.
In our study we carried out a Hazop with Dr. Titiloye on the Feed pipe entering
the Propane Distillation column. (As highlightedGreen in Figure attached in
Appendix VII). General consequence of a Hazop leads to an updated version of
the PID to be made after including all the safety features discussed during the
meeting. Hence the slight deviation in the final P and ID (ISSUE no. 2) is due to
Hazop done on the pipe.
In practise Hazop should be carried out over the whole process, but due to time
constraints and requirements of the project only one line of the process is looked
at.
Hazop discussions have also been added, this includes all the causes and their
consequences looked at and also preventive actions have been highlighted. The
Hazop is attached in Appendix VII.
10.0 Conclusion:
The design project has been successful in its aims of providing a detailed
knowledge a chemical process unit. This project was a learning process where
different challenges were faced. At this stage, such a project is aimed to
increase general design knowledge of a given operating unit in this case; a
packed bed distillation column. As this was just a preliminary design, the amount
of detail of the design and the accuracy of the final calculations might be
questionable. However, it remains a fact that this project targets more than just
design but also gives an idea of how to make reasonable assumptions and
where data is not available, the use of values which can be used to make
reasonable estimates. Overall the project enhances ones ability to play around
with available data in order reach a reasonable estimate.

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After calculating all the values over my distillation column I conclude that one
distillation column can be used to separate propane and recover 1,3 butadiene.
A stepped column can be used as the diameter for the pentane distillation
column, (the unit where the 1,3 butadiene is pumped to for further purification.)
is 2 m as suggested my group mate. Since the diameter for the propane
distillation column is 0.65m the top part of the column can have this diameter
and the lower part of the column should have a diameter of 2m. This can
reduce the operating costs and also a significant amount of raw material to build
the column would be reduced.
Also a separator can be used instead of a distillation column, but the
temperature has to be reduced too low, to obtain such separation. This can be
more expensive than providing high pressure inside the column.
11.0 References:
[1]: http://www.wakefield.gov.uk/NR/rdonlyres/F456AD74-5BC2-4697-9414-
55C32FCBE9E2/0/s1_13Butadiene.pdf,( (Part 1: Group Project on1,3 Butadiene
Production) accessed date 28/11/09
[2]: http://www.icis.com/v2/chemicals/9075172/butadiene/uses.html; accessed

date 07/02/10
[3]: http://www.dow.com/productsafety/pdfs/butadiene_guide.pdf accessed date

15/03/10
[4]: http://www.gansu.gov.cn/en/BasicDetail.asp?CID=50 (Part 1: Group Project

on1,3 Butadiene Production)
[5]: http://www.britannica.com/EBchecked/topic/166112/distillation-column;
accessed date 13/02/10
[6]: http://www.websters-online-dictionary.org/re/reflux+ratio.html accessed date

13/02/10
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[7]: http://www.separationprocesses.com/Distillation/DT_Chp04n.htm; accessed

date 23/02/10
[8]: Dr. Bruce, 3rd year Chemical Engineering Advanced Separation Class Notes,
Aston University, 2010; Lecture 1
[9]: http://www.processglobe.com/Liquid_Specific_Heat.aspx; accessed date

24/02/10
[10]: Coulson J.M & Richardson J.F Chemical Engineering Design, 4th ed., vol.
6, Pergamon, Oxford, 2005 page 567-569,
6, Pergamon, Oxford, 2005 page 579
[14] : Coulson J.M & Richardson J.F Chemical Engineering Design, 4th ed., vol.
6, Pergamon, Oxford, 2005 page 588-593
[16]: Dr. Bruce, 3rd year Chemical Engineering Advanced Separation Class Notes,
Aston University, 2010; Lecture 3
[17]: http://www.tower-packing.com/metal/metal_pall_ring_tower_packing.htm,
accessed date 29/02/10
6, Pergamon, Oxford, 2005 page 216 and 221
[21]: http://www.zehua-chem.com/

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[24]: http://www.alibaba.com/showroom/condenser-tube.html; assessed on

26/02/10
[25]: Dr. John Brammer, 2nd Year Chemical Engineering Heat transfers Notes,
Aston University.
[26] : http://www.processglobe.com/Liquid_Specific_Heat.aspx
[30]: http://www.azom.com/Details.asp?ArticleID=863; accessed date 09/03/10
[31]:
http://www.documentation.emersonprocess.com/groups/public/documents/book/
cvh99.pdf ; accessed date 14/03/10
6, Pergamon, Oxford, 2005 page 197 -198
[33]: Dr. Fletcher, 2nd Year Chemical Engineering Control Process Notes, Aston
University
[34]:Page S. Buckley, William L. Luyben and Joseph P. Shunta Design of
Distillation Column Control Systems
[35]
:http://www.see.ed.ac.uk/~jwp/control06/controlcourse/restricted/course/fourth/c
ourse/module3-1.html
[36]: Dr. Drahun, 2nd Year Chemical Engineering Advanced Design Process,
Aston University.
[37]: Dr Brammers, 3rd Year Chemical Engineering Process Economics lecture

notes, Section C,
notes
[39]: (ref: www.informaworld.com/index/778741608.pdfl); accessed date

24/03/10

notes, Section 4(a)

notes, Section 4(b)

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Graphs and Correlations:
Graph 1 : Coulson J.M & Richardson J.F Chemical Engineering Design, 4th ed.,
vol. 6, Pergamon, Oxford, 2005 page 524
Grapgh 2: Coulson J.M & Richardson J.F Chemical Engineering Design, 4th ed.,
Graph 3: Dr, Bruce Davies; 3 year Chemical Engineering advanced Separation

notes; Lecture 3
Graph 4: Coulson J.M & Richardson J.F Chemical Engineering Design, 4th ed.,

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i

CE 3003 Advanced Process Design - Individual Project: Executive Summary

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CE 3003 Advanced Process Design Individual Project

Richie Gandhi Page 69

Richie Gandhi Page 69

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5.6Tube Side Pressure Drop:............................................................................63

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1.0 Project Brief:

1.1 Introduction to the product:

Butadiene is a simple conjugated diene. It is

1, 3 Butadiene (CH2=CH-CH=CH2), is a colourless gas with mild aromatic odour.

In 1863, a French chemist isolated a previously unknown hydrocarbon from

products of petroleum.[1] In 1910, the Russian chemist Sergei

In 1929,Eduard Tschunker and Walter Bock, working for IG Farben in Germany,

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Figure 2: Chart Showing Various Uses of different forms of 1,3

Butadiene can also be produced by the catalytic dehydrogenation of normal

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In the previous project it was decided that Oxydehydrogenation Process would

1.3 Location [4]

Figure 3 : graph to show Production Capacity and Output of Butadiene

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Figure 4: Map of Gansu Province in China

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Transportation - Lanzhou is very well interconnected to various cities and

2.0 Project Plan and Objectives:

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Chemical engineering design to achieve the following outcomes is to be

Piping and Instrumentation Diagram for the distillation column is

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2.2 Personal Objectives:

Enhance organisational skills and keeping to deadlines: The tasks would

Develop Communication Skills: Communication skills are enhanced both

Enhance Team-working Skills: HAZOP and Economic Appraisal have to be

Professional report writing: At the end of our project I wish to able to

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2 Tutor meeting and discussing the

3 Discuss findings with tutor

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4 Calculating diameter and size of 08/02/1 19/02/1

5 Piping and instrumentation 1/03/09 10/03/1

6 HAZOP 10/03/1 19/03/1

7 Calculating cost and profit 01/03/1 15/03/1

8 Completing referencing 25/01/1 17/03/1

9 Ensuring completion of all section 20/03/1 21/03/1

10 Proof read 22/03/0 26/03/0

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3 The Revised Process:

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Equation (1) gives 100% completion; higher conversions at lower temperatures

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4 The Chemical Design:

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vaporise the volatile components is provided by the reboiler. The components

Figure 5: Basic Distillation Column

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Table 1 (b): Distillate:

Table 1 (c): Bottom:

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The boiling points of the feed components at 1 atmospheric pressure are as

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Feed condition: Cold Liquid under pressure

4.1.1 Reflux ratio and the number of Theoretical Stages

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