PRODUCTION OF 1350 TONS/DAY ACETIC

ACID FROM WOOD SAWDUST

(Session 2015-2019)

Project Advisor: Professor Dr. Shah Muhammad

Co-Advisor: Engr. Muhammad Asim
Group Members:
Muddassar Abbas Mahu 2015-UET-ShCET-LHR-CE-03
Muhammad Sarkhan Tariq 2015-UET-ShCET-LHR-CE-06
Muhammad Fawad Anwar 2015-UET-ShCET-LHR-CE-08
Afifah Aurangzeb Dar 2015-UET-ShCET-LHR-CE-18

SHARIF COLLEGE OF ENGINEERING &

TECHNOLOGY LAHORE
1
 DEDICATION
This work is dedicated to:

“The Sake of Allah, our Creator and our Master and the greatest teacher, our Messenger Muhammad
(S.A.W.W), who taught us the purpose of life”

“Our Parents, whose blessings brought us at this stage and trample their inclination and longings for uploading
our studies”

Lastly a list has been comprised of the fortunate people whom ALLAH has given us to help with this project.
The contributions vary but the appreciation is still large thus we leave it in the hands of ALLAH to pay the debt
to these beautiful people and reward them.

2
 ACKNOWLEDGEMENT
All thanks and praise to Allah Almighty

We bow our heads before Allah Almighty for blessing us with such an opportunity, strength and resources to
complete our final year project work. The completion of this project was indeed a dauntless task which
demanded dedicated efforts from many people whom we owe a lot of gratitude. For timely completion of this
project we needed a driving and guiding force. This power was provided to us by our respected advisor
Professor Dr. Shah Muhammad and co-advisor Engr. Muhammad Asim. Their knowledge in field of Chemical
Engineering has benefitted us in very comprehensive way and imparted life learning lessons not only for our
profession but for our daily lives. Through their exemplary guidance and leadership, we were able to achieve
the objective of this project. It has been a real honour to have worked and learn under their guidance indeed.

3
 Preface
It is a project report, espousing the great efforts of a team to whoever more inspired than equipped, that covers
the design aspects of the “Production of Acetic Acid”. The main raw materials used are wood sawdust and
nitrogen.

The design report of our project is made very carefully and honestly, so hopefully the content is adequate for the
basic understanding of the process as each and every aspect is discussed in detail with clear visual graphics. All
the designing and calculations are done by using up to date correlations of heat transfer, mass transfer and
equipment design. This report should also be useful to the engineers in the chemical engineering department.

Separate chapters are devoted to each of the step for the designing of a project including introduction, process
description, material and energy balances and equipment designs. For the good operation and safety purpose,
the instrumentation of equipment is done and explained in a separate chapter. Also the project cost evaluation is
done in the other chapter. Environmental aspects are also done in the last chapter.

This report is the result of a modest effort by a group of students.

4
 Table of Content

SECTION l Introduction, Process Description

Chapter 1 Literature Survey , Process Description

1.1 Introduction………………………………………………….…………………………………… 8
1.2 Literature Survey…………………………………………………………..……………………. 10
1.3 Uses…….…………………………………………………………………….…………………… 10
1.4 Process Selection………………………………………….………..…………………………….. 11
1.5 Process Description………………………….…………….…...……………………………….. 12
1.6 Process Flow Diagram................................................................................................................... 13

Chapter 2 Material Balance

2.1 Material Balance across Dryer……………………………………………………….……….. 14
2.2 Material Balance across Reactor………………………..………….…………………………. 15
2.3 Material balance across Cyclone Separator………..…..……….……………………………. 15
2.4 Material balance across Condenser…………………………...………………………...…….. 16
2.5 Material balance across Distillation Column…………………………..……...……………… 16

Chapter 3 Energy Balance

3.1 Reference conditions……………………………………………………………………………. 19
3.2 Energy balance across Reactor………………………………………….…………………...… 19
3.3 Energy balance across Heat Exchanger……………………………………………….………. 21
3.4 Energy balance across Distillation Column…………………………….……………..………. 22

SECTION ll Design of Process Equipments & Economic Analysis

Chapter 4 Designing of Process Equipments

4.1 Introduction…………….…………………………………….………………………………… 25
4.2 Type of Reactors……………………………….………………………………..……………… 25
4.3 Classification of Reactors…………….…..…………………………………………………….. 27
4.4 Selection Criteria…….……..…………………………………………………………………… 27
4.5 Purpose of Reactor……………………………………………………………………………… 28
4.6 Reactor Design…………………..………………………………………………………………. 29
4.7 Cyclone Design……………………………...……………………………………...……………. 36
4.8 Condenser Design…………………………...…………….…………………………………….. 40

5
 4.9 Distillation Column Design………………………………………………………………………. 49

Chapter 5 Cost Analysis

5.1 Introduction………………………………………………………………………………….. 63
5.2 Fixed Capital Investment…;;;………………………………………………………………. 63
5.3 Working capital//…………………………………………………………………………….. 63
5.4 Cost Index….………………………………………………………………………………… 64
5.5 Purchased Equipment Cost…………….…………………………………………………… 64
5.6 Product cost……………………………………;…………………………………………….. 66

SECTION lll Hazop & Control of Process

Chapter 6 Hazop Analysis

6.1 What is Hazop? …………………………………………..…………………………………. 69
6.2 Brief Summary of Characteristics ………………………………………………………… 69
6.3 Potential Hazards and Operability problems ………………………………….…………. 70
6.4 Key Words ………………………………………………………………………………...… 70
6.5 Limitations of Hazop…………………………………………………………………………70
6.6 Hazop Study of Complete Plant……………………………………………………………. 71

Chapter 7 Instrumentation and control

8.1 Various Control Loops …………………………………………………………………….. 77

8.2 Distillation Control Objective …………………………………….……………………….. 81
8.3 Distillation Column Control………………………………………………………………... 83

References ………………..……………………………………………………………………... 84

6
 CHAPTER
1
INTRODUCTION
Recent statistics show an increase in acetic acid consumption. Natural reserves have started to deplete and
will be empty in about 5 decades. The growth of acetic acid demand is driven by its end-use applications,
which include vinyl acetate monomer, purified terephthalic acid, acetic anhydride and ethyl acetate.

1.1 Acetic Acid:

Acetic acid, also known as ethanoic acid is a colorless liquid compound which is organic in nature. It is
also known as a glacial acid when it is undiluted. It has a pungent smell and sour taste.

1.1(a) Natural Occurrence:

Acetic acid is produced and excreted by acetic acid bacteria, notably the genus Acetobacter and Clostridium
acetobutylicum. These bacteria are found universally in foodstuffs, water, and soil, and acetic acid is produced
naturally as fruits and other foods spoil.

1.1(b) Synthetic Acetic Acid:

Acetic acid is majorly produced by methanol carbonylation reaction, where carbon dioxide and methanol
react to give acetic acid as a final product.

1.1(c) Properties:
Table 1.1
Chemical formula C2H4O2 or CH3COOH
Molecular weight 60.052 g/mol
Melting point 16.6 0C
Boiling point 118 0C
Density 1.05 g/ml
Flash point 40 0C
Surface tension 26.10 mN/m (250C)
dynamic viscosity 1.037 mPa.s
Specific heat (250C) 2.043 kJ/kg.K
Latent heat of vaporization 23.7 kJ/kg
Heat of formation -438.1 kJ/mol
Critical temperature 320 0C
Critical pressure 57.8 bar
Appearance Colorless crystalline.
Heat capacity 123.1 j/mol.k
Heat of combustion -876.1 kJ/mol
Triple point 16.65 0C

7
1.2Literature Survey:
As the population is growing across the globe the demand for clothes and other packed products is
increasing, which is in turn driving the growth of the packaging and textile industries that utilize Purified
Terephthalic Acid (PTA), thus contributing towards the growth of the overall acetic acid market . Vinyl
acetate monomer, which accounts for one-third of global acetic acid demand, will still be major acetic acid
end-use in the coming years. Global market is expected to grow at around 5% per year fueled by demand
increase from traditional and new application spheres
to meet the growing demand, new capacity will be introduced, mostly in China. According to 2019-2028
world market outlook and forecast the demand of acetic acid is:

Figure 1.1: Global Acetic Acid Demand By Region

Global demand for acetic acid has been steadily increasing over the last 10 years. In 2000, global acetic acid
demand stood at 6,112,418 tons, before increasing to 10,246,522 tons in 2011, as per GBI Research. A
significant portion of this increase in demand was from the Asia-Pacific region and the US, and the same
trend is expected to continue in the forecast period. USA was the second-largest consumer of acetic acid
after China in 2011, and a complete recovery in the US economy will boost the global growth of acetic acid
in the future. The Asia-Pacific region will continue to account for more than 72% of global acetic acid
demand in 2020. Global demand for acetic acid is expected to grow at a Compound Annual Growth Rate
(CAGR) of 4.7% between 2011 and 2020, to reach 15,539,000 tons in 2020. The demand for acetic acid was
highest in Asia in 2011, with China driving the majority of the demand globally. Asia accounted for more
than 60% of world consumption in 2011, and China accounted for almost 30% of that. With new capacity
coming on-line in the forecast period, China should continue to be the engine of global acetic acid growth
over the next few years. Demand in advanced countries such as Japan and Germany has largely been
stabilized. Emerging economies like China and India, because of their giant populations, have huge
consumption potential and offer tremendous growth opportunities. This is reflected in the high growth rates
seen from acetic acid downstream segments such as Vinyl Acetate Monomer (VAM), Purified Terephthalic
Acid (PTA), ethyl acetate and acetic anhydride in these countries. Asia-Pacific will continue its growth
momentum in the coming years and stands to be the global growth engine for the acetic acid market.

8
1.3 Uses:
Acetic acid is synthetic carboxylic acid having antifungal and antibacterial properties.
• A wide area of application of acetic acid in agriculture, paper, chemical, and water treatment industries
is expected to accelerate the demand for acetic acid during the forecast period and thereby, drive the
growth of the acetic acid market.
• Acetic acid is used for the treatment of outer ear infections like the growth of fungus and
bacteria. World Health Organization has listed acetic acid in its list of essential medicines.
• Acetic acid is used in vinegar, which is used as a condiment & in the pickling of raw vegetables and
other foods.
• Acetic acid is used for the manufacture of inks and dyes.
• Acetic acid is also used in making perfumes.

1.4 Process Selection:

There are many processes for the production of acetic acid having different raw materials. As our raw
material is bio-mass (wood sawdust) so there are 3 major process that are used in the production of bio-oil :

1 GASIFICATION
2 FAST PYROLYSIS
3 SLOW PYROLYSIS

And all produce 3 basic products in different quantity according to the plant source and process selection:

1 GAS
2 LIQUID
3 CHAR

1 GASIFICATION:
Gasification is a process in which materials are exposed to some oxygen, but not enough to allow
combustion to occur. Biomass gasification is a process of converting solid biomass fuel into a gaseous
combustible gas (called producer gas) consisting of carbon monoxide, carbon dioxide, hydrogen, methane,
water, nitrogen, along with contaminants like small char particles, ash and tars, through a sequence of thermo-
chemical reactions. The main product of gasification is syn gas.

2 FAST PYROLYSIS:
It is defined as the thermo-chemical decomposition of the bio-mass in the absence of oxygen. Fast pyrolysis
is the high temperature process in which the bio-mass is rapidly heated in the absence of oxygen, vaporizes and
condenses to a dark brown mobile liquid. The main product of fast pyrolysis is the bio oil.

3 Slow pyrolysis :
Slow pyrolysis is same as fast pyrolysis the only difference is that the main product of slow pyrolysis is biochar
and another difference is it take much more time as compared to the fast pyrolysis. Slow pyrolysis take several
hours to complete and fast pyrolysis take few seconds to complete the process.

9
We select our process on the bases of the yield of the bio oil therefore fast pyrolysis has the highest yield of the
bio-oil and the major part of the bio-oil is acetic acid as calculated in material balance.

Table 1.2

1.5 Process Description :

The overall process taking place is placed into 3 steps as following:
1. Pre treatment.
2. Reactor
3. Post treatment.

1.5.1 Pre-treatment:
The raw material is collected from the market to produce the bio-oil. The major source of our raw material is
wood and paper industry. For the treatment of the raw material particles size should be less than 3mm ranging
from (0.8-2mm) and getting required particle size we use chipper to reduce the particle size and then we need
to reduce the moisture content of the raw material and that should be less than 10% therefore we use dryer.

1.5.2 Reactor :
There are a variety of reactor configurations for continuous feed pyrolysis. Following are used for the pyrolysis
of bio-mass:

1. Rotating cone.
2. Bubbling Fluidized bed reactor.
3. Circulatory fluidized bed reactor.
4. Entrained flow.
5. Ablative.

We use circulatory fluidized bed reactor for our process. Reactor no 4 and 5 is laboratory scale reactors.
Rotating cone reactor have less bio-oil yield than other 2 and also its size is smaller. Circulatory bed is
highest yield of bio-oil among all the reactors and high efficiency and easy to handle than bubbling and
rotating cone reactor.

10
1.5.2(a) Process & Operating conditions:
The feed is entered from the bottom of the reactor along with the nitrogen gas, the carrier gas and also for
the inert atmosphere inside the reactor. The temperature of the reactor is 500 ℃ and pressure is 5 bar and
the residence time is 2 seconds and sand bed is used in the reactor. The feed is entered with the help of
piston pump. The temperature is set with the help of yield-temperature graph :

Figure 1.2

From this graph, we get the optimum temperature. As feed is entered from bottom and the carrier gas took
it out after 2 second from the top and this is a continuous process the thermal decomposition take place and
continuously circulated and exit after every 2 seconds.

1.5.3 Post treatment:

After reactor the raw material is converted into bio-oil , char and gas having some quantity of sand after
the reactor cyclone separator is used
Which separates the char and sand from the bio-oil and gas. Char and sand goes in the reheater where char
is burn and increase the temperature of sand and then the sand is sent back to the reactor and by this the
reactor temperature is maintained. After the cyclone separator ,condenser is used to liquify the bio-fuel and
separate the gas and oil. the coolant used in the condenser is water, and it is a partial condenser and reduce
the temperature from 500℃ to 143℃ . and at outlet we get bio-oil and bio-gas .bio oil is next send to the
distillation columns to get the acetic acid and bio gas is used as heating medium in dryer.
The next equipment is distillation column in which bio-oil is treated and we get our desired product with
13 more products. There are 2 distillation column used to get our desired product in 1 st the water and acetic
acid is removed from distillate because there boiling point are near to each other and remaining compounds
removed from bottom. The distillate of 1st column is treated in next distillation column where we get pure
acetic acid and pure water.

11
 CHAPTER 2
Material Balance

Definition:
A material balance also known as mass balance, is an application of conservation of mass to the analysis of
physical systems. By accounting for material entering and leaving a system, mass flows can be identified which
might have been unknown, or difficult to measure without this technique. The exact conservation law used in
the analysis of the system depends on the context of the problem, but all revolve around mass conservation, i.e.
that matter can neither be created nor destroyed spontaneously.

Assumptions:
There are some basic assumption that we take for the material balance. These assumptions are following.
• Rate of heat transfer, power, mass flows are constant.
• No accumulation of mass, energy in system.
• Properties in each point inside the system do not change with time (may change with position though).
• Constant temp.
• Pressure-volume changes in the reservoir are assumed to occur without any temperature changes.
We defined the breakdown of our components on the basis of literature survey. We did our material balance on
components which is given below

12
Component Material Balance:
A material balance applied around each equipment of the process to specify each inlet and outlet stream and its
components along with their masses.

1) Material balance across Dryer:

Water 31.25 ton/hr

Input Output
500 ton/hr 468.7 ton/hr

‘
500 ton/hr mass in = 5000 ton/hr mass out
We are drying out our sawdust so we could get rid of as much water as possible . As water would ruin
our product.

13
 2) Material Balance across Reactor:

Input Output
Hard wood Weight % ton/hr Products weight % ton/hr
Cellulose 0.42 197.5 Organic liquids 0.64 300
Hemi Cellulose 0.32 152.6 Gases 0.09 42.18
Lignin 0.21 98.79 Char 0.15 76.3
Water 0.04 19.68 Water 0.12 56.2

474.57 ton/hr mass In = 474.57 ton/hr Mass Out

After the pyrolysis of wood sawdust in the reactor we get same mass of product as we entered in the reactor.
The reactor is used to decompose the wood sawdust into different components.

3) Material balance across Cyclone Separator:

Input Output
Components Weight % ton/hr Components Weight Ton/hr
Organic liquids 0.64 300 Organic Liquids 0.64 300
Gases 0.09 42.18 Gases 0.09 42.18
Char 0.15 76.3 Water 0.12 56.2
Water 0.12 56.2
Cyclone
Separator

Char 0.08 9.37

Sand 0.05 23.43
Ash 0.02 37.5
474.68 ton/hr Mass In = 474.6 ton/hr Mass Out

14
We separate out few of our undesired product and impurities like char and sand in this cyclone separator and the
mass going in and coming out remains unchanged.

4) Material balance across Condenser:

Input Output
Components Weight (Ton/hr) Components Weight (Ton/hr)
Organic Liquids 0.64 300 Organic Liquids 0.64 300
Gases 0.09 42.18 Water 0.12 56.2
Water 0.12 56.2
Gases 0.09 42.18
398.38 ton/hr mass in = 398.3 ton/hr mass out
In condenser on given conditions gasses are separated from liquid by condensing the liquid down and the mass
remains same in input and output.

5) Material Balance across DC 1:

Compounds mass(ton/hr)
Water 56.25 Compounds
acetic acid 56.25 ton/hr
hydroxy Water 56.2
acetaldehyde 51.56 acetic acid 56.2
Acetol 34.68 hydroxy acetaldehyde 51.56
Furfural 5.15 Acetol 34.68
furfuryl alcohol 24.37 Furfural 5.15
Phenol 17.81 furfuryl alcohol 24.37
o-cresol 2.81 Phenol 17.81
2-ethylphenol 6.09 o-cresol 2.81
p-cresol 2.34 2-ethylphenol 6.09
m-cresol 1.87 p-cresol 2.34
Guaiacol 5.15 DC 1 m-cresol 1.87
2,4-dimethylphenol 1.40 1 Bar Guaiacol 5.15
2-methoxy-4- 2,4-dimethylphenol 1.40
methylphenol 8.90 2-methoxy-4-methylphenol 8.9
2,6- 2,6-dimethoxyphenol 22.5
dimethoxyphenol 22.5 Isoeugenol 33.75
Isoeugenol 33.75
Levoglucosan 25.31 Levoglucosan 25.31 ton/hr

15
356.19 ton/hr mass in = 356.19 ton/hr mass out
In our first distillation column levoglucosan is being separated from the rest of the products and the mass in and
mass coming out are equal. We are separating levoglucosan as its is the most heavy component and we can
separate out our other impurities at the bottom of the distillation column for further pure and efficient
separation.

6) Material Balance across DC 2:

INPUT (Ton/hr) OUTPUT( Ton/hr)

Water 56.25 Water 56.25

acetic acid 56.25 acetic acid 56.25
hydroxy acetaldehyde 51.56
Acetol 34.68
Furfural 5.15
furfuryl alcohol 24.37 hydroxy acetaldehyde 51.56
Phenol 17.81 Acetol 34.68
o-cresol 2.81 Furfural 5.15
2-ethylphenol 6.09 furfuryl alcohol 24.37
p-cresol 2.34 Phenol 17.81
m-cresol 1.87 o-cresol 2.81
Guaiacol 5.15 2-ethylphenol 6.09
2,4-dimethylphenol 1.40 p-cresol 2.34
2-methoxy-4- m-cresol 1.87
methylphenol 8.90 Guaiacol 5.15
2,6-dimethoxyphenol 22.5 2,4-dimethylphenol 1.40
Isoeugenol 33.75 2-methoxy-4-
methylphenol 8.90
2,6-dimethoxyphenol 22.5
Isoeugenol 33.75
330.88 ton/hr mass in = 330.88 ton/hr mass out
In this column we are separating acetic acid and water from rest of the product with 100 percent separation and
mass in and out remains same. We are separating acetic acid and water so that it would be easy to separate out
our final product with it. And it will be kept as simple as possible.

7) Material Balance across DC 3:

Input Output ton/hr

Water 54.54
Acetic acid 1.65

16
 water 56.25
Water
acetic acid 56.25 1.65

Acetic acid 54.54

112.5 ton/hr mass in = 112.5 ton/hr mass out

In this column we are separating our final product acetic acid from water and the mass going in and coming out
is same.

17
 CHAPTER 3
ENERGY BALANCE

3.1 Reference Conditions:-

Temperature: 500 C

Pressure: 1 Bar

3.2 Energy Balance Across Reactor:-

Identification item: Vertical Fixed Bed Pyrolysis Reactor

Function: Decomposition of Raw Material into various products

Operation: Continuous

Input:-

Mass Flow Rate Cp at 773K Temp. temp. Q=mcp∆T

(kg/day)
Wood 468750 0.0062 298 773 1380468.75
Nitrogen 144 1.1143 298 773 76218.12
468894 1456686.87
Output:-

Mass Flow Mass Cp Temp. temp. Q=mcp∆T

Rate Flow
(Tons/day) Rate
(kg/day)
acetic acid 56.25 56250 2.0146 298 773 53827594
furfural 5.15625 5156.25 1.9774 298 773 4843085.2
furfuryl alcohol 24.375 24375 2.2073 298 773 25556395
hydroxyacetaldehyde 51.5625 51562.5 1.826 298 773 44722734
acetol 34.6875 34687.5 2.1809 298 773 35933735
levoglucosan 25.3125 25312.5 3.1398 298 773 37751189
guaiacol 5.15625 5156.25 2.1958 298 773 5377994.5
2-methoxy-4- 8.90625 8906.25 2.5192 298 773 10657397
methylphenol
isoeugenol 33.75 33750 2.903 298 773 46538719
2,6-dimethoxyphenol 22.5 22500 2.5101 298 773 26826694
phenol 17.8125 17812.5 2.2334 298 773 18896658

18
o-cresol 2.8125 2812.5 2.349 298 773 3138117.2
p-cresol 2.34375 2343.75 2.343 298 773 2608418
m-cresol 1.875 1875 2.3508 298 773 2093681.3
2,4-dimethylphenol 1.40625 1406.25 2.5192 298 773 1682746.9
2-ethylphenol 6.09375 6093.75 2.2003 298 773 6368837.1
water 56.25 56250 2.15 298 773 57445313
gases 42.1875 42187.5 1.8101 298 773 36272707
char+sand 70.3125 70312.5 2.2 298 773 73476563
494018577

(mCp∆T)r - ∆HR +Q = (mCp∆T)p

Ʃ(mCp)r = 1456686.87
Ʃ(mCp)p =494018577

∆HR= -3301261918 J/hr

Cooling Water Calculation:

Cp of Water= 4.18 kJ/kmol.0C
T1= 25 C T2= 45 C
∆T= 200C
Qhot=Qcold Qcold=mCp∆T

mcold= 13438756115 mol/h Qcold= 2808700028 J/hr

Product:

Q = Ʃ(mCp∆T)p: Q= 1456686.87 J/hr

Reactant:

Q = Ʃ(mCp∆T)r: Q = 494018577 J/hr

Overall balance:

(mCp∆T)r - ∆HR +Q = (mCp∆T)p

494018577 – (-3301261918) + (-2808700028) = 3302718605
3302718605 J/hr = 3302718605 J/hr

19
Description of Cooling medium:-

Cooling Medium: (Water)

Ideal coolant must have following characteristics.
• High thermal capacity
• Low viscosity
• Low cost
• Non toxic
• Chemically inert
• Less corrosive
The most commonly used cooling medium is water. It is due to its high heat capacity and
low cost, which makes it suitable for cooling applications.

3.3 Energy Balance across Heat Exchanger:-

Identification Item: Shell & Tube Heat Exchanger

Function: Sudden decrease in the temperature

Operation: Continuous

T1= 500 C T2= 143.6 C

Mass Flow Mass Flow Cp

Rate Rate
(Tons/day) (kg/day)
acetic acid 56.25 56250 2.0146
furfural 5.15625 5156.25 1.9774
furfuryl alcohol 24.375 24375 2.2073
hydroxyacetaldehyde 51.5625 51562.5 1.826

20
 acetol 34.6875 34687.5 2.1809
levoglucosan 25.3125 25312.5 3.1398
guaiacol 5.15625 5156.25 2.1958
2-methoxy-4-methylphenol 8.90625 8906.25 2.5192
isoeugenol 33.75 33750 2.903
2,6-dimethoxyphenol 22.5 22500 2.5101
phenol 17.8125 17812.5 2.2334
o-cresol 2.8125 2812.5 2.349
p-cresol 2.34375 2343.75 2.343
m-cresol 1.875 1875 2.3508
2,4-dimethylphenol 1.40625 1406.25 2.5192
2-ethylphenol 6.09375 6093.75 2.2003
water 56.25 56250 2.15

Q(total)= 130174.42 KW

3.4 Energy Balance across Distillation Column:-

Identification Item: Distillation Column

Function: Separation of Acetic Acid and other components

Operation: Continuous

Reboiler duty:
Mass Flow Rate= 60.67
kg/sec

21
 Total heat = mλ
=21.12*39303 Total
Heat= 65441245.89
KW

Condenser duty:

Temperature = 100 OC
Latent heat of vaporization = λ=23770.47
kJ/kgmol Mass flow rate=15.6 kg/kgmol
Total heat =mλ
=23770.47 *37.078
Total heat:
Q=7064778.108 KW

Cooling water Requirement:

Inlet Temp of water= 25C

Outlet temperature= 45 C
Cp=4.18 kJ/kgmol.C
Qwater= mCpΔT

m= 881361.5505/ [79.15 *(48.89-25)]

m=466.108 kg/s
Mass flow rate of water =8389.95 kg/s

22
 CHAPTER 4
DESIGNING OF PROCESS EQUIPMENT

REACTOR DESIGN

INTRODUCTION:
Chemical reactors are basically specific apparatus used for industrial transformations
(chemical reactions) and their design is one of the well-established and developed areas of
Chemical engineering.
The reactor does not generally represent a large financial commitment in
the chemical plant, but it is technically the most important part. And it is the job of
chemical engineer to ensure the safe operation of reactor. The most significant factors
which control the behavior of a chemical reactor are briefly listed below[31]:
a) Physico chemical data on the nature of the chemicalreactions.
b) Reactionrates
c) Role of pressure and of temperature on the reaction and reactingspecies.
d) Diluted state of thespecies

• TYPES OF REACTORS:
The general types of chemical reactors which differ in design are enlisted below:

1. Fixed-Bed Reactor
2. Multi tubuler Reactor
3. Slurry Reactor
4. Moving Bed Reactor
5. Fluidized-Bed Reactor
6. Thin or Shallow Bed Reactor
7. Dispersion Reactor
8. Film Reactor
9. Continues Stirred Tank Reactor

23
 • CLASSIFICATION OF REACTORS:
Classification of chemical reactors can be achieved in two different kinds.
Depending upon the nature of reactants and product.
a. Homogeneous Reactors
b. Heterogeneous Reactors
c. Multiphase Flow Reactors
Depending upon the mode of operation
a. Batch Reactors
b. Continuous Reactors (Stirred tank reactor, Tubular flow Reactor)

Selection Criteria of Reactor

• Conversion
• Selectivity
• Yield
• Heat exchange
• Mixing
• Catalyst Distribution
• Residence Time
• Availability
• Energy utilization
• Safety
• Economics
For finding best type of reactor we should know Following things;
• Conditions in the reactor i.e.; temperature and pressure, reaction time
• Whether the reaction is exothermic or endothermic or is there any means for removal and addition of
heat.
• Whether reaction carried as batch or continuous flow process.
• Will unit operate isothermally or adiabatically.

24
• Equipment Selection:
As our process is continuous we only consider reactors for continuous and heterogeneous processes as gas,
liquid and solid phases are present
Reactors are;
Fixed and Fluidized bed reactors.

• Purpose of reactor

The Catalytic decomposition, as discussed in above chapter, is done via the use of a Fluidized bed

reactor, using nitrogen as the fluidizing as, with the use of amorphous Silica-Alumina as the catalyst.

The reactor consists of an arrangement similar to what is shown in Figure 4.1. As seen below, gases

leaving the bed also pass through a cyclone separator in order to remove entrained catalyst particles.

FIGURE 4.1: Fluidized Bed System

25
 Design of Reactor Vessel
STANDARD DESIGN PROCEDURE FOR REACTOR
• Calculate molar flow rate from given mass flow rates
• Calculate volumetric flow rate from molar flow rate
• Calculate initial concentration from volumetric flow rate
• Calculate the concentration for given conversion
• Calculate the rate of reaction by the given kinetic equation
• Calculate the residence time
• Calculate the reactor volume
• Calculate the dimensions of reactor

• MASS FLOW RATE =468750 (kg/hr)

⚫ MOLAR FLOW RATE:

MOLAR FLOW =

MOLAR FLOW RATE=3534.31(mol/hr)

⚫ VOLUMETRIC FLOW RATE

26
• KINETICS

• Initial Concentration
Ca0 =100 (mol/m3)

• Rate Constant
K= 0.5(1/sec)

• Residence Time
T =2.5 (sec)

• Order of Reaction
N=1
• Conversion
1-X = exp (-KT)
X = 0.713
X =71.3%

• Final Concentration
X = CA0 – CA/CA0
CA =28.65 (mol/m3)

• Rate law
(-rA)= k Ca
(-rA) =14.32 (mol/m3.sec)
• Volume OF reactor (PFR)

• Diameter of Reactor
D = 1 (m2)

27
• Area OF Reactor

• Length of Reactor

Figure 4.2: Conversion verses Rate curve

BED DESIGN
• Terminal velocity

• Minimum Fluidized velocity

• Fluidized velocity

• Cross sectional area

• Void fraction of bed

• Flow rate at minimum velocity

28
 • Flow rate at fluidized velocity

• Flow rate at terminal velocity

• Pressure drop

BEDS DESIGN SPECIFICATION

Gravitational acceleration 9.8 m/sec2
Density of particle 1680 kg/m3
Density of fluid 100 kg/m3
Diameter of fluid 0.0018 m
Viscosity of fluid 0.000055 cp
Bed height 0.025 m
Void fraction of bed 0.5
Sand weight 2.5 kg/m3
Flow rate of sand 200 kg/sec

Terminal velocity:

𝒈(𝒑 − 𝝆𝒇 ) 𝒅𝟐𝒑
𝑼𝒕 =
𝟏𝟖µ𝒇

Ut =50.6 m/sec

⚫ Minimum Fluidized Velocity

Umf = Ut/52
Umf = 0.974 (m/sec)

⚫ Fluidized Velocity

(𝜌𝑝 − 𝜌𝑓 )𝑔𝑑𝑝2 ɛ3
𝑢𝑓 =
150µ 1−ɛ

29
 Uf = 1.52 (m/sec)

⚫ Void Fraction of Bed

ϵ= 0.5 (literature)

⚫ Cross Sectional Area

Whereas D=0.0018m

A=2.54E-06 m2

⚫ Flow rate at minimum velocity

φ = AUmf

=2.47977E-06 m3/sec

⚫ Flow rate at fluidized velocity

φ= AUf

=3.86844E-06 m3/sec

⚫ Flow rate at terminal velocity

Φ = AUf

= 0.000128948 m3/sec

⚫ Pressure Drop
△𝑷
= (𝝆𝒔 − 𝝆𝒇 )(𝟏 − ɛ)𝒈
𝒉

Whereas; ∆P= 0.0019355 bar

30
Table 4.1

31
 Cyclone Separator Design
Cyclone separators provide a method of removing particulate matter from air or other gas streams at low cost
and low maintenance. Cyclones are somewhat more complicated in design than simple gravity settling systems,
and their removal efficiency is much better than that of settling chamber. Cyclones are basically centrifugal
separators, consists of an upper cylindrical part referred to as the barrel and a lower conical part referred to as
cone.

Figure 4.3: Cyclone Separator

Designing Parameters:
⚫ Inlet Flow Area

G=Density x u x Ai
⚫ Diameter of Separator

Ai=0.5Dc x 0.2Dc

32
 ⚫ Efficiency

n= dpc/dp X 100
⚫ Number of Turns Inside the Cyclone

Nc=(1/Hc) X (Lc+Zc/2)

⚫ Preliminary Calculations to Determine Overall Size of Separator:

⚫ Volume
⚫ Diameter of Gas outlet duct

D0=0.5 X Dc
⚫ Length of Body

Lc=1.5 X Dc

⚫ Length of Cone (L/D=0.6)

Zc=2.5 X Dc

• Other Important Consideration

⚫ Pressure Drop Calculation

∆P=a*density*(Vi^2/2) = 2.8 kPa (Allowable= Below kPa)

Whereas:

a= (16 X W X Hc)/(Dc/2)^2
W= Dc/4
Hc= Dc/2
Vi= Q/(HC X W)
Q= Volumetric Flow Rate

33
Figure 4.4: Cyclone separator

34
Figure 4.5

35
 Condenser Design

⚫ Condenser is a device or unit used to condense a substance from its gaseous to its liquid state or reduce
the temperature of hot fluid, by cooling it.

There are 3 types of water condensers that we generally use:

1. Shell and tube.

2. Tube and tube.
3. coil and tube.

Selection Criteria

1. Select shell and tube heat exchanger because only shell and tube use for phase change and other
two are use for reducing the temperature.
2. In shell and tube , we select spilt ring floating head type because it is easy in cleaning and also
consume less area for as compare to other types.
3. Select 1-8-passes.
4. Hot fluid (organic solvents) on shell side and cold fluid (water) on tube side.
5. Select square pitch because fluid is corrosive.
6. Select 25 baffle cut.

Thermophysical Properties:
Table 4.2
INLET OUTLET
TEMPERATURE TEMPERATURE

500 © (HOT) 25© 143© (HOT) 45© (COLD)

COLD FLUID At 35© HOT FLUID (organic At 321.595©

(water) vapors)
Density 993 kg/m3 Density 1.927 kg/m3

Cp 4.21 kj/kg.k Cp 2.052 kj/kg.k

Viscosity 0.0008 N/s m Viscosity 0.00002 N/s m

Mass flowrate 1527.69 kg/sec Mass flowrate 97.786kg/sec

Overall heat transfer coefficient assumed 500 w/m2 © range = 500-700

36
 Design Steps

▪ Calculate the Heat Duty.

▪ Calculate the tube Pitch
▪ Calculate tube clearance.
▪ Calculate tube side cross sectional area.
▪ Calculate tube per pass.
▪ Calculate tube side flow area.
▪ Calculate tube mass velocity.
▪ Calculate Reynolds number.
▪ Calculate tube side heat transfer co-efficient.
▪ Calculate baffle spacing.
▪ Calculate number of baffles.
▪ Calculate equivalent diameter.
▪ Calculate shell side mass velocity.
▪ Calculate linear velocity.
▪ Calculate Reynolds number.
▪ Calculate prandtl number.
▪ Calculate nussetl number
▪ Calculate shell side heat transfer co-efficient.
▪ Calculate the overall heat transfer co-efficient.
▪ Find the friction factors for tube and shell side.
▪ Calculate the pressure drops on both sides.

FIGURE 4.6: PROCESS FLOW DIAGRAM

37
 FIGURE 4.7: TEMPERATURE PROFILE

DESIGN STEPS
HEAT DUTY:
Q=7064778.108 KW

38
Bundle Diameter
Db =10 m

39
Equipment Design

Reynolds’s Number:
𝑑𝑖 × 𝐺
𝑅𝑒 =
µ
=6592.626
Tube side heat transfer co-efficient:

4200(1.35+0.02t)U2t
hi=
d0.2
i

=963.126 w/m2C

40
Tube side pressure drop:

Np = no of passes = 8
Fr = friction factor = 0.013
Pressure drop = 0.244 psi

𝐋 𝛍 −𝐦 𝐮𝟐𝐭
∆𝐏 = 𝐍𝐩 [𝟖𝐣𝐟 ( )( ) + 𝟐. 𝟓]
𝐝𝐢 𝛍𝐰 𝟐

𝟐
𝐏 −𝛑𝐝𝐨 𝟐
𝟒( 𝐭 )
𝟒 𝟏.𝟐𝟕
De=
𝛑𝐝𝐨
=
𝐝𝐨
(𝐏𝐭𝟐 − 𝟎. 𝟕𝟖𝟓𝐝𝟐𝐨 )

De = 0.037 m

41
Reynolds’s number:
𝒅𝒆 × 𝑮𝒔
𝑹𝒆𝒔 =
µ

= 8766.144

Prandtl number:

𝑪𝑷 × µ
𝑷𝒓 =
𝒌
= 138.744

Nusselt number:

1 0.14
ho De 0.55 3 μ
= 0.36𝑅𝑒 Pr ( )
k μw

Nu = 2454.37

𝐝𝐨
𝟏 𝟏 𝟏 𝐝𝐨 𝐥𝐧 ( ) 𝐝 𝟏 𝐝𝐨 𝟏
𝐝𝐢 𝐨
= + + + ⨯ + ⨯
𝐔𝐨 𝐡𝐨 𝐡𝐨𝐝 𝟐𝐤 𝐰 𝐝𝐢 𝐡𝐢𝐝 𝐝𝐢 𝐡𝐢

42
 Shell side pressure drop:
𝐷𝑠 𝐿 𝜌𝑢𝑠2 𝜇 −0.14
∆𝑃𝑆 = 8𝑗𝑓( )( ) ( )
𝑑𝑒 𝑙𝐵 2 𝜇𝑤

Jf = 0.08

Pressure drop = 0.33 psi

43
Figure 4.8

44
Distillation Column Design
⚫ Distillation is a process in which a liquid or vapor mixture of two or more substances is separated into
its component fractions of desired purity.
⚫ Binary distillation column is used to separate two components (Component A & component B) .
Example for Binary mixture is Acetic acid and water. Which we are separating in the following column
design.

⚫ Types of Distillation Columns:

There are numerous types of distillation columns, each designed to achieve precise types
of Separation, and each design differs in terms of complexity.

⚫ Batch Columns:
In batch operations, the feed to the column is introduced in batch wise. That is the column
is charged with a batch and then the distillation process is carried out. When the desired
task is achieved a next batch of feed is introduced.

⚫ Continuous Columns:
In contrast, continuous columns process a continuous feed stream. No interruption occurs
unless there is a problem with the column or surrounding process units. They are capable
of handling High throughputs and are the more common of two types. We shall
concentrate only on this class of columns.

CHOICE BETWEEN PLATE AND PACKED COLUMN:

Vapor liquid mass transfer operation can be performed either in a plate column or in a
packed column and that Two types of operations are totally different.
Comparison between Plate and Packed Column

Table 4.3
Comparing Parameters Plate Packed
Column Column
Provision for cooling Easy Difficult
Provision for side stream Easy Difficult
Provision for cleaning Easy Difficult

45
 Liquid Holdup High Low
Corrosive Fluid handling Costly Cheaper
Foaming system handling Not suitable Suitable
High Temperature application Suitable Not suitable

For this particular process, I have selected plate column because:

i) System is non-foaming.
ii) Temperature is very high i.e. about260°C

⚫ CHOICE OF DISTILLATION TYPE:

Vacuum distillation is considered when the boiling
point of the compound (or the solvent) is very high (Tb>150oC) in order to distill the
compound without substantial decomposition. Vacuum distillation is the distillation of
liquids achieved at a pressure under atmospheric pressure to take benefit of the statement
that decreasing the pressure depresses the boiling point of liquids.
The distillation process that take place under one atmosphere and in vacuum is known as
vacuum distillation. Low pressure allows vaporization at low temperatures. Due to this,
heating and cooling both needs fewer energy and make it energy effective process.

⚫ CHOICE OF PLATE TYPE

There are four main tray types, the bubble cap, sieve tray, ballast or valve trays and the
counter flow trays. I have selected sieve tray because
comparison between plate types

Comparing Sieve Plate Bubble Cap Valve Plate

Parameters Plate

Cost Low High Moderate

Capacity High Low Low

Pressure Drop Low High Moderate

Fouling Low High High

46
 • DESIGNING STEPS OF DISTILLATION COLUMN:
Steps for design of Distillation Column are following.
▪ Bubble point and Dew point calculation

▪ Minimum Reflux RatioRm.

▪ Optimum reflux ratio.
▪ Theoretical number of stages.
▪ Actual number of stages.
▪ Diameter of the column.
▪ Weeping point.
▪ Residence time.
▪ Pressure drop.
▪ The height of the column.
⚫ Number of plates at total Reflux
𝑥 𝑥
log [𝑥 𝑙𝑘 ] 𝑑 [ 𝑥ℎ𝑘] 𝑏
ℎ𝑘 𝑙𝑘
= 10.95
log 𝑎𝑙𝑘

⚫ Minimum reflux ratio by colmer method

Rm = 0.68
⚫ Optimization of number of plates and total reflux and total reflux
Table 4.4
R R/R+1 Nm/N N
2 0.66667 0.82 13.3598
3 0.75 0.88 12.44
4 0.8 0.92 11.9

47
From figure:

Figure 4.9
We find the value of N through this graph. By using this graph we find Nm/N and after this by calculation we
find the value of N.

48
 ⚫ Feed plate location
LogNr/Ns = 0.206 log [b/d*(xfHK/xfLK)*(xbLK/xbHK)^2] =0.199522

Nr/Ns =1.583151 Nr =8.187816

Nr +Ns= 13.35983 Ns = 5.172014

Liquid Vapor flow factor (k mole/sec)

⚫ Flooding Velocity

49
Figure

Figure 4.10
From this graph we will find K1 which is used to find flooding velocity by tracing the lines of
Flv and our plate spacing.

50
⚫ Maximum volumetric Flowrate

⚫ Net Area Required

⚫ Column Cross Sectional Area

Take downcomer area as 20% of total

⚫ Column Diameter

51
⚫ Provisional Plate Design

⚫ Down Comer Area

Ad = 0.20* Ac = 1.50433 m2

Net Area = An = Ac –Ad = 6.0173 m2

Active area = Aa = Ac - 2Ad = 4.51299 m2

Hole area =Ah = Take 20 % of Aa = 0.20*Aa = 0.9025 m2

From fig below (fig 11.31 Coulson and Richardson) Calculate

Weir length = Lw = 2.6620 m

Figure 4.11

52
From this figure we will calculate our weir length by tracng the line and then calculating lw as
we already know the value of Dc.

⚫ Check weeping

From figure
Actual Vapor Velocity= minimum vapor rate/ Ah = 21.56

53
 Figure 4.12
From this figure we will find the value of K2 which would be used to ceck our weeping in the
distillation column.

Plate Pressure Drop

From figure

54
 Figure 4.13
From this figure we will find our Co as we already know our other values . we fill find this by
tracing our lines . Co will help us find our plate pressure drop.

⚫ Down comer Pressure loss

55
 ⚫ Check residence time

⚫ Check Entrainment

From figure

Figure 4.14

56
From this figure we will find ᵠ

⚫ Column Height
Top clearance = 1m

Bottom clearance = 1m

H = (Actual num of trays+1)*tray spacing+ top clearance +bottom clearance+

plate thickness .

H = 14.9288 m

Table 4.4

Specification sheet for distillaion column

Identification Specification

Column dia 3.095437444 m

Area of column 7.521660379 m2

Height 14.92884704 m

Minimun Reflux Ratio 0.680239172

Reflux Ratio 2

Feed tray(from top) Feed would b given at 5th plate

Operating Pressure 1 atm

Number of trays 13.35983004

Tray spacing 0.9 m

Weir height 100 mm

Weir length 2.662076201 m

L/D 4.82285535

Tray type Sieve tray

Distlltion type Binary

57
 CHAPTER 5
COST ESTIMATION

Economic Analysis
5.1Introduction[10]

Before the plant to be operated, specified money must be supplied to purchase and install the
equipment. The capital needed to supply the necessary plant facilities is called fixed capital
investment while that for the operation of the plant is called the working principal and sum of
two capitals is called total capital investment.
An acceptable plant design must present a process that is capable of operating under conditions
which will yield a profit. Since, Net profit total income-all expenses it is essential that chemical
engineer be aware of the many different types of cost involved in manufacturing processes.
Capital must be allocated for direct plant expenses; such as those for raw materials, labor, and
equipment. Besides direct expenses, many other indirect expenses are incurred, and these must
be included if a complete analysis of the total cost is to be obtained. Some examples of these
indirect expenses are administrative salaries, product distribution costs and cost for interplant
communication.

5.2 Fixed Capital Investment

Manufacturing fixed capital investment represents the capital necessary for the installed process
equipment. With all auxiliaries that are needed for the completeprocess operation. Expenses for
piping, instruments, installation, and foundation and site preparation are typical examples of cost
included in the manufacturing fixed capital investment. Fixed capital required foe the
construction overhead and for all plant components that are not directly related to the process
operation is designed as the non-manufacturing fixed capital investment.

58
5.3 Working Capital
The working capital for an industrial plant consists of the total amount of the money invested in:
Raw material and supplies carried in stock.
Finished products in stock and semi finished products in the process of being manufactured.
Accounts receivable
Cash kept on hand for monthly payments of operating expenses, such as salaries, wages and raw
material purchases.
Accounts payable
Taxes payable

5.4 Cost Index

It is an index value for a given point in time showing the cost at that time relative to certain base
time. if the cost at any time in past is know, the equivalent cost at the present time can be
determined by multiplying the original cost by the ratio of present of index value to the index
value applicable when the original cost was obtained. There are many types of cost indexes and
the most commune type are Marshall and swift all industry and process industry equipment
indexes and engineering News Record construction index.
Present cost = Original cost × cost index value at present time/cost index value at past

5.5 Purchase Equipment Cost

Distillation Column
Average diameter of plate = 0.69 m
Cost of sieve plates = 275 $
No. of plates = 22
Cost of plates = (22×275) $
= 6,050$
Installed cost = 3800 $ per plate
= (22×3800) $
= 8,3600
Total cost (purchased) = 6050 + 83600

59
 = 89,650 $ (based on 2002)
Cost in 2010 = 89,650*525/395.6
= 118,974.34 $

Equipments Total Cost

Equipment Cost of equipment

Distillation Column $118,974.34

Reactor $28000
Vaporizer $15000
Scrubber $35260

Total Cost = $ 197,234

Direct Cost
Purchased equipment cost, E = $197,234
Installation cost (8.3%E) = $16370
Instrumentation and control cost (9.2%E) = $18145
Piping cost (7.3% E) = $14398
Electric cost (4.6%E) = $9073
Building (including services) (4.6%E) = $9073
Yard improvement (1.8%E) = $3550
Land cost (2%E) = $3944
Total Direct Cost = $271,787

Indirect Cost
Engineering and Supervision Cost (7.3%E) = $14398
Construction Expenses (9.2%E) = $18145
Contractor fee (1.8%E) = $3550
Contingency Cost (7.3%E) = $14398
Total Indirect Cost = $50,491
Total Capital Investment

60
Fixed Capital Investment = Direct cost + Indirect cost
F.C.I = D.C + I.C
F.C.I = $271,787+ $50,491
F.C.I = $322,278
Working Capital (18%F.C.I) = $58,010
Total Capital Investment = Working Capital Cost + Fixed Capital Investment
T.C.I = W.C + F.C.I
T.C.I = $58,010 + $322,278
T.C.I = $380288

5.6 Product Cost

Assume that the Fixed Capital Investment depreciate by straight line method for 20 years.
Assuming 5 % Salvage value at the end of plant life,
Depreciation = D = (V-VS)/N
V = F.C.I
V = $322,278
VS = 0.05*F.C.I
VS = $16,113.9
N = no. of years = 20
D = $15,308
Total Product Cost = Total Capital Investment – Depreciation
= $380,288– $15,308
T.P.C = $364,979
Fixed Charges (12%T.P.C) = $43,797
Direct Product Cost (55%T.P.C) = $200,738
Plant Overhead (10%T.P.C) = $36,498
Manufacturing Cost = Direct product cost + Fixed Charges + Plant Overhead Cost
Manufacturing Cost = $281,033
General Expenses
General Expenses = Administrative Cost + distribution and selling cost + research and
development cost

61
Administrative Cost
It is 2-6% of total product cost
Consider
Administrative cost = 5% of total product cost
Administrative cost = $18,240

Distribution and Selling Cost

It includes cost for sales offices, salesmen, shipping, and advertising.
It is 2-20% of total product cost
Consider that
Distribution and selling costs = 15% of total product cost
Distribution and selling costs = $54,719

Research and Development Cost

It is about 5 % of total product cost
Research and development cost = $18,240

Financing (Interest)
It is about 0-10% of total Capital Investment
Consider interest is 5% of total capital investment
Interest = $19,014
Thus,
General Expenses = $110,21
So,
Total product cost = Manufacturing cost + General Expenses
Total product cost = $281,033 + $110,21
Total product cost = $391,246

62
 CHAPTER 6
HAZOP STUDY

6.1 What is HAZOP?

A Hazard and Operability (HAZOP) study is a structured and systematic examination of a

planned or existing process or operation in order to identify and evaluate potential hazards and
operability problems. Or to ensure the ability of equipments in accordance with the design intent.

The HAZOP analysis technique uses a systematic process to identify possible deviations
from normal operations and ensure that appropriate safeguards are in place to help prevent
accidents. It uses special adjectives combined with process conditions to systematically consider
all credible deviations from normal conditions. The adjectives, called guide words, are a unique
feature of HAZOP analysis.

63
6.2 Brief Summary Of Characteristics:

A HAZOP study is conducted in the following steps:

Figure 6.1

64
6.3 Potential hazards AND operability problems:

You will note the bold AND in the above handing, it’s because high profile of production plant
accident, emphasis is too often placed upon the identification of hazards to the neglect of
potential problems. Yet it is the latter area that benefits of HAZOP study are usually the greatest.

6.4 Key Words:

An essential feature in this questioning and systematic analysis in the use of Key words to focus
the attention of the team upon deviations and their possible causes. The key words are divided
into two subsets.

Primary key words: which focus upon a particular aspect of the design intent or an associated
process condition or parameter.

Secondary key words; which when combined with a primary key word, suggest possible
deviations. The entire technique of HAZOP revolves around the effective use of key words, so
their meaning and use must be clearly understood by the team. Example often used key words
are listed below.

6.5 Limitation of the HAZOP Technique:

• Requires a well-defined system or activity

• Time consuming
• Focuses on one-event causes of deviations

65
6.6 HAZOP STUDY OF WHOLE PLANT:
CHIPPING

DEVIATION CAUSE CONSEQUENCES ACTION

RECOMMENDED
BLADE RPM LESS ELECTRICAL WOOD WILL PLACE SENSORS
RPM FAULTS NOT BE OF TO DETECT
/POWER ENOUGH MESH POWER
SHORTGE SIZE SHORTAGE
RPM MORE ELECTRICAL ENERGY CONTROLED
FAULTS / WASTAGE RPM
UNCONTROLED
RPM
NO RPM TECHNICAL NO CHIPPING REGULAR
DEFCIENCY CHECKUP
/DISABILITY

DRYER

DEVIATIO CAUSE CONSEQUENCE ACTION

N S RECOMMENDED
FLOWRATE LOW VALVE NOT NOT ENOUGH GREASING
FLOWRAT FULLY OPEN DRYING VALVES
E
HIGH UNCONTROLED CARRY AWAY INSTAL
FLOWRAT VALVE WOOD CONTROLERS
E SAWDUST
NO PUMP DAMAGE NO DRYING REGULAR
FLOWRAT CHECKUP /
E REPAIR PUMP
TEMPERATUR LOW TEMP HEATING COIL NOT ENOUGH INTALL
E NOT WORKING DRYING SENSORS LIKE
WELL THERMOCOUPLE
S
HIGH UNCONTROLLE ENERGY INSTALL
TEMP D HEATING WASTAGE CONTROLLERS

PYROLYSIS REACTOR

DEVIATIO CAUSE CONSEQUENCE ACTION

N S RECOMMENDE
D
FLOWRATE LOW VALVE NOT REACTION VALVE

66
 FLOWRAT FULLY OPEN WILL CHECKUP /
E PROCEEED IN INSTALL
OTHER SENSORS
DIRECTION
HIGH UNCONTROLLE REACTION INSTALL
FLOWRAT D PUMPING WILL NOT BE CONTROLLERS
E COMPLETED
TEMPERATUR LOW TEMP HEATER NOT RECTION WILL INSTALL
E DOING WELL PROCEED IN SENSORS
OTHER
DIRECTION
HIGH UNCONTROLED REACTION INSTALL
TEMP HEATING WILL PROCEED CONTROLLERS
IN OTHER
DIRECTION
PRESSURE LOW PUMP NOT DESIRED INSTALL
PRESSURE DOING WELL REACTION SENSORS AND
WILL NOT STANDBY
OCCUR PUMPS
HIGH UNCONTROLLE REACTOR INSTALL
PRESSURE D PUMPING MIGHT CONTROLLERS
RUPTURE OR
EXPLODE

CYCLONE SEPERATOR

DEVIATION CAUSE CONSEQUENCES ACTION

RECOMMENDED
FLOWRATE LOW VALVES ARE SEPERTION INSTALL
FLOWRATE NOT OPEN WILL NOT SENSORS
PROPERLY OCCUR
PROPERLY
HIGH UNCONTROLLED ASH MAY GET INSTALL
FLOWRATE PUMPNG CARRIED STANDBY
AWAY/ ENERGY PUMPS AND
WSTAGE COTROLLERS
NO PUMP IS NO SEPERATION REAGULAR
FLOWRATE DAMAGED CHECKUP

CONDENSOR

DEVIATIO CAUSE CONSEQUENCE ACTION

N S RECOMMENDE
D

67
TEMPERATUR LOW TEMP UNCONTROLLE ENERGY CONTROLED
E D SUPPLY WASTAGE SUPPLY
HIGH LESS SUPPLY OF IMPROPER INSTALL
TEMP COOLENT CONDENSATIO SENSORS AND
N CONTROLLERS
FLOWRATE LOW VALVE NOT ENOUGH INSTALL
FLOWRAT CONTAMINTION CONDENSATIO SENSORS/
E N CONTROLLERS
HIGH IMPROPER ENERGY INSTAL
FLOWRAT PUMPING WASTAGE CONTROLLERS
E

DISTILLATION COLUMN

DEVIATIO CAUSE CONSEQUENCE ACTION

N S RECOMMENDE
D
TEMPERATUR LOW TEMP REBOILER NOT IMPROPER ISTALL
E DOING WELL DISTILLTION SENSORS
HIGH UNCONTROLLED IMPROPER INSTALL
TEMP HEATING DISTILLATION CONTROLLERS
/REGULAR
CHECKUP
FLOWRATE LOW VALVE WILL CAUSE INSTALL
FLOWRAT CONTAMINATIO WEEPING SENSORS /
E N CONTRLLERS
HIGH UNCONTROLLED WILL CAUSE INSTALL
FLOWRAT PUMPING FLOODING CONTROLLERS
E /REGULR
CHECKUP

PUMP

DEVIATION CAUSE CONSEQUENCES ACTION

RECOMMENDED
FLOWRATE LOW VALVE PERODUCT REGULAR
FLOWRATE CONTAMINATION WILL BE CHECKUP/
/ NOT OPEN AFFECTED CLEANING
PROERLY
HIGH UNCONTROLED ENERGY INSTALL
FLOWRATE PUMPING WASTAGE CONTROLLERS

68
COMPRESSOR

DEVIATION CAUSE CONSEQUENCES ACTION

RECOMMENDED
PRESSURE LOW PISTONS NOT NOT ENOUGH REGULAR
PRESSURE WORKING WELL FLOWRATE AS CHEKUPS
REQUIRED /CLEANING/
INSTALLATION
OF SENORS
HIGH UNCONTROLLED RUPTURE INSTALLATION
PRESSURE COMPRESSION /EXPLOSION OF
CONTROLLER

69
 CHAPTER 7
INSTRUMENTATION AND
CONTROL

7.1 Various Control Loops[12]

7.1.1 Feedback Control Loop:
Consider the general process shown in Figure 1
Disturbance

Manipulated Output
Variable Process
Figure 8.1.1(a)

It has an output, a potential disturbance, and an available manipulated variable. The disturbance
(also known as load or process load) changes in an unpredictable manner and our target is to
keep the output variable at a fixed value, that is to offset the effect of the disturbance. A feedback
control action takes the following steps;
1. Measure the value of the output (flow, pressure, liquid level, temperature, composition)
using the appropriate measuring device.
2. Compares the indicated value to the desired value (the set point) of the output. The
deviation is computed and is termed as the difference between the set point and the
measured value .
3. The value of the deviation is supplied to the main controller. The controller in turn
changes the value of the manipulated variable so as to minimize the deviation. Usually,
the controller does not effect directly with the manipulated variable but through another
device

70
 ( known as the final control element) which in most cases is a control valve.
The foregoing three steps are summarized in the Figure8.1.1(b)

Figure 8.1.1(b)
The system in Figure 8.1.1(a) is known as the open loop, in contrast to the feedback control
system shown in the Figure 8.1.1(b) which is known as the closed loop. Also, when the value of
disturbance or manipulated variable changes, the response of the first is open loop response and
the response of the second is called the closed loop response.
8.1.2Feedforward Control Loop
Feedback control loops can never achieve perfect control of a chemical process, that is, keep the
output continuously to the desired step at the desired set point value in the presence of load or set
point changes. The reason is simple: A feedback controller reacts only when it has felt a
detection of deviation of the output value from the set point value.
Unlike the feedback systems, a feed forward control loop measures the disturbance (load)
directly and takes a control action to eliminate its impact on the process output. Therefore, feed
forward controllers have theoretical potential for perfect control.

8.1.3 Logic Of Feed forward Control

Consider the stirred tank heater shown in Figure 8.1.3(a)

71
 Figure 8.1 .3(a) Stirred Tank Heater

The control objective is to keep the temperature of the liquid in the tank at a desired value (set
point) despite any changes of temperature in the incoming stream. Figure 8.1.3(b)

Figure 8.1.3(b) Feedback Temperature Control For A Stirred Tank Heater

72
shows the conventional feedback loop, which measures the temperature in the tank and after
comparing it with the desired value, increases or decreases the steam pressure, thus providing
more or less heat into the liquid. A feed forward control system uses a different approach. It
measures the temperature of the inlet stream (disturbance) and adjusts appropriately the steam
pressure ( the manipulated variable). Thus it increases the steam pressure if the inlet temperature
goes down and decreases the steam pressure if the inlet temperature goes up.

8.1.5 Simple Feedback Control

If we use simple feedback, we will take the control configuration as shown in Figure 8.1.5(i.e.
measure temperature Tand manipulate the coolant flow rate Fc ).

Figure 8.1.5 Feedback Temperature Control Of ACSTR With Cooling Jacket

It is clear that will respond to changes in Ti much faster as compared to changes in Tc. Therefore,
the simple feed backward control of Figure 9will be very compensating for changes in Ti and
less effective for compensating in changes in Tc.

73
8.2 DISTILLATION CONTROL OBJECTIVES:
The starring point of any design project is a definition of objectives. For distillation there are
many possible approaches, but the one chosen here is one the authors have found broadly useful
in virtually all kinds of processes. It has three main facets:
1) Material-balance control
2) Product quality control
3) Satisfaction of constraints
As applied specifically to distillation columns, this philosophy suggests the following:
8.2.1 Material-balance control:
This term is sometimes used to mean a control system in which reflux is set by reflux drum level
control, and distillate feed ratio is set manually or by a composition (temperature) controller.
Column holdup and overhead and bottoms inventories should be maintained between maximum
and minimum limits. It is important to note that the material-balance controls on any given
column must be consistent with the material-balance controls on adjacent process equipment. In
most cases material balance will be controlled by so-called “averaging” liquid-level or pressure
controls

8.2.2 Product quality control:

The control system for a binary distillation in most cases must:
• Maintain the concentration of one component in either the overhead or bottoms at a
specified value.
• Maintain the composition at the other end of the column as close as possible to a desired
composition.
It is usually true that minimum operating cost is achieved when the products are controlled at
minimum acceptable purities. This is so because the relationship between thermodynamic work
of separation and purity is nonlinear.” For some columns compositions are allowed to vary at one
end, and sometimes both ends, to satisfy certain economic constraints.
Both material-balance and composition controls must function satisfactorily
in the face of possible disturbances in:

• Feed flow rate

• Feed composition

74
 • Feed thermal condition
• Steam supply pressure
• Cooling-water supply temperature
• Cooling-water header pressure
• Ambient temperature, such as that caused by rainstorms
8.2.3 Satisfaction of constraints
For safe, satisfactory operation of the column, certain constraints must be observed. For
example:
The column shall not flood.
• Column pressure drop should be high enough to maintain effective
• Column operation, that is, to prevent serious weeping or dumping.
• The temperature difference in the reboiler should not exceed the critical temperature
difference.
• Column feed rate should not be so high as to overload reboiler or condenser heat-transfer
capacity.
• Boil up should not be so high that an increase will cause a decrease in product purity at
the top of the column.
• Column pressure should not exceed a maximum permissible value.

Several other facts of column control:

There are, in addition, several other facets of column control.
• Startup and Shutdown
• Column controls should facilitate startup and shutdown and, by implication,
• Transitions
• When it is desired to change product compositions, the column control should facilitate
doing so. This is particularly important when feed stock composition varies widely and it
is desired to optimize column or train operation, as, for example, with a computer.

75
7.3 Distillation Column Control:

Figure: Control Loops on Distillation Column

76
References:

1.Harold Gunardson,‘‘Industrial Gases In Petrochemical Processing”, chap#5, Marckel

Dekker, INC., United States Of America, 1998.

2. Chenier, PhilipJ, “ Survey Of Industrial Chemistry” , Third Edition, chap#9, Kluwer

Academic/Plenum Publishers, 233 Spring Street New York, 2002.

3. Agredaetal,V.H, “ Acetic Acid And Its Derivatives”, chap#12, Marckel Dekker, INC.,
United States Of America, 1993.

4. Reid,C.Reid, etal “ The Properties Of Gases And Liquids”, Second Edition, chap#7,
McGraw Hill Book Company,United States Of America, 1966 `.

5. Smith, J.M, “Chemical Engineering Kinetics”, Third Edition, McGraw Hill

International Addition,1981.

6. Kern,D.Q, “ Process Heat Transfer”, International Student Edition, United States Of

America.

7. Rase,F,. “ Fixed Bed Reactor Design And Diagnostics”, Chap.5, Butterworth Publishers,
United States Of America, 1990.

8. StanleyM.Walas, “Reaction Kinetics For Chemical Engineers”, International student

edition,Chap.8, McGraw Hill Book Company,Kogakusha company limited Tokyo,1959.

9. Willard H. Gehrke, Menasha, Wls., ( To Monsanto Chemical Co.), U.S Patent 2,485,044
(October 18,1949).

10. B.O Kruger etal. U.S Patent 3,652,659 (March 28, 1972)

11. Peters,Max S. etal., “ Plant Design And Economics For Chemical Engineers”, 5th
Edition, University Of Colarado.

12. George Stephanopoulos,“ Chemical Process Control”, Prentice Hall Of India Private
Limited, New Delhi,2000.

77
12. Ernest J. Henley, ETAL.,˝Equilibrium-Stage Separation Operations in Chemical
Engineering” CH # 12,John Wiley & Sons ,1996.

13. Coulson & Richardson’s, “Coulson & Richardson’s Cemical Engineering” Volume 6 th .
4thed, Ch # 2, Butterworth-heinemann,2003.

14. Coulson & Richardson’s, “Coulson & Richardson’s Cemical Engineering” Volume 2 th .
5thed, Ch # 11, Butterworth-heinemann,2002.

15. Ernest J. Henley, et-al., “Equilibrium-Stage Separation Operations in Chemical

Engineering” CH # 12,John Wiley & Sons ,1996.

16. Ernest E. Ludwig, “Applied Process Design for Chemical and petrochemical
plants”Volume2,Third ed. Butterworth-heinemann,1979.

17. Zhigang Lei, et-al. “Separation Distillation Processes” 1sted. ELSEVIER. 2005.

18. Robert H. Perry, et-al. “Perry Chemical Engineering Handbook” 7th ed. McGraw-
Hill,1997.

19. Robert H. Perry, et-al. “Perry Chemical Engineering Handbook” 6th ed. McGraw-
Hill,1997.

20.Henry Z. Kister, “Distillation Operation” McGraw -Hill

21. Treybal: “Mass Transfer Operations” McGraw Hill.

22. Ulman , “Chemical Engineering Encyclopedia”

23. McKetta“ Encyclopedia of Chemical Processing and Design”

24.Charles A. Defazio, ETAL., ( Celanese Corporation, New York), U.S Patent 3,551,299
(December 29,1970).
25.Henry Z. Kister, “Distillation Design” McGraw -Hill

78