Design Project On Nitric Acid Production

1
PLANT DESIGN FOR THE PRODUCTION OF
400,000 METRIC TONNES OF NITRIC ACID
PER ANNUM FROM AIR OXIDATION OF
AMMONIA GAS
BY
ANDREW OFOEDU
DEPARTMENT OF CHEMICAL
ENGINEERING
FEDERAL UNIVERSITY OF TECHNOLOGY,
OWERRI.
SEPTEMBER 2013
2
EXECUTIVE SUMMARY
This report describes the detailed design of a plant to produce

400000 tonnes of nitric acid per year by Ostwald Process. The
single pressure process was selected as the most advantageous,
having considered several factors one of which is efficient energy
management. The process begins with the vaporization of
ammonia at 1000 kPa and 35°C using process heat. Steam is then
used to superheat the ammonia up to about 80°C. Filtered air is
compressed in an axial compressor to a discharge pressure of
about 740kPa and temperature of 155°C. Part of the air is
diverted for acid stripping. This preheated air and the ammonia
vapour are then mixed and passed through the platinum/rhodium
catalyst gauze in a converter for oxidation. The reaction gas flows
through a series of heat exchangers for recovery of energy as
either high-pressure superheated steam, or as shaft horsepower
from the expansion of hot tail gas in the turbine. Considering the
proximity to market, sea port and source of raw materials, it was
decided to site the plant in Eleme, Rivers State. The plant’s
3
estimated capital investment is ₦5.41 billion. The rate of return

on investment is 26.25% and the payback period is estimated to
be 3 years and 7 months. Thus, the project is both technically and
economically feasible.
TABLE OF CONTENT
Title page-----------------------------------------------------------------------i
Executive
Summary---------------------------------------------------------------------------ii
Table of
content-------------------------------------------------------------------------------iii
CHAPTER ONE
1.0 Introduction-----------------------------------------------------------1
1.3--------------------------------------------------------------------------------
Design
justification-------------------------------------------------------------------3
1.4--------------------------------------------------------------------------------
Design
Objectives---------------------------------------------------------------------4
CHAPTER TWO
2.0 Literature
review------------------------------------------------------------------------5
2.1 History of Nitric acid
production-------------------------------------------------------5
2.2 Ammonia oxidation
chemistry----------------------------------------------------------8
4
2.3 Emission and

Control-----------------------------------------------------------------------14
2.4 Structure and
bonding---------------------------------------------------------------------15
2.5
Reactions-------------------------------------------------------------------------------
------16
2.6
Uses--------------------------------------------------------------------------------------
-------19
2.7
Safety-----------------------------------------------------------------------------------
--------21
2.8 Pinch technology in modern
plant------------------------------------------------------22
2.9 Plant Location --------------------------------------------------------
24 2.9.5 Plant layout--------------------------------------------------
29
2.9.6 Process routes for the production of nitric acid------------------
33
CHAPTER THREE
3.0 Material balance ------------------------------------------------------42
3.1 Conservation of mass -----------------------------------------------42
3.2 Methods of material balancing -----------------------------------43
3.3 Materials balance assumptions-----------------------------------44
3.4 Summary of material balance calculations-------------------44
3.5 Material balance for each unit------------------------------------44

5
CHAPTER FOUR
4.0 Energy balance -------------------------------------------------------53
4.1 Conservation of energy---------------------------------------------54
4.2 Energy balance assumptions -------------------------------------56
4.3 Summary for energy balances------------------------------------56
CHAPTER FIVE
5.0 Chemical Engineering
design--------------------------------------------------------61
5.1 Process units of Nitric acid
Production--------------------------------------------61
CHAPTER SIX
6.0 Equipment design and specification ---------------------------66
6.1 Problem specification------------------------------------------------67
6.2 Analyzing the problem solution----------------------------------68
6.3 Preliminary
design-----------------------------------------------------------------------68
6.4 Material
Selection-----------------------------------------------------------------------69
6.5 Design
optimization---------------------------------------------------------------------69
6.6 Summary of design and equipment specification

calculation---------------70
CHAPTER SEVEN
7.0 Process control and instrumentation----------------------------73

6
7.1
Objective-------------------------------------------------------------------------------
----73
7.2 Plant control instrumentation-------------------------------------74
7.3 Alarms and safety trips --------------------------------------------77
7.4 Lining, piping, valves and pumps -------------------------------78
7.5 Pipe support------------------------------------------------------------81
CHAPTER EIGHT
8.0 Safety and environmental

considerations---------------------------------------82
8.1
Safety----------------------------------------------------------------------------------
--82
8.2 Hazard and Operability (HAZOP)

study-------------------------------------------89
8.3 Environmental impact

assessment-------------------------------------------------97
CHAPTER NINE
9.1 Overview----------------------------------------------------------------103
9.2 Economic Consideration--------------------------------------------103
9.3 Cost
estimation---------------------------------------------------------------------------
106
9.6 Economic analyses calculation-----------------------------------108

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CHAPTER TEN
10.0 Start up and shut down procedure----------------------------113
10.1 Emergency shut down and emergency depressurization

------------------------------------------------------------------------------------ 114
10.2 Notification------------------------------------------------------------114
10.3 Record keeping -----------------------------------------------------115
10.4 Startup operation---------------------------------------------------116
CHAPTER ELEVEN
11.0 Conclusion/
Recommendation----------------------------------------------------118
11.1
Conclusion-----------------------------------------------------------------------------
-118
11.2 Recommendation
-------------------------------------------------------------------119
REFERENCES----------------------------------------------------------------120
APPENDIX I
Tables and
Charts--------------------------------------------------------------------------------
123
APPENDIX II
8
Material Balance
Calculation------------------------------------------------------------------126
APPENDIX III
Energy Balance
Calculation------------------------------------------------------------------132
APPENDIX IV
Equipment Design
Calculation----------------------------------------------------------------137
APPENDIX V
Equipment Costing
Calculation---------------------------------------------------------------141
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CHAPTER ONE
INTRODUCTION
1.1 BACKGROUND INFORMATION
Nitric acid is a strong acid and a powerful oxidizing agent with

enormous possibilities for applications in the chemical processing
industry. It has commercial uses as a nitrating agent, oxidizing
agent, solvent, activating agent, catalyst and hydrolyzing agent.
In relation to world production, approximately 65% of all nitric
acid produced is used for the production of ammonium nitrate
(specifically for fertilizer manufacture).
10
Nitric acid is now produced commercially using the stepwise,

catalytic oxidation of ammonia with air, to obtain nitrogen
monoxide and nitrogen dioxide. These nitrogen oxides are
subsequently absorbed in water to yield between 50% and 68%
strength nitric acid by weight. For applications requiring higher
strengths, several methods of concentrating the acid are used.
The traditional methods are:
(a) Extractive distillation with dehydrating agents such as

sulphuric acid or magnesium nitrate;
(b) Reaction with additional nitrogen oxides.
The latter technique has the greatest application in industry.
The chemistry of ammonia oxidation is remarkably simple with

only six main reactions that need to be considered.
1.1.1 PROPERTIES AND USES
Nitric acid is an oxidizing mineral acid with physical and chemical

properties that make it one of the most useful inorganic minerals.
It is a colorless liquid at room temperature and atmospheric
pressure. It is soluble in water in all proportions and there is a
release of heat of solution upon dilution. Its high solubility in
water is the basis for the process methods used for commercial
nitric acid manufacture. It is a strong acid that almost completely
ionizes when in dilute solution. It is also a powerful oxidizing
agent with the ability to passivate some metals such as iron and
11
aluminum. A compilation of many of the physical and chemical

properties of nitric acid are presented in the Appendix. Arguably
the most important physical property of nitric acid is its
azeotropic point, this influences the techniques associated with
strong acid production. The constant-boiling mixture occurs at
121.9°C, for a concentration of 68.4%(wt) acid at atmospheric
pressure.
Nitric acid has enormously diverse applications in the chemical

industry. It has commercial uses as a nitrating agent, oxidizing
agent, solvent, activating agent, catalyst and hydrolyzing agent.
The most important use is undoubtedly in the production of
ammonium nitrate for the fertilizer and explosives industries,
which accounts for approximately 65% of the world production of
nitric acid.
Nitric acid has a number of other industrial applications. It is used

for pickling stainless steels, steel refining, and in the manufacture
of dyes, plastics and synthetic fibers. Most of the methods used
for the recovery of uranium, such as ion exchange and solvent
extraction, use nitric acid.
An important point is that for most uses concerned with chemical

production, the acid must be concentrated above its azeotropic
point to greater than 95%(wt). Conversely, the commercial
manufacture of ammonium nitrate uses nitric acid below its
azeotropic point in the range 50 -65 %(wt.). If the stronger
12
chemical grade is to be produced, additional process equipment

appropriate to super-azeotropic distillation is required.
There is a potential health hazard when handling, and operating

with, nitric acid. Nitric acid is a corrosive liquid that penetrates
and destroys the skin and internal tissues. Contact can cause
severe burns. The acid is a potential hazard, the various nitrogen
oxides present as product intermediates in the process are also
toxic. An assessment of the health risk must be fundamental to
the design of any process. Further consideration and
recommendations for the operating health risk and environmental
impact of the plant are presented in the Appendix.
1.2 DESIGN JUSTIFICATION
At present, there is no Nitric acid plant in Nigeria. The little Nitric

acid produced mainly by fertilizer plants in the country is used up
immediately by them to make their fertilizer. This means that
most of the all Nitric acid used in the country is imported.
A Nitric acid plant sited in the country producing Nitric acid made
available to the Nigerian market will not only reduce importation
of the acid but also encourage fertilizer production, create job
opportunities as well as develop the area in which it is sited.
1.3 DESIGN OBJECTIVES

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 To design a plant that will deliver 400000 metric tonnes of

60%(wt) Nitric Acid per annum.
 To determine the technical and economic feasibility of the
plant.
CHAPTER TWO
14
LITERATURE REVIEW
2.1 HISTORY OF NITRIC ACID PRODUCTION
Until the beginning of the 20th century, Nitric acid (HNO 3), also
known as aqua fortis and spirit of niter was prepared
commercially by reacting sulphuric acid with either potassium
nitrate (saltpetre) or with sodium nitrate (Chile saltpetre or nitre).
Up to four tonnes of the two ingredients were placed into large
retorts and heated over a furnace (Kirk 1996). The volatile
product vapourized and was collected for distillation. An acid of
93-95 %( wt) was produced (Gregory 1999).
In 1903 the electric-arc furnace superseded this primitive original

technique. In the arc process, nitric acid was produced directly
from nitrogen and oxygen by passing air through an electric-arc
furnace (Ray 1990).
Gregory (1999, p.40) argues that ‘Although the process benefitted

from an inexhaustible supply of free feed material (air), the power
consumption for the arc furnace was cost prohibitive’
According to Ray (1989, p.8) Researchers returned to the

oxidation of ammonia in air, (recorded as early as 1798) in an
effort to improve production economics. In 1901 Wilhelm Ostwald
had first achieved the catalytic oxidation of ammonia over a
platinum catalyst. The gaseous nitrogen oxides produced could be
easily cooled and dissolved in water to produce a solution of nitric
15
acid. This achievement began the search for an economic process

route.
By 1908 the first commercial facility for production of nitric acid,

using this new catalytic oxidation process, was commissioned
near Bochum in Germany (Ray et al 1989). The Haber-Bosch
ammonia synthesis process came into operation in 1913, leading
to the continued development and assured future of the ammonia
oxidation process for the production of nitric acid. (Ray et al 1989)
During World War 1, the intense demand for explosives and

synthetic dyestuffs created an expansion of the nitric acid
industry.
Many new plants were constructed, all of which employed the

ammonia oxidation process. This increased demand served as the
impetus for several breakthroughs in process technology.
These included:
(a) The development of chrome-steel alloys for tower

construction, replacing the heavy stoneware and acid-proof
bricks. This enabled process pressures above atmospheric levels
to be used.
(b) The improved design of feed preheaters enabled higher

process temperatures to be attained. Higher temperatures
improved the yields and capacities, and also reduced equipment
requirements (Ohrue et al 1999).
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(c) Early developments in automatic process control improved

process performance and reduced labor requirements.
All of these factors helped to improve the process efficiency. The

increasing availability of ammonia reduced processing costs still
further.
In the late 1920’s the development of stainless steels enabled

manufacturers to use higher operating pressures. The increase in
yield and lower capital requirements easily justified the use of
high pressure operation despite increased ammonia consumption.
The introduction of higher pressure processes resulted in a

divergence of operating technique within the industry. The United
States producers opted for a high-pressure system, using a
constant high pressure throughout the process. The European
manufacturers opted for a split-pressure system. This latter
system entails operating the ammonia oxidation section at
atmospheric pressure, while the absorption unit is operated at
higher pressures, thus capitalizing on improved absorption rates.
(Harvin et al 1979)
Recent developments in the ammonia oxidation process have

included efforts to reduce catalyst losses in the process. Platinum
recovery filters have been installed at various stages in the
process. (Ohrue et al 1999)
Gold/palladium gauze filter pads have been added on the exit side
of the catalyst bed, inside the reactor/converter units. These
17
filters have reportedly ensured a platinum recovery of 80% (Anon

1979). Another trend has been for the use of additional filters in
the downstream units. These filters are of alumino-silicate
construction.
Perhaps the greatest progress in nitric acid production technology

has been in the manufacture of strong nitric acid (>90% by
weight). Advances in the areas of super-azeotropic distillation and
in high pressure absorption are most significant. (Ohkubo et al
1999)
Research work is continually being performed in an effort to

reduce nitrogen oxide emissions from nitric acid plants. The
Humphreys and Glasgow/Bolme nitric acid process is just one
example of a new philosophy being applied to the absorption
systems of weak nitric acid plants (50-68% by weight). Nitrogen
oxide emissions have been reduced from 2000-5000 ppm to less
than 1000 ppm (Ray et al 1989).
For the production of stronger nitric acid, tail gases are now being
treated by selective or non-selective catalytic combustion
systems. These innovative units have reduced the nitrogen oxide
emissions to below 400 ppm (Ray et al 1989).
2.2 AMMONIA OXIDATION CHEMISTRY
Notably, all commercial nitric acid production methods used today

are centered on the oxidation of ammonia. It is therefore
appropriate to investigate the chemistry of this process, in the
18
knowledge that it is directly applicable to any of the production

processes available. (Chilton 1960)
The chemistry of the oxidation of ammonia is surprisingly simple.

It begins with a single pure compound, plus air and water, and
ends with another pure compound in aqueous solution, with
essentially no by-products. The process may be described by just
six major reactions as shown as follows:
N H 3(g) +2 O2 → HN O3 (aq )+ H 2 O(l )

1.
2. 4 N H 3(g )+ 5O2 (g) → 4 N O(g )+ 6 H 2 O(l )
2 N O(g) +O2 → 2 N O 2 (g)

3.
2 N O2 (g) ⇌ N 2 O4
4.
3 N 2 O 4 + 2 H 2 O(l) → 4 HN O 3 +2 N O (g)
5.
3 N O2 (g) + H 2 O(l) →2 HN O3 (aq )+ N O(g)

6.
Reaction 1 is the overall reaction for the process. This net result is
achieved from three separate, and distinct, chemical steps. The
first is the oxidation of ammonia to nitrogen monoxide (Reaction
2). The second is the further oxidation of nitrogen monoxide to
nitrogen dioxide (Reaction 3), then nitrogen dioxide to nitrogen
tetroxide (Reaction 4). The third and final stage involves the
absorption of these nitrogen-based oxides into water to form the
nitric acid product (Reactions 5 and 6). In most commercial
19
processes, each of these three stages is conducted in separate

process units. (Chilton 1960)
The first step in the process is the heterogeneous, highly

exothermic, gas-phase catalytic reaction of ammonia with oxygen
(Reaction 2). The primary oxidation of ammonia to nitric acid
(over a catalyst gauze of 9:l platinum/rhodium alloy) proceeds
rapidly at process temperatures between 900-970°C. (Kent 1983)
The second step in the process involves two reactions (Reactions

3 and 4). These are the oxidations of nitrogen monoxide to the
dioxide and tetroxide forms. The equilibrium mixture is loosely
referred to as nitrogen peroxide. Both reactions are homogenous,
moderately exothermic, gas-phase catalytic reactions. All
reactions shown are highly exothermic. (Chilton 1960)
The third step in the process involves cooling the reaction gases
below their dew point, so that a liquid phase of weak nitric acid is
formed. This step effectively promotes the state of oxidation and
dimerization (Reactions 3 and 4), and removes water from the gas
phase. This in turn increases the partial pressure of the nitrogen
peroxide component. (Chilton 1960)
Finally, nitric acid is formed by the reaction of dissolved nitrogen

peroxide with water (Reactions 5 and 6).
Nitric acid is produced by 2 methods. The first method utilizes

oxidation, condensation, and absorption to produce a weak nitric
acid. Weak nitric acid can have concentrations ranging from 30 to
20
70 percent nitric acid. The second method combines dehydrating,

bleaching, condensing, and absorption to produce a high-strength
nitric acid from a weak nitric acid. High-strength nitric acid
generally contains more than 90 percent nitric acid. The following
text provides more specific details for each of these processes.
(Chilton 1960)
2.2.1 WEAK NITRIC ACID PRODUCTION
According to Ray(1989, Nearly all the nitric acid produced in the
U. S. is manufactured by the high-temperature catalytic oxidation
of ammonia. This process typically consists of 3 steps: (1)
ammonia oxidation, (2) nitric oxide oxidation, and (3) absorption.
Each step corresponds to a distinct chemical reaction.
1. AMMONIA OXIDATION
First, a 1:9 ammonia/air mixture is oxidized at a temperature of
1380 to 14700F as it passes through a catalytic convertor,
according to the following reaction:
4 N H 3 +5 O2 → 4 NO +6 H 2 O
The most commonly used catalyst is made of 90 percent platinum

and 10 percent rhodium gauze constructed from squares of fine
wire. Under these conditions, the oxidation of ammonia to nitric
oxide (NO) proceeds in an exothermic reaction with a range of 93
to 98 percent yield. Oxidation temperatures can vary from 1380 OF
to 16500F. (Chilton 1960) Higher catalyst temperatures increase
reaction selectivity toward NO production. Lower catalyst
temperatures tend to be more selective toward less useful
products: nitrogen (N2) and nitrous oxide (N2O).
21
Nitric oxide is considered to be a criteria pollutant and nitrous

oxide is known to be a global warming gas. The nitrogen
dioxide/dimmer mixture then passes through a waste heat boiler
and a platinum filter. (Chilton 1960)
2. NITRIC OXIDE OXIDATION
The nitric oxide formed during the ammonia oxidation must be
oxidized. The process stream is passed through a
cooler/condenser and cooled to 100 0F or less at pressures up to
116 pounds per square inch absolute (psia). The nitric oxide
reacts non-catalytically with residual oxygen to form nitrogen
dioxide (NO2) and its liquid dimmer, nitrogen tetra-oxide:
2 N O2 +O2 → 2 N O2 ⇌ N 2 O4
This slow, homogeneous reaction is highly temperature and

pressure dependent. Operating at low temperatures and high
pressures promotes maximum production of NO 2 within a
minimum reaction time (Kent 1983).
3. ABSORPTION
The final step introduces the nitrogen dioxide/dimmer mixture
into an absorption process after being cooled. The mixture is
pumped into the bottom of the absorption tower, while liquid
dinitrogen tetra-oxide is added at a higher point. De-ionized
process water enters the top of the column. Both liquids flow
countercurrent to the nitrogen dioxide/dimmer gas mixture.
Oxidation takes place in the free space between the trays, while
absorption occurs on the trays. The absorption trays are usually
22
sieve or bubble cap trays. The exothermic reaction occurs as

follows:
3 N O2 + H 2 O→ 2 HN O3+ NO
A secondary air stream is introduced into the column to re-oxidize

the NO that is formed in Reaction 3. This secondary air also
removes NO2 from the product acid. An aqueous solution of 55 to
65 percent (typically) nitric acid is withdrawn from the bottom of
the tower. The acid concentration can vary from 30 to 70 percent
nitric acid. The acid concentration depends upon the temperature,
pressure, number of absorption stages, and concentration of
nitrogen oxides entering the absorber.
There are 2 basic types of systems used to produce weak nitric

acid: single-stage pressure process and dual-stage pressure
process (Harvin et al 1979). In the past, nitric acid plants have
been operated at a single pressure, ranging from atmospheric
pressure to 14.7 to 203 psia. However, since Reaction 1 is favored
by low pressures and Reactions 2 and 3 are favored by higher
pressures, newer plants tend to operate a dual stage pressure
system, incorporating a compressor between the ammonia
oxidizer and the condenser. The oxidation reaction is carried out
at pressures from slightly negative to about 58 psia, and the
absorption reactions are carried out at 116 to 203 psia. (Harvn et
al 1979)
In the dual-stage pressure system, the nitric acid formed in the
absorber (bottoms) is usually sent to an external bleacher where
air is used to remove (bleach) any dissolved oxides of nitrogen.
23
The bleacher gases are then compressed and passed through the
absorber. The absorber tail gas (distillate) is sent to an
entrainment separator for acid mist removal. Next, the tail gas is
reheated in the ammonia oxidation heat exchanger to
approximately 3920F. The final step expands the gas in the power-
recovery turbine. The thermal energy produced in this turbine can
be used to drive the compressor.
2.2.2 HIGH STRENGTH NITRIC ACID PRODUCTION
A high-strength nitric acid (98 to 99 percent concentration) can be
obtained by concentrating the weak nitric acid (30 to 70 percent
concentration) using extractive distillation. (Imai et al 1999) The
weak nitric acid cannot be concentrated by simple fractional
distillation. The distillation must be carried out in the presence of
a dehydrating agent. Concentrated sulfuric acid (typically 60
percent sulfuric acid) is most commonly used for this purpose.
The nitric acid concentration process consists of feeding strong
sulfuric acid and 55 to 65 percent nitric acid to the top of a
packed dehydrating column at approximately atmospheric
pressure. The acid mixture flow downward, countercurrent to
ascending vapors. Concentrated nitric acid leaves the top of the
column as 99 percent vapor, containing a small amount of NO 2
and oxygen (O2) resulting from dissociation of nitric acid. The
concentrated acid vapor leaves the column and goes to a
bleacher and a countercurrent condenser system to effect the
condensation of strong nitric acid and the separation of oxygen
and oxides of nitrogen (NO2) byproducts. (Ohkubo et al 1999)
24
These byproducts then flow to an absorption column where the

nitric oxide mixes with auxiliary air to form NO 2, which is
recovered as weak nitric acid. Inert and un-reacted gases are
vented to the atmosphere from the top of the absorption column.
Emissions from this process are relatively minor. A small absorber
can be used to recover NO2. (Kirk et al 1981)
2.3 EMISSIONS AND CONTROL

Emissions from nitric acid manufacture consist primarily of NO,
NO2 (which account for visible emissions), trace amounts of HNO 3
mist, and ammonia (NH3). By far, the major source of nitrogen
oxides (NO2) is the tail-gas from the acid absorption tower. In
general, the quantity of NO2 emissions is directly related to the
kinetics of the nitric acid formation reaction and absorption tower
design. NO2 emissions can increase when there is (1) insufficient
air supply to the oxidizer and absorber, (2) low pressure,
especially in the absorber, (3) high temperatures in the cooler-
condenser and absorber, (4) production of an excessively high-
strength product acid, (5) operation at high throughput rates, and
(6) faulty equipment such as compressors or pumps that lead to
lower pressures and leaks, and decrease plant efficiency. (Leray et
al 1979)
Roudier (1979) states that the two most common techniques used
to control absorption tower tail gas emissions are extended
absorption and catalytic reduction. Extended absorption reduces
25
NO2 emissions by increasing the efficiency of the existing process

absorption tower or incorporating an additional absorption tower.
An efficiency increase is achieved by increasing the number of
absorber trays, operating the absorber at higher pressures, or
cooling the weak acid liquid in the absorber. The existing tower
can also be replaced with a single tower of a larger diameter
and/or additional trays.
In the catalytic reduction process (often termed catalytic
oxidation or incineration), tail gases from the absorption tower are
heated to ignition temperature, mixed with fuel (natural gas,
hydrogen, propane, butane, naphtha, carbon monoxide, or
ammonia) and passed over a catalyst bed. In the presence of the
catalyst, the fuels are oxidized and the NO2 are reduced to N2. The
extent of reduction of NO2 and NO to N2 is a function of plant
design, fuel type, operating temperature and pressure. Space-
velocity through the comparatively small amounts of nitrogen
oxides is also lost from acid concentrating plants. These losses
(mostly NO2) are from the condenser system, but the emissions
are small enough to be controlled easily by inexpensive
absorbers. Acid mist emissions do not occur from the tail-gas of a
properly operated plant. The small amounts that may be present
in the absorber exit gas streams are removed by a separator or
collector prior to entering the catalytic reduction unit or expander.
(Kent 1983)
26
The acid production system and storage tanks are the only
significant sources of visible emissions at most nitric acid plants.
Emissions from acid storage tanks may occur during tank filling.
2.4 STRUCTURE AND BONDING
Fig 2: Two major resonance representations of HNO 3.
The molecule is planar. Two of the N-O bonds are equivalent and
relatively short (this can be explained by theories of resonance.
The canonical forms show double bond character in these two
bonds, causing them to be shorter than typical N-O bonds.), and
the third N-O bond is elongated because the O is also attached to
a proton.
2.5 REACTIONS
2.5.1 ACID-BASE PROPERTIES
Nitric acid is normally considered to be a strong acid at ambient

temperatures. The pKa value is usually reported as less than −1.
This means that the nitric acid in solution is fully dissociated
27
except in extremely acidic solutions. The pK a value rises to 1 at a

temperature of 250 °C.
Nitric acid can act as a base with respect to an acid such as

sulfuric acid.
HNO3 + 2H2SO4 NO2+ + H3O+ + 2HSO4–
The nitronium ion, NO2+, is the active reagent in aromatic nitration

reactions. Since nitric acid has both acidic and basic properties it
can undergo an autoprotolysis reaction, similar to the self-
ionization of water
2HNO3 NO2+ + NO3– + H2O
2.5.2 REACTIONS WITH METALS
Nitric acid reacts with most metals but the details depend on the
concentration of the acid and the nature of the metal. Dilute nitric
acid behaves as a typical acid in its reaction with most metals.
Magnesium, manganese and zinc liberate H2. Others give the
nitrogen oxides. (Ababio 2007)
Nitric acid can oxidize non-active metals such as copper and

silver. With these non-active or less electropositive metals the
products depend on temperature and the acid concentration. For
example, copper reacts with dilute nitric acid at ambient
temperatures with a 3:8 stoichiometry to produce nitric oxide
28
which may react with atmospheric oxygen to give nitrogen

dioxide.
3 Cu + 8 HNO3 → 3 Cu2+ + 2 NO + 4 H2O + 6 NO3-
With more concentrated nitric acid, nitrogen dioxide is produced

directly in a reaction with 1:4 stoichiometries.
Cu + 4 H+ + 2 NO3− → Cu2+ + 2 NO2 + 2 H2O
Upon reaction with nitric acid, most metals give the corresponding
nitrates. Some metalloids and metals give the oxides, for
instance, Sn, As, Sb, Ti are oxidized into SnO2, As2O5, Sb2O5 and
TiO2 respectively.
Some precious metals, such as pure gold and platinum group

metals do not react with nitric acid, though pure gold does react
with aqua regia, a mixture of concentrated nitric acid and
hydrochloric acid. However, some less noble metals (Ag, Cu, ...)
present in some gold alloys relatively poor in gold such as colored
gold can be easily oxidized and dissolved by nitric acid, leading to
color changes of the gold-alloy surface. Nitric acid is used as a
cheap means in jewelry shops to quickly spot low-gold alloys
(< 14 carats) and to rapidly assess the gold purity.
Being a powerful oxidizing agent, nitric acid reacts violently with

many non-metallic compounds and the reactions may be
explosive. Reaction takes place with all metals except the noble
metals series and certain alloys. As a general rule, oxidizing
29
reactions occur primarily with the concentrated acid, favoring the

formation of nitrogen dioxide (NO2). (Ababio 2007) However, the
powerful oxidizing properties of nitric acid are thermodynamic in
nature, but sometimes its oxidation reactions are rather
kinetically non-favored. The presence of small amounts of nitrous
acid (HNO2) greatly enhances the rate of reaction.
Although chromium (Cr), iron (Fe) and aluminum (Al) readily

dissolve in dilute nitric acid, the concentrated acid forms a metal
oxide layer that protects the bulk of the metal from further
oxidation. The formation of this protective layer is called
passivation. Typical passivation concentrations range from 20–
50% by volume (ASTM A967-05 2000). Metals which are
passivated by concentrated nitric acid are Iron, Cobalt, Chromium,
Nickel, and Aluminum.
2.5.3 REACTIONS WITH NON-METALS
Being a powerful oxidizing acid, nitric acid reacts violently with

many organic materials and the reactions may be explosive. (Kent
1983)
Reaction with non-metallic elements, with the exceptions of

nitrogen, oxygen, noble gases, silicon and halogens, usually
oxidizes them to their highest oxidation states as acids with the
30
formation of nitrogen dioxide for concentrated acid and nitric

oxide for dilute acid. (Ababio 2007)
C + 4 HNO3 → CO2 + 4 NO2 + 2 H2O

OR
3 C + 4 HNO3 → 3 CO2 + 4 NO + 2 H2O
Concentrated nitric acid oxidizes I2, P4 and S8 into HIO3, H3PO4 and
H2SO4 respectively.
2.5.4 XANTHOPROTEIC TEST
Nitric acid reacts with proteins to form yellow nitrated products.

This reaction is known as the xanthoproteic reaction (Gregory
1999). This test is carried out by adding concentrated nitric acid
to the substance being tested, and then heating the mixture. If
proteins that contain amino acids with aromatic rings are present,
the mixture turns yellow. Upon adding a strong base such as
liquid ammonia, the color turns orange. These color changes are
caused by nitrated aromatic rings in the protein. Xanthoproteic
acid is formed when the acid contacts epithelial cells and is
indicative of inadequate safety precautions when handling nitric
acid
2.6 USES
2.6.1 NITRIC ACID IN A LABORATORY.

The main use of nitric acid is for the production of fertilizers. Nitric
acid is neutralized with ammonia to give ammonium nitrate.
31
According to Gregory (1999, p.408) this application consumes 75-

80% of the 26M tons produced annually. The other main
applications are for the production of explosives, nylon
precursors, and specialty organic compounds.
2.6.2 PRECURSOR TO ORGANIC NITROGEN COMPOUNDS
In organic synthesis, industrial and otherwise, the nitro group is a

versatile functionality. Most derivatives of aniline are prepared via
nitration of aromatic compounds followed by reduction. Nitrations
entail combining nitric and sulfuric acids to generate the
nitronium ion, which electrophilically reacts with aromatic
compounds such as benzene. (Gregory 1999) Many explosives,
e.g. TNT, are prepared in this way.
The precursor to nylon, adipic acid, is produced on a large scale

by oxidation of cyclohexanone and cyclohexanol with nitric acid.
1.6.3 ROCKET FUEL
Nitric acid has been used in various forms as the oxidizer in liquid-
fueled rockets. These forms include red fuming nitric acid, white
fuming nitric acid, mixtures with sulfuric acid, and these forms
with HF inhibitor. IRFNA (inhibited red fuming nitric acid) was one
of 3 liquid fuel components for the BOMARC missile. (Gregory
1999)
2.6.4 ANALYTICAL REAGENT

32
In elemental analysis dilute nitric acid (0.5 to 5.0%) is used as a

matrix compound for determining metal traces in solutions.
Ultrapure trace metal grade acid is required for such
determination, because small amounts of metal ions could affect
the result of the analysis. (Kirk 1981)
It is also typically used in the digestion process of turbid water

samples, sludge samples, solid samples as well as other types of
unique samples which require elemental analysis via flame atomic
absorption spectroscopy. Typically these digestions use a 50%
solution of the purchased HNO3 mixed with deionized water.
In electrochemistry, nitric acid is used as a chemical doping agent

for organic semiconductors, and in purification processes for raw
carbon nanotubes.
2.6.5 WOODWORKING
In a low concentration (approximately 10%), nitric acid is often

used to artificially age pine and maple. The color produced is a
grey-gold very much like very old wax or oil finished wood (wood
finishing).
2.6.6 ETCHANT AND CLEANING AGENT
The corrosive effects of nitric acid are exploited for a number of

specialty applications, such as pickling stainless steel. A solution
of nitric acid, water and alcohol, Nital, is used for etching of
metals to reveal the microstructure (Gregory 1999). Commercially
33
available aqueous blends of 5–30% nitric acid and 15–40%

phosphoric acid are commonly used for cleaning food and dairy
equipment primarily to remove precipitated calcium and
magnesium compounds (either deposited from the process
stream or resulting from the use of hard water during production
and cleaning). The phosphoric acid content helps to passivate
ferrous alloys against corrosion by the dilute nitric acid.(Anon
1979) Nitric acid can be used as a spot test for alkaloids, giving a
variety of colors depending on the alkaloid.
2.7 SAFETY
Nitric acid is a strong acid and a powerful oxidizing agent. The

major hazard posed by it is chemical burns as it carries out acid
hydrolysis with proteins (amide) and fats (ester) which
consequently decomposes living tissue (e.g. skin and flesh).
Concentrated nitric acid stains human skin yellow due to its
reaction with the keratin. These yellow stains turn orange when
neutralized. Systemic effects are unlikely, however, and the
substance is not considered a carcinogen or mutagen.
The standard first aid treatment for acid spills on the skin is, as for
other corrosive agents, irrigation with large quantities of water.
Washing is continued for at least ten to fifteen minutes to cool the
tissue surrounding the acid burn and to prevent secondary
damage. Contaminated clothing is removed immediately and the
underlying skin washed thoroughly. (Othmer et al 1981)
34
Being a strong oxidizing agent, reactions of nitric acid with

compounds such as cyanides, carbides, metallic powders can be
explosive and those with many organic compounds, such as
turpentine, are violent and hypergolic (i.e. self-igniting). Hence, it
should be stored away from bases and organics.
2.8 PINCH TECHNOLOGY IN MODERN PLANTS

One of the most successful and generally useful techniques is that
developed by Bodo Linnhoff and other workers: pinch technology.
The term derives from the fact that in a plot of the system
temperatures versus the heat transferred, a pinch usually occurs
between the hot stream and cold stream curves. (Sinnot 2005)
Pinch technology is a relatively modern engineering tool
developed in the late 1970s and early 1980s. This new approach
to evaluating the energy requirements of a site quickly identified
ways of improving the overall energy use. The name “pinch
technology” was applied because the technique identified the
point or points in the energy flow where restrictions applied and
hence limited one’s ability to reuse low grade energy.
The major difference between this new technology and the
previous engineering approaches was the formalized
methodology involving the rigorous application of thermodynamic
principles. Pinch technology was initially adopted by major
chemical companies and petrochemical energy. Beet sugar was
quite quick to adopt it because of the industry’s energy profile
and it is now being adopted by the cane industry too. It has also
been shown that the pinch represents a distinct thermodynamic
35
break in the system and that, for minimum energy requirements,

heat should not be transferred across the pinch, (Linnhoff et al
1983)
2.8.1 APPLICATIONS
Pinch technology is equally applicable to Greenfield project and

refurbishments. In either case, their objectives are to achieve:
1. Minimum energy consumption

2. Optimization of utilities
3. Minimum capital expenditure to achieve these
Minimizing energy consumption implies minimizing cooling water
requirements too because all of the energy used ultimately has to
be rejected again in some low grade form. ( Sinnot 2005)
The technology strength are its overall approach to process

integration (rather than optimizing a single station) and its blend
of thermodynamics with commercial requirements. It also takes
into account the operational requirements of the site and does
reduce flexibility or availability.
2.9 PLANT LOCATION
Plant location refers to the choice of a region or the selection of a

particular site for settling up the business or a factory. However,
the choice is made only after considering alternative sites. It is a
strategic decision that cannot be changed once it is taken.
36
Therefore, careful care must be taken before a decision is made

on the location of the plant site (Ray et al 1989).
2.9.1 IDEAL PLANT LOCATION
An ideal plant location is one where the cost of the production is

minimal, with a large market availability, least risk involved and
maximum gain obtainable. It is a place of maximum net
advantage or with lowest unit cost of production and distribution.
For achieving this objective, small and large scale entrepreneur
can make use of local analysis.
2.9.2 LOCAL ANALYSIS
Local analysis is a dynamic process where the entrepreneur

analyses and compares the feasibility of different sites with the
aim of selecting the best site for a given enterprise. It considers
the following:
a. Demographic analysis: it involves the study of the

population in the area in terms of total number of people in
the area, age composition, per capital income, educational
level and occupational structures etc.
b. Trade area analysis: it is an analysis of the geographic
area that provides continued clientele to the industry. It is
advisable to also see the feasibility of accessing the trade
area from alternative sites. (Ray et al 1989)
c. Competitive analysis: it helps to judge the nature,
location, size and quality of competition in a given trade
area.
37
d. Traffic analysis: this is done to have a rough idea about the

number of potential customers passing by the proposed site
during the working hours of the industry. The traffic analysis
aims at judging the alternative sites in terms of pedestrian
and vehicular traffic passing by the site.
e. Site economics: alternative sites are evaluated in terms of
establishments, costs and operational costs under this. Cost
of establishment of a plant is basically cost incurred for
permanent physical facilities but operation costs are incurred
for running the plant.
2.9.3 SELECTION CRITERIA
According to Ray (1989, p. 76) the important considerations for

selecting a suitable location are as follows:
I. Nature or climate conditions

II. Availability and nearness to the sources of raw materials
III. Transport costs: this should be considered both for
obtaining raw material and also distribution or marketing
finished products to the ultimate users.
IV. Close proximity to the anticipated market: the industry’s
warehouse should be located within the vicinity of densely
populated areas.
V. Availability of infrastructural facilities such as developed
industrial shed or site, link roads, nearness to railway
stations, airports or seaports, availability of electricity,
38
water, public utilities, civil amenities and means of

communication are important.
VI. Availability of skilled and non-skilled labor and technically
qualified and trained managers.
VII. Banking and financial institutions should be located
nearby.
VIII. Safety and security should be given due consideration
IX. Government influences: tax relief, subsidies, liberation
and other positive policies of the government to support
the start off of any industry should be duly considered
before any industry is set up. Also, negative government
influences like restrictions for setting up industries in an
area for reason of pollution control and decentralization of
industries should be considered.
X. Utility costs and availability.
2.9.4 SELECTION OF PLANT LOCATION FOR THE NITRIC

ACID PLANT
There were three plant locations proposed. Each was evaluated

and the final decision based on maximum net advantage was
made.
2.9.4.1 LOCATION ONE: AGBARA INDUSTRIAL ESTATE

(OGUN STATE)
Advantages
1. Relatively cheap available land and labor cost.

2. Relatively close to market (Lagos Nylon and plastic market).
3. Relatively close to sea (Lagos Apapa) for import of raw
material and export of product if need be.
39
4. Availability of infrastructural facilities such as link roads,

public utilities etc.
5. Availability of financial institution.
6. Relatively secure.
7. Availability of social amenities and means of communication.
8. Disadvantages
1. No local source of raw material nearby meaning all raw
materials have to be transported to the plant location.
2. The major roads that will be used for transportation (i.e form
Apapa to Agbara) are bad and one is prone to experience
hold up on it.
3. Transport cost will be very high for both bringing in of raw
material and marketing finished product as the target market
is Lagos and things are known to be very expensive there.
4. The Nylon and plastic market in Lagos is not large enough to
exhaust all nitric acid produced by the plant.
5. Additional cost of providing water and electricity for the
plant.
2.9.4.2 LOCATION TWO: ABA (ABIA STATE)
Advantages
1. Relatively cheap available land and labor cost.

2. Availability of market (plastic and Nylon market)
3. Availability of financial institution.
Disadvantages
40
1. Not close to source of raw material

2. Additional cost of providing water and electricity for the
plant.
3. Market available not enough to exhaust all nitric acid
produced in the plant.
4. Lack of infrastructural facilities such as sea port, airport and
railway stations nearby.
2.9.4.3 LOCATION THREE: ELEME, PORT-HARCOURT

(RIVERS STATE)
Advantages
1. Close to source of raw material: National Fertilizer Company

of Nigeria (NAFCON), an ammonia and fertilizer plant at
Onne, Port-Harcourt, Rivers State bought over by Notore
started operation in Jan 2009. Their production of ammonia
per day of ammonia was 1,000MT as at 2009 of anhydrous
ammonia (more than enough raw material for our nitric acid
plant). Eleme Petrochemical located in Eleme, Port-harcourt,
Rivers State is also billed to come up with an ammonia plant
in 2014 which will make available to the Nigeria market
2300MT.
2. Availability of market in Port-Harcourt, closeness to sea for
export of product if necessary.
3. Availability of public utilities such as water, sea port, airport,
etc.
4. Availability of both skilled and unskilled labor.
5. Availability of banking and financial institutions.
41
Disadvantages
2. High cost of land

3. No regular power supply
2.9.5 PLANT LAYOUT
Having selected a suitable site for the chemical plant, it is

possible and necessary to make a preliminary decision regarding
the layout of the plant equipment. (Ray et al 1989) Although the
equipment has not been designed in detail, preliminary estimates
of the physical size of each item should be available in the
equipment list. Any sizing differences between the initial and final
estimates should not be too excessive, and appropriate areas
should be allowed around the plant items when determining the
layout.
A preliminary determination of the plant layout enables

consideration of pipe runs and pressure drops, access for
maintenance and repair and in the event of accidents and spills,
and location of the control room and administrative offices. The
preliminary plant layout can also help to identify undesirable and
unforeseen problems with the preferred site, and may necessitate
a revision of the site selection. (Baasel 1989) The proposed plant
layout must be considered early in the design work, and in
sufficient detail, to ensure economical construction and efficient
operation of the completed plant. The plant layout adopted also
affects the safe operation of the plant, and acceptance of the
42
plant (and possibly any subsequent modifications or extensions)

by the community.
There are two schemes that can be adopted for determination of

the plant layout. (Buckhurst & Harker 1973) First, the ‘flow-
through’ layout (or ‘flow-line’ pattern) where plant items are
arranged (sequentially) in the order in which they appear on the
process flow sheet. This type of arrangement usually minimizes
pipe runs and pressure drops (and is often adopted for small
plants). Second, the equipment is located on site in groupings of
similar plant items, e.g. distillation columns, separation stages,
reactors and heat exchanger pre-heaters, etc. The grouped
pattern is often used for larger plants and has the advantages of
easier operation and maintenance, lower labor costs, minimizing
transfer lines and hence reducing the energy required to transfer
materials. These two schemes represent the extreme situations
and in practice some compromise arrangement is usually
employed. The plant layout adopted depends upon whether a new
(‘grass roots’) plant is being designed or an
extension/modification to an existing plant. Space restrictions are
the most common constraints; however, space limitations are
usually imposed even with new sites. Other factors to be
considered are:
(a) Siting of the control room, offices, etc., away from areas of
high accident risk, and upstream of the prevailing winds.
43
(b) Location of reactors, boilers, etc., away from chemical storage

tanks.
(c) Storage tanks to be located for easy access, and a decision

made as to whether all tanks (for raw materials and product)
should be located together or dispersed around the site.
(d) Labor required for plant operation.
(e) Elevation of equipment.
(f) Requirements of specific plant items, e.g. pumps.
(g) Supply of utilities, e.g. electricity, water, steam, etc.
(h) Minimizing plant piping systems.
(i) Suitable access to equipment requiring regular maintenance or

repair.
(j) Plant layout to facilitate easy clean-up operations and

dispersion of chemicals in the event of a spillage.
(k) Access to the plant in the event of an accident.
(1) Siting of equipment requiring cooling water close to rivers,

estuaries, etc.
(m) Location of plant waste and water drainage systems (separate

or combined?) and treatment tanks.
(n) Adopting a plant layout that will act to contain any fires or
explosions.
44
(o) Spacing between items of equipment (insurance companies

specializing in the insurance of chemical plants have specific
recommendations for the distances required between particular
items of equipment).
The layout of plant equipment should aim to minimize:
(i) damage to persons and property due to fire or explosion;
(ii) Maintenance costs;
(iii) Number of plant personnel;
(iv) Operating costs; construction costs;
(v) Cost of plant expansion or modifications.
Some of these aims are conflicting, e.g. (i) and (iv), and
compromises are usually required when considering the plant
layout to ensure that safety and economic operation are both
preserved. The final plant layout will depend upon the measures
for energy conservation within the plant and any subsequent
modifications, and the associated piping arrangements.
The process units and ancillary buildings are laid out in such a
way to give the most economical flow of materials and personnel
around the site. Hazardous processes are located a safe distance
from other buildings. Consideration for future expansion is also
put in place. The ancillary buildings and service required on the
site include:
 Administrative block
45
 Laboratory
 Storage for both raw materials and products
 Maintenance workshop
 Utilities (generator, steam boiler, transformer station)
 Store for maintenance and operation supplies
 Other amenities like car park, restaurant and clinic.
Emergency
Fire Station Water
Tank Farm Plant Area
Stores
Workshop
Roads
Canteen
Medical
Center
Waste Car Pack
Utilities
Incinerator
Auditorium
Offices
Roads
Fig 1.1 Expected plant layout.
2.9.6 PROCESS ROUTES FOR THE PRODUCTION

OF NITRIC ACID
CHILE SALTPETRE/NITRATE PROCESS

46
Chile saltpetre is material which contains sodium nitrate NaNO 3

with percentage around 35-60%, and remaining percentage
compounds with KNO3 and NaCl. This raw material Chile saltpetre
is concentrated by crystallization in pre-treatment of ore to attain
95% NaNO3 and remaining KNO3 as feed raw material. (Kent 1983)
Sulphuric acid with 93% is mixed with the refined Chile saltpetre
as per the ratio required as per stoichiometry and sent into a
retort which is made with cast iron and the mixture is heated to
200oC with help of furnace flue gasses and coal fire. Thus at this
temperature, the following reaction is carried forward to produce
HNO3, nitric acid vapors.
NaNO 3 + H2SO4 → NaHSO4 + HNO3
All hot vapors of nitric acid are sent to cool down in water
circulated cooled silica pipes, condensed HNO3 are collected in
receiver which has material resistance to nitric acid. Uncondensed
gas which escapes from the collector is scrubbed with cooled
water in packed bed tower to collect nitric acid in dilute format.
Liquid sodium bi-sulphate is collected from the bottom outlet of
the retort.
Advantage: it was one of the first methods used in the

manufacture of nitric acid.
Disadvantage: source of raw material can be exhausted.

47
Fig 1.2: Manufacture of nitric acid from Chile Saltpetre.
BIRKELAND-EYDE PROCESS/ARC PROCESS
This process is based upon the oxidation of atmospheric nitrogen

by atmospheric oxygen to nitric oxide at very high temperature.
An electric arc is used to provide the high temperatures, and
yields of up to 4% nitric oxide were obtained. ( Ohrue 1999)
N2 + O2 →2NO
The nitric oxide was cooled and oxidized by the remaining

atmospheric oxygen to nitrogen dioxide
2 NO + O 2 →2NO2
This nitrogen dioxide is then dissolved in water to give dilute nitric

acid.
48
3 NO2 + H2O → 2HNO3 + NO
Advantage: unlimited source of raw material (air)
Disadvantage: The process is very energy intensive and is only

feasible when electricity is available and cheap.
WINSCONSIN PROCESS/NITROGEN FIXATION PROCESS
Atmospheric oxygen and nitrogen are combined in a high

temperature regenerative furnace operating at about 2000 oC.
Nitric oxide is formed with a yield of nearly 2%.
Advantage: it does not use electricity to provide the high

temperature and therefore does not have the disadvantage of the
Birkeland-Eyed process.
Disadvantage: cannot compete favorably with the Ostwald

process.
Another method of production of nitric acid via nitrogen fixation is

the nuclear nitrogen fixation route. This method directly combines
oxygen and nitrogen. Yields of nitrogen oxide of 5-15% have been
reported by exposing air at 150 and 400 oF to radiation from
Uranium 235.
Advantage: gives a greater yield of nitrogen oxide than the

Winsconsin process
Disadvantage: with this method comes all the disadvantages of

nuclear reaction (problem of managing the radiation which is
harmful to living things)
49
OSTWALD PROCESS
In this process, anhydrous ammonia is oxidized to nitric oxide, in

the presence of platinum or rhodium gauge catalyst at high
temperature of about 500K and a pressure of 9bar. (Ray et al
1989)
4 NH3 (g) + 5 O2 (g) → 4 NO (g) + 6 H2O (g) (∆H= -905.2KJ)
Nitric acid is then reacted with oxygen in air to form nitrogen

dioxide.
2 NO (g) + O2 (g) → 2NO2 (g) (∆H= -114KJ/mol)
This is subsequently absorbed in water to form nitric acid and

nitric oxide
3 NO2 (g) + H2O (l) → 2 HNO3 (aq) + NO (g) (∆H= -117KJ/mol)
The nitric oxide is cycled back for re-oxidation. Alternately, if the

last step is carried out in air:
4 NO2 (g) + O2 (g) + 2H2O (l) → 4HNO3 (aq)
The aqueous HNO3 obtained can be concentrated by distillation

up to about 68% by mass.
There are 2 basic types of systems used to produce weak nitric

acid:
Both processes follow the basic Ostwald process for the catalytic
oxidation of ammonia. In summary, this involves an oxidation
stage whereby ammonia is reacted with air in a catalytic
50
converter at temperatures in the range of 850-950°C. Reaction

gases pass through a series of energy recovery stages before
entering an absorption column. The bottoms from the column are
bleached of dissolved nitrogen peroxide using air, and the
resulting solution is the weak nitric acid product (Roudier et al
1979).
The major difference between the two processes lies in the initial
conversion stage. The dual-pressure process employs a
conversion stage operating in the range l00-350kPa, and a reactor
temperature of about 865°C. The single-pressure process however
operates the converter at 800-1100 kPa, with a reactor
temperature closer to 940°C. ( Harvin et al 1979)
1. Single-stage pressure process: in this case, the plant is

operated at a single pressure throughout.
51
Fig 1.3. Process flow diagram for single-stage pressure process.

Advantage:
 Less expensive as less equipment’s are used.
 The single-pressure process uses a higher ammonia
conversion pressure. This higher pressure provides
advantages in terms of equipment design, e.g. smaller
converter dimensions and a single heat-exchanger-train
layout.( Leray et al 1979)
 The higher temperature and the favorable pressure both
increase the energy recovery from the process.
 Limited space availability may favor the single-pressure
process
Disadvantage:
52
 Less efficient as the overall process is favored by varying

pressure.
 Experimental work indicates that the rate loss of catalyst
(without a catalyst recovery system) is approximately three
times more rapid at 973°C than at 866°C. This means that
more catalyst is lost in the single-stage pressure process
( Harvin et al 1979).
 Absorber efficiency is reduced prompting the need for larger
absorber thereby increasing cost.
2. Dual-stage pressure process: here, the plant is operated
at different pressures and different stages.
Advantages:
 The first reaction (catalytic conversion of anhydrous
ammonia to nitric oxide) is favored by lower pressure while
the remaining reactions are favored by higher pressures.
This variation in pressure is achieved in dual-stage pressure
process. (Harvin et al 1979)
 Capacities of 1130-1360 tonnes per day favor the dual-
pressure process, because of the possibility of absorption up
to 1550 KPa.
 Less catalyst is lost because of lower operating temperature
53
Fig 1.4. Process flow diagram for dual-stage pressure process.
The process selected for this design of nitric acid is single-stage

pressure Ostwald process because of its above mentioned
advantages.
54
Fig1.5: Selected Process flow diagram for Nitric acid plant.
CHAPTER THREE
55
MATERIAL BALANCE
Material balance is one of the most important components of a

process design. Overall raw material of the entire process
determines the qualities of raw materials required and the
products produced in the process.
Balance over individual process units determines the process

stream flows and their compositions and also the sizes of the
various process equipment used in the process.
Material balance on the plant used in the production of 400000

tonnes of Nitric acid per year.
kg kg
Mass flow rate = 400000 x 1000 year = 50000 hr
3.1 CONSERVATION OF MASS
For a steady state process, the accumulation term will be zero;

but if a chemical reaction takes place, particular chemical specie
may be formed or consumed in the process. When there is
chemical reaction, the material balance equation is given as,
Input + Generation = Output + Consumption
If there is no chemical reaction, the steady state balance reduces

to;
Input = Output
56
A balance equation can be written for any identifiable specie

present, elements or compound; and for the total material.
3.2 METHODS OF MATERIAL BALANCE
There are two basic methods of material balance and they are;
(a) Algebraic Method
The algebraic method of material balancing is one of the simplest

and most common methods applied in balancing the materials
that flow through a system. It involves the systematic and
sequential technique in indentifying some variable sets which are
related by some sets of linear or non-linear equations whose
solution depends on the resulting degree of freedom for the
system. This degree of freedom provides us with the limit of
freedom for which we can set values for some of the variable
which is referred to as the design variables. A choice of values for
the design variables result in a corresponding value for the
remaining variables. The solutions to the equation set are
obtained by the various method of solution for simultaneous
equations, most appreciably the methods of substitution and
elimination. The algebraic method is most efficient for simple
system but it may be inappropriate for complex systems involving
large number of units. The split fraction and method is
recommended for such systems.
(b). Split Fraction Method

57
This method is based on the theory of recycle processes

published by Magier (1964). The method is based on the
realization that the basic function of most chemical processing
units (Unit Operation) is to divide the inlet flow of a component
between two or more outlet streams. This method is ideal in
carrying out material balancing of complex of multi-unit plants.
3.3 MATERIALS BALANCE ASSUMPTIONS
The following assumptions were made during the material

balance calculations:
1. The system is operating at steady state i.e. there is no

accumulation of any sort in the system.
2. There is negligible amount of inert in the process air.
3. Reasonably high conversion in the reactors.
4. Effect of side reactions is minimal.
3.4 SUMMARY OF MATERIAL BALANCE
CALCULATIONS
From the steady state material balance equation, the flow rates of
each stream are calculated as follows.
3.5 MATERIAL BALANCE FOR EACH UNIT
Basis: 1hr
THE COMPRESSOR
1a 1a
Stream 1 Stream 2
58
Stream 3
Components Stream 1( kg/hr) Composition Stream

1a( kg/hr)
O2 49720. O2 49720.
N2 187080 N2 187080
Total 236750 Total 236750
THE MIXER
Stream 2 Stream 5
Stream 4
59
Components Stream 2(Kg/hr) Stream 4 Stream 5(Kg/hr)

(Kg/hr)
O2 42760 - 42760
N2 160860 - 16086
NH3 - 13500 13500
H2O - 65 65
Total 203620 13565 217185
TOTAL 217185 217185
THE COVERTER
Stream 5 Stream 7
Stream 6
Composition Stream 5 Stream 6 Stream 7

60
O2 42760 - 11660
N2 160860 - 160860
NH3 13500 270 -
H2O 65 21060 -
NO - - 23320
HNO3 - - -
NO2 - - -
Total 217185 21330 195840
TOTAL 217185 217170
OXIDISATION VESSEL
Stream 7 Stream 8
Component Stream 7 Stream 8

(Kg/hr) (Kg/hr)
O2 11660 -
N2 160860 160860
NH3 - -
H2O - -
NO 23320 1460
HNO3 - -
NO2 - 33530
Total 195840 195850
61
ABSORBER Stream 6 + Make -up water
Stream 9
Stream 8
Component Stream 6 + Stream 8 Stream 9

make-up (Kg/hr) (Kg/hr)
water
(Kg/hr)
O2 - - -
N2 - 160860 160860
NH3 270 - 270
H2O 28120 - 23830
NO - 1460 8600
HNO3 - 30000
NO2 - 33530 672
Total 28390 195850 224232
62
TOTAL 224240 224232
STRIPPER Stream 10
Stream 9
Stream 3 Stream 11
Component Stream 9 Stream 3 Stream 10 Stream 11

(Kg/hr) (Kg/hr) (Kg/hr) (Kg/hr)
O2 - 6960 4030 30000
N2 160860 26170 160860 -
NH3 270 - - -
H2O 23830 - 4260 20000
NO 8600 - 580 -
HNO3 30000 - - -
NO2 672 - 7260 -
Total 224232 33130 176990 50000
TOTAL 257362 226990
63
COMBUSTION CHAMBER
Stream 13
Stream 10
Stream 12
Component Stream 10 Stream 12 Stream 13

(Kg/hr) (Kg/hr)
O2 4030 37370 2440
N2 160860 140580 301440
NH3 - - -
H2 - - 330
H2O 4260 - 26710
NO 580 - 410
HNO3 - - -
NO2 7260 - 7520
CH4 - - 860
C2H6 - - 50
CO2 - - 24480
Total 176990 177950 364240
TOTAL 354940 364240
64
PURIFICATION REACTOR
Stream 13 Stream 14
Component Stream 13 Stream 14

(Kg/hr) (Kg/hr)
O2 2440 2670
N2 301440 303790
NH3 - -
H2 330 170
H2O 26710 30230
NO 410 20
HNO3 - -
NO2 7520 380
CH4 860 -
C2H6 50 -
CO2 24480 27000
Total 364240 364260
Table 3.1: Summary of Material balance on each stream.
STREA COMPONENT FLOW RATE (Kg/hr) TOTA

MS L
65
HNO CH C2
O2 N2 NH3 H2O NO NO2 CO2
3 4 H6
4972 1870 2367
1 - - - - - - - -
0 80 50
4972 1870 2367
1a - - - - - - - -
0 80 50
4427 1608 2036
2 - - - - - - - -
60 60 20
2617 3313
3 6960 - - - - - - - -
0 0
135 1356
4 - - 65 - - - - - -
00 5
4276 1608 135 2171
5 65 - -
0 60 00 80
210 2133
6 - - 270 - - - - - -
60 0
1166 1608 233 1958
7 - - - - - - -
0 60 20 40
1608 146 335 1958
8 - - - - - - -
60 0 30 50
1608 238 860 300 2242
9 - 270 670 - - -
60 30 0 00 32
1608 426 726 1769
10 4030 580 - - - -
60 0 0 90
3000 200 5000
11 - - - - - - - -
0 00 0
3737 1405 1779
12 - - - - - - - -
0 80 50
3014 267 752 86 244 3642
13 2440 - 410 - 50
40 10 0 0 80 40
3037 302 270 3642
14 2670 - 20 - 380 - -
90 30 00 60
Table 3.2: Process matrix of the Nitric acid production process
EQUIPMENT ASSOCIATE
66
NUMBER NAME STREAMS

1 COMPRESSOR 1, -1a
2 SPLITTER 1a, -2, -3
3 MIXER 2,4, -5
4 CONVERTER 5, -6, -7
5 OXIDISATION UNIT 7, -8
6 ABSORBER 6, 8, -9
7 STRIPPER 3, 9, -10, -11
8 COMBUSTION 10, 12, -13
CHAMBER
9 PURIFICATION 13, -14
REACTOR
CHAPTER FOUR
ENERGY BALANCE
The Energy balance gives the account of all the energy

requirement of the process which is based on the principle of
conservation of energy. The principle states that energy can
either be create nor destroyed but can be transformed from one
form to another. Also energy can be transferred from one body to
another.
If a plant uses more energy than its competitor, its product could
be priced out of the market. Accountability of the energy
utilization of a process plant is necessary in every design project.
The conservation of energy however differs from the mass in that

energy can be generated (or consumed) in a chemical process.
67
Material can change form; new molecular specie can be formed in

a process unit and must be equal to the one out at steady state.
The same is not true for energy. The total enthalpy of the outlet
stream will not be equal to that of the inlet stream if energy is
generated or consumed in the processes, such as that due to heat
of reaction.
Energy can exist in various forms: head, mechanical, electrical

energy, and it is the total energy that is conserved. In plant
operation, an energy balance on the plant will show the patterns
of energy usage and suggest area for conservation and saving.
4.1 CONSERVATION OF ENERGY
As for materials balance, a general equation can be written for

energy balance;
Energy out – Energy in + Generation – Consumption =

Accumulation
This is a statement of the first law of thermodynamics. An energy

balance can be written for any process step. Chemical reactions
will evolve energy (exothermic) or consume energy
(endothermic). For steady state processes, the accumulation of
both mass and energy will be zero (0).
68
Energy exists in many forms; the basic forms are listed below:
Potential Energy: This is due to position or height due to motion
Internal Energy: This is the energy associated with molecules

and is dependent on temperature.
Work: This is achieved when a force gets through a distance.

Work done on a system is positive while work done by a system is
negative
Kinetic Energy: This is the energy due to motion.
W Q
Z1
For unit mass of material
Z2
2 2
U U
U 1 + P1 V 1 + 1 + Z 1 g+Q=U 2+ P2 V 2 + 2 + Z 2 g+W
g g
Where, Q = Heat transferred across the system boundary
W = Work done by the system
P1P2 = Pressure in Pressure Out
V1V2 = Volume in, Volume out

69
U1U2 = Velocity in, Velocity out
Z1Z2 = Height in, Height out
g = Acceleration due to gravity (9.81m/s 2)
U2
In chemical processes the kinetic energy factor ( )
g and the
Potential energy factor (zg) are small and negligible and the
relation between U and PV is correlated in terms of enthalpy (H)
H = U + PV
H2 – H1 = Q – w
Also, the work term can be negligible in many chemical

engineering systems. Hence,
H 2 - H1 = Q
4.2 ENERGY BALANCE ASSUMPTIONS
1. The process is at steady state
2. No heat is lost from the vessel and from the pipe i.e. there is
proper lagging.
3. Effect of pressure on enthalpy is ignored .
4. Potential and kinetic energy changes are negligible.

70
4.3 SUMMARY OF ENERGY BALANCE
THE COMPRESSOR
Tin= 20°C Tout=155°C
TABLE 4.1: HEAT BALANCE AROUND COMPRESSOR.
Component nin (Kg/hr) Hin (KJ/Kg) nout (KG/hr) Hout (KJ/Kg)

N2 187030 0 187030 140.4
O2 49720 87.56 49720 87.56
PROPERTIES QUANTITY/VALUE
Inlet Temperature( °C ) 20
Outlet Temperature( °C ) 155
Heat duty( KJ/hr ) 26259012
Power and Actual Shaft work, 399515.49 and
repectively.(KJ/hr and KJ) 475613.68
TABLE 4.2 HEAT BALANCE ABOUT THE AIR HEATER
For air component that passes through the air heater

N2 187030 0 187030 80.79
O2 49720 152.49 49720 152.49
Inlet Temperature (oC) 155
Outlet Temperature (oC) 200
Heat Duty( KJ/hr ) 15107946.75
For nitrous gases recycled back to the air heater

71

N2 160860 -161.10 16080 -161.10
NO 1460 0 1460 -155.11
NO2 33530 -196.5 3350 -196.5
Heat Duty( KJ/hr ) -226460.6
TABLE 4.3 HEAT BALANCE AROUND THE CONVETER

NH3 13500 0 270 1902.99
O2 42760 612.58 11660 612.58
NO2 - - 23320 610.38
N2 160860 693.63 160860 693.63
H2O 65 1309.44 21060 1309.44
Heat Duty( KJ/hr ) 20579273.83 KJ/hr
TABLE 4.4 HEAT BALANCE AROUND THE WASTE HEAT

BOILER (Unit 9)

O2 11660 -669.8 11660 -669.8
N2 160860 -719.25 160860 -719.25
NO 23320 0 23320 -685.09
Heat Duty( KJ/hr ) -15976252
Outlet Temperature of Steam 410
(°C )
72
TABLE 4.5 HEAT BALANCE AROUND THE OXIDIZING VESSEL

O2 11660 100.27 - -
N2 160860 107.80 160860 107.80
NO 23320 0 1460 103.96
NO2 - - 33530 131.00
Heat Duty( KJ/hr ) 1240891.54
TABLE 4.6 HEAT BALANCE AROUND THE STACK GAS

HEATER

N2 160860 -52.909 160860 -52.909
NO 1460 0 1460 -719.25
NO2 33530 -65.50 33530 -65.50

Heat Duty of Steam( KJ/hr ) -74322.76
Temperature of Steam (°C ) 118.48
TABLE 4.7 HEAT BALANCE AROUND THE ABSORPTION

COLUMN
73

NH3 270 0 270 576.48
H2O 28120 117597.84 23830 99657.0
N2 160860 167616.12 160860 167616.12
NO 1460 1437.66 8600 8586.24
HNO3 - - 30000 51600.0
NO2 33530 43924.39 670 880.32
74
HEAT BALANCE AROUND THE AMMONIA VAPORIZER,

SUPERHEATER AND STRIPPER.
 AMMONIA VAPORIZER
Heat Duty = 14978 KJ/hr
Outlet Temperature = -28.20 °C
 THE AMMONIA SUPPERHEATER
Heat Duty = -1596252 KJ/hr
Outlet Temperature = 26.65 °C
 THE STRIPPER
Heat Duty = -25873200 KJ/hr
Inlet Temperature = 250 °C
Outlet Temperature = 120°C

75
CHAPTER FIVE
CHEMICAL ENGINEERING DESIGN
The equipment used in chemical process industries can be divided

into two classes: proprietary equipment such as pumps,
centrifuge, etc which are designed and manufactured by
specialist firms; non-proprietary equipment which includes the
reactor, heat exchanger, evaporators, still, condensers and
bleaching vessels.
The proprietary equipment will only be selected and specified

while the non-proprietary equipment will be designed as special,
one-off, items for the particular processes and purposes they are
expected to serve.
The chemical Engineer’s part in the design of “non-proprietary”

equipment is usually limited to “selecting” and “sizing” the
equipment. Same will be done in this design work.
5.1 PROCESS UNITS OF NITRIC ACID PRODUCTION

PLANT
The nitric acid process plant comprises:
1. Ion- Exchange Unit
This unit consists of series of packed beds containing various

organic polymer resins for the removal of unwanted divalent and
monovalent ions. Used for the generation of de-ionized water.
76
2. De-ionized water Cooler
Consist of finned fan-type cooler for cooling the circulating de-

ionized water.
3. Air Compressor
Here air is compressed in two stages. The first-stage compression

is a low-pressure compression from atmospheric pressure up to
310 kPa. An axial compressor is used which takes its shaft drive
from a gas turbine. The second compression utilizes a centrifugal-
type compressor. The centrifugal compressor is more efficient for
the air flow-rate (36 000 kg/h) and outlet pressure (1090 kPa). The
centrifugal compressor takes its shaft drive from the expansion of
tail gas. Intermediate to the two compression stages is an
intercooler which allows the air temperature to be lowered from
180°C to 45°C, with a pressure loss of 10 kPa. The temperature
drop enables a more efficient second compression stage.
4. Ammonia Vaporizer
This unit consists of a shell and tube-type heat exchanger with

two passes per shell on the tube side. Operating pressure is 1240
kPa. The exchanger is made from mild steel.
5. Ammonia Super-heater
77
It consists of a shell and tube-type heat exchanger of similar

mechanical construction to the ammonia vaporizer. It is
constructed from mild steel.
6. Reactor
The reactor is a pressure vessel operating in the range 1050 kPa

to 1100 kPa. The bottom section of the reactor is jacketed. Air is
preheated in this jacket prior to mixing with ammonia. The bottom
section of the reactor also contains a shell and tube-type heat
exchanger. This exchanger provides the final stage of tail-gas
preheating. Tail gas enters at 235°C and the reaction gases leave
the exchanger section of the reactor at 645°C.
7. Steam Super-heater
This unit superheats saturated steam from 250°C (and 4000kPa)

to 380°C. The product steam is of medium pressure and suitable
quality for ‘in-house’ application and also for export. The super-
heater cools the reaction gases from the reactor exit temperature
of 645°C to 595°C.
8. Waste-heat Boiler
A shell and tube-type exchanger required to heat pressurized

(4000 kPa) hot water from 117°C to a saturated vapour at 250°C.
The waste-heat boiler cools reaction gases from 595°C to 280°C.
9. Tail-gas Pre-heater
78
Also comprises of shell and tube-type exchanger. It takes reaction

gases leaving the platinum filter at about 315°C and 1020 kPa,
and subsequently reduces their temperature to 185°C. The
cooling medium is tail gas. It enters at about 50°C and leaves the
tail-gas pre-heater at 235°C.
10. Cooler/Condenser
This unit condenses weak nitric acid from the gaseous mixture
and cools the remaining gases from an inlet temperature of 185°C
to 60°C. The shell and tube-type heat exchanger uses de-ionized
water as its cooling medium.
11. Oxidation Unit
The oxidation unit is an empty pressure vessel that takes input

reaction gases and blends in additional air from the bleaching
column. The extra oxygen provided enables further oxidation to
occur and raises the gas mixture temperature to 140°C. At the
top of the oxidation unit is a mist eliminator to prevent carry-over
of acid vapor by entrainment. At the bottom of the vessel is the
weak-acid drain.
12. Secondary Cooler
The secondary cooler takes the exit gases from the oxidation unit
at 140°C and cools them down to 65°C, a suitable temperature for
entry into the absorption column. The cooling medium is
79
circulating warm water from the warm-water loop. The inlet

temperature is 50°C and the exit temperature is about 80°C.
13. Absorber
The absorber is usually a sieve tray-type column. It has an

operating pressure around 990 kPa. A bursting disc is used for
pressure relief. Each tray is provided with cooling coils to allow the
cooling of the absorption liquor. There are two independent
cooling circuits, each uses de-ionized water. The top section has
an inlet temperature of 7°C and an outlet temperature of 20°C.
The bottom section cooling loop has an inlet temperature of 20°C
and an exit of 40°C. The use of two cooling circuits provides
greater flexibility in manipulating absorption conditions in the
column. The tail gas leaves the column at about 10°C. Weak acid
from the cooler/condenser is added to an appropriate tray midway
up the column, and make-up water at 7°C is added to the top tray.
The acid drained from the bottom of the column contains some
dissolved nitrogen oxides.
14. Stripping Column
The bleaching column is a smaller sieve tray-type column. Impure

acid runs down the column from the top tray and air is bubbled up
through the liquor to remove dissolved nitrogen oxides. The acid
from the base of the column is the final desired 60% (wt.)
product.
15. Storage Tank

80
Stores the supply of nitric acid produced from the process

plant.
CHAPTER SIX
EQUIPMENT DESIGN
The need to design process equipment may arise as a result of

the desire to:
i. Modify an existing process equipment or

ii. Develop new equipment.
81
Modification of existing equipment may be required as a result of

poor performance or the need of scale up (or down). For example,
increased market success of a product may lead to increased
production. It may be more economical to increase the capacity of
the existing equipment rather than add another line of
equipment. This is usually the case when operational cost costs
(man power, energy etc.) are high.
New equipment, on the other hand may be desired as a result of

successful laboratory research and pilot plant studies or as a
result of satisfactory process simulation using the computer.
In either situation (new or existing equipment), the actual design

commences with the assessment of the characteristics of the feed
materials, the products and the physical and chemical processes
required to convert the raw material to products. The overall
satisfactory performance and reliability of the equipment would
depend on the following factors.
I. Optimum processing conditions

II. Appropriate materials of construction
III. Strength and rigidity of components
IV. Satisfactory performance of mechanical part
V. Reliable methods of fabrication
VI. Ease of maintenance and repairs
VII. Ease of operation and control.
VIII. Safety requirements
IX. Environmental impact
The typical process equipment design procedure will involve:
1. Specifying the problem

82
2. Analyzing the probably solution

3. Preliminary design, applying chemical engineering process,
principles and theories of mechanics relevant to the
problem.
4. Selecting appropriate materials of construction.
5. Evaluating and optimizing the design, the possible
application of computer aided design (CAD) system like
HYSIS, Aspen Plus etc
6. Preparing the drawings and specifications
6.1. PROBLEM SPECIFICATION
The specification of the problem is the key stone in the quest to

design an equipment to meet the needs of the customer.
Specification of a problem may include:
1. The quantity of material to be processed in a given time

such as the proposed capacity of the equipment.
2. The physical and chemical properties of the product.
Constraints such as:
a. Availability and cost of materials of construction

b. Availability and cost energy, water, oil etc.
c. Budget for production
d. Availability and cost of manpower with relevant skill for
fabrication
e. Space to be occupied by the equipment
f. Environmental issues
g. Safety issues
h. Number of working days in the year
i. Ergonomics
83
6.2. ANALYZING THE PROBLEM SOLUTION
A thorough analysis will reduce the list for example if the

equipment is to be used for small scale processing. All the
constraint listed above will need to be considered.
6.3. PRELIMINARY DESIGN: APPLYING CHEMICAL

ENGINEERING
PROCESS PRINCIPLE AND THEORIES OF
MECHANICS.
Probably the most important expression in the design of process

equipment is that of mass and energy balance which may be
expressed in general term as;
Input + generation – output – consumption = accumulation
This expression is found in various forms in thermodynamics, fluid

mechanics, transport phenomena, heat transfer, separation
process and other subject areas. It is simply an expression of
indestructibility of matter and energy. This expression applies to
all raw materials, intermediate and product.
6.4 MATERIAL SELECTION
Materials are critical in the design of process equipment. Materials

must be selected to take care of possible corrosion problems.
Materials of construction should also possess adequate
mechanical properties to withstand tensile, compressive, shear
and impact stresses.
84
Stainless steel of various grades finds wide application in process

equipment design especially for parts in contact with raw
materials and product. Glass, plastic and rubber lined vessels are
also used are also used when materials tend to react with steel.
Steel of various carbon contents are used for compounds such as
shaft, springs and gears and for support structure.
6.5 DESIGN OPTIMIZATION
The calculation process in the design of equipment may require

simple arithmetic, algebraic, differential calculus or integral
calculus. In many cases an exact solution may not be feasible
thus necessitating the use of various approximation techniques
such as graphical or numerical methods.
In many cases also, only some parts of the equipment are

designed on the basis of analytical calculations. Practical
conditions are used to determine the specifications of the
remaining part. It is thus not unusual to have several feasible
solutions. There is thus the need to select the best solution. The
ultimate goal is to minimize cost or maximize profit.
In chemical process industries, equipment used are classified into

two; Proprietary equipment such as pumps, centrifuges which are
designed and manufactured by a specialist firm.
Non- proprietary equipment such as reactors, heat exchangers,

condenser, bleaching vessels etc are designed as specially
requested.
85
6.6 SUMMARY OF THE DESIGN AND SPECIFICATION

OF EQUIPMENT CALCULATION.
In designing and specifying of equipment for chemical industries,

the variables /parameters involved namely; pressure,
temperature, density, volume, area, diameter, height, heat duties,
heat capacities etc must be carefully calculated. This gives the
designer exact data for fabrication and manufacturing. For the
production of Nitric Acid; the following equipment are designed
and specified; Nitric Acid storage tank, Ammonia storage tank,
Absorber, Converter, Oxidation vessel, heat exchangers.
 FOR REACTORS
The operating intensity is given for the
reactors=11296.324kg/m2/24hrs
=11296.324kg/m2/day
Equipment Mass of Area(m2) Diameter(m)

reactant (kg/h)
Converter 13500 28.68 6.04
Oxidation 23320 49.55 7.94
Vessel
Absorber 33530 71.24 9.52
The stripper column has 10 plates
 FOR STORAGE TANKS
Equipment Type Nitric Acid storage

tank
86
Shape Cylindrical
Nature Insulated
Material of Stainless Steel
Construction
Capacity 50000000kg/hr
Volume(m3) 23.8
Diameter(m) 4.6
Height(m) 13.9
Equipment Type Ammonia Storage tank

Shape Cylindrical
Nature Insulated
Material of Construction Stainless Steel

Capacity 13565kg/hr
Volume(m3) 66.8
Diameter(m) 6.5
Height (m) 19.6
 FOR HEAT EXCHANGERS

Using the formulae; Q=AUDTm
A= Q/UdTm
Where
Q= Heat Duty of the heat exchanger(KW)
A= area(m2)
U= Overall Heat Transfer Coefficient(KW/m2)( This is assumed for
all)
DTm=Log Mean Temperature Difference(Celsius)
87
Using a countercurrent flow; DTM= DT1 −¿ DT2/ ln(DT1 /DT2)

DT1 = Thin-Tcout
DT2 = Thout –TCin
Equipment Q (KJ/hr) Thin Thout TCout Tcout
Waste Heat Boiler (1) 15976252890 250 30 410
Air Heater 350 200 150 250
Stack 74323 200 150 30 118.5

Gas
Heater
Waste 149781.4 208 50 150 32
Heat
Boiler(2)
NH3 4437.85 410 330 26.6 28.2
Super
Heater
NH3 149781.4 208 167.2 28.2 33.4
Vaporizer
Table 6.1: Table showing the heat transfer area of some

equipment
Equipment Q(KW/S) Area(M2)

Stack Gas Heater 20.65 2
Waste Heat Boiler(1) 4437.85 130.5
Waste Heat Boiler(2) 41.61 11.83
NH3 Super Heater 4437.85 127.6
NH3 Vaporizer 41.61 1.87
Air Heater 4133.7 588.7
88
CHAPTER SEVEN
PROCESS CONTROL AND INSTRUMENTATION
Instruments are provided to monitor the key process variables

during plant operation. They may be incorporated in automatic
control loops, or used for the manual monitoring of the process
operation. They may also be part of an automatic computer data
logging system. Instruments monitoring critical process variables
will be fitted with automatic alarms to alert the operators to
critical and hazardous situations.
It is desirable that the process variable to be monitored be
measured directly; often, however, this is impractical and some
dependent variable, that is easier to measure, is monitored in its
place.
7.1 OBJECTIVES
The primary objectives of the designer when specifying
instrumentation and control schemes are:
1. Safe plant operation:
(a) To keep the process variables within known safe operating
limits.
(b) To detect dangerous situations as they develop and to provide
alarms and automatic shut-down systems.
(c) To provide interlocks and alarms to prevent dangerous
operating procedures.
2. Production rate: To achieve the design product output.
89
3. Product quality: To maintain the product composition within the

specified quality standards.
4. Cost: To operate at the lowest production cost, commensurate
with the other objectives.
These are not separate objectives and must be considered
together. The order in which they are listed is not meant to imply
the precedence of any objective over another, other than that of
putting safety first. Product quality, production rate and the cost
of production will be dependent on sales requirements. For
example, it may be a better strategy to produce a better-quality
product at a higher cost.
In a typical chemical processing plant these objectives are
achieved by a combination of automatic control, manual
monitoring and laboratory analysis.
7.2 PLANT CONTROL CONFIGURATION
The plant will be designed for manned operation and will be linked
to the adjacent fertilizer manufacturing plant. Certain
configurations will be put in place to monitor some key
parameters of the plant.
The acid plant process control will be embedded in the plant DCS.
The instruments of the individual process units will be terminated
in junction boxes located at the unit’s skid limits. From here these
instruments will be connected to instrument cabinets in the
auxiliary room and integrated in the PAS.
The plant safety instrument system (SIS) will be independent of
the PAS. There will be a link between the PAS and the SIS for data
90
monitoring/logging and maintenance/operational override control

purposes. Fire and gas monitoring will also be a dedicated module
integrated in the safeguarding system.
The process control schemes of some vital units are discussed as
follows:
Absorption column
The process control scheme for the absorption column is

presented in fig It was designed from the recommendations
presented in the HAZOP analysis.
It features ratio control on the make-up water stream. The signals

from flow transmitters on this line and on the gas input line are
fed to the ratio controller, whereby the make-up water stream is
adjusted.
Other control features include a pressure controller on the tail-gas
outlet stream so that the column absorption pressure can be
maintained at the design operating value of 950 kPa. A
temperature transmitter on the tail-gas outlet stream provides the
signal for control of the overall cooling-water flow rate. This is the
temperature which is most useful in determining good absorption.
The cooling circuit itself is fed from a common line (on which the
overall flow rate is controlled). Small block valves on each of the
tray cooling-coil feed lines enable flow rate regulation to each of
the coils. These valves feature a removable top whereby a
magnetic flow meter may be inserted to read the flow rate. The
valves need only be set initially and then periodically adjusted
manually.
91
There is no automatic control on the flow rate of the gas inlet

stream or weak-acid condensate stream, since both of these flows
are predetermined by feed flow rates earlier in the process.
Isolation valves and provision for spectacle blinds are included to
enable the column to be isolated during shutdown periods.
The product-acid solution is withdrawn from the column using a
level control valve on this line. The liquid level in the base of the
column must be maintained slightly above the level of the plate
downcomer to prevent incoming gas from by-passing the sieve
plates.
All controllers suggested for the absorption column feature HIGH
and LOW alarms for good control.
The final safety requirement is a relief line with a relief valve
protected by a bursting disc.
 Air heater
The process control scheme suggested for the air heater is shown
in Fig. This flow scheme features a control valve on the
compressed air inlet line. A temperature controller taking its
signal from the heater outlet line ensures the flow is regulated to
maintain the heater temperature of 250°C. Air pressure is
controlled prior to entry into the unit and is kept constant at 7.3
atm.
A pressure indicator on both inlet and outlet steam lines enables
this parameter to be adequately monitored.
92
The nitrogen oxide reaction gas stream cannot be directly

controlled from the air heater. Instead the flow rate, temperature
and pressure are predetermined by the reactor feed conditions.
Both inlet and outlet lines possess isolation valves for plant
shutdown. These lines would be blanked before any platinum
recovery work was attempted on the heater. Inlet and outlet lines
also feature temperature indicators, consistent with the policy of
constant monitoring of this parameter throughout the process.
 Ammonia Vaporiser and Superheater
Pressure indicator and controller will be installed to maintain
ammonia vapor at 7.3 atm. Temperature indicator and controller
is required to ensure that the outlet temperature of 250°C is
achieved in the superheater. The control scheme is shown in the
figure below.
 Ammonia Converter
Temperature control system is needed within the converter to
ensure that the temperature in the converter does not drop below
the reaction temperature of 890-900°C, to avoid loss of heat.
7.3 ALARMS, SAFETY TRIPS AND INTERLOCKS

Alarm systems need to be installed in specific areas to alert
operators of serious, and potentially hazardous, deviations in
process conditions. Key instruments are fitted with switches and
relays to operate audible and visual alarms on the control panels
and annunciator panels. Where delay or lack of response, by the
operator is likely to lead to the rapid development of a hazardous
93
situation, the instrument would be fitted with a trip system to take

action automatically to avert the hazard; such as shutting down
pumps, closing valves, operating emergency systems.
The basic components of an automatic trip system are:
1. A sensor to monitor the control variable and provide an output
signal when a preset value is exceeded (the instrument).
2. A link to transfer the signal to the actuator, usually consisting
of a system of pneumatic or electric relays.
3. An actuator to carry out the required action; close or open a
valve, switch off a motor.
The high-temperature alarm operates a solenoid valve, releasing
the air on the pneumatic activator, closing the valve on high
temperature.
7.3.1 INTERLOCKS
Where it is necessary to follow a fixed sequence of operations for
example, during a plant start-up and shut-down, or in batch
operations interlocks are included to prevent operators departing
from the required sequence. They may be incorporated in the
control system design, as pneumatic or electric relays, or may be
mechanical interlocks. Various proprietary special lock and key
systems are available.
Table 7.1: Letter Code for Instruments Symbols
Property First letter Indicating only Controlling
measured only
Flow – rate F FI FC
Level L LI LC
Pressure P PI PC
94
Temperature T TI TC
Humidity H HI HC
I- Indicator C - Controller
L- Level T - Temperature
F- Flow rate P - Pressure
H- Humidity
(Source: Sinnott, R.R 1999).
7.4 LINING, PIPING, VALVES AND PUMPS
In Fig.7.1, which is the piping and instrument diagrams, there are

various mechanical component introduced in the plant to obtain
maximum efficiency some of which includes, flanges, valves,
piping lines, blinds, gaskets and so on.
7.4.1 VALVES
The valves used for chemical process plant can be divided into
two broad classes, depending on their primary function:
 Shut-off valves (block valves), whose purpose is to close off

the flow.
 Control valves, both manual and automatic, used to regulate
flow.
The table below shows some of the valves used in the P and I
diagram (figure 5), their symbols, and functions.
Table 7.2: Types of Valves and Symbol Used In PID
NAME SYMBOL FUNCTIONS

95
Control
Valves Used to control flow in lines.
Automatic Fitted on sensitive lines and are

Valves either pneumatically or digitally
controlled.
Check
Valves
Fitted in lines of relatively high
pressure or velocity
Butterfly
Valves
Used for control of gas or vapour

flows
7.4.2 JOINTS
There are various joints used in fig 3.0 either as flow reducers, or
to aid the carrying property of pipe. And effective transport of
fluids in the piping flow. Below is a table of the various elbows and
joints used in the P and I diagram:
96
Table 7.3: Joints
JOINTS SYMBOLS FUNCTIONS

AND
ELBOWS
EQUAL ‘T” Used to reduce a flow
REDUCER JOINT line into three equal
lines
Used in joining a
90o T – running line to a flow
CONNECTOR line.
Used in channeling lines

also reduces flow
ELBOW
speed.
Used in channeling lines

in pipe support.
LONG – RADIUS
ELBOW
Used in branching lines.
45o LATERAL
Used in reducing
pressure flow.
CHAPTER 8 97
SAFETY AND ENVIRONMENTAL

CONSIDERATIONS
REDUCER
8.1 SAFETY
Safety is the condition of being protected against any danger.

Every organization has a legal and moral obligation to safeguard
the health and welfare of its employees and the general public.
7.5 PIPE SUPPORT
The good management practices needed to ensure safe operation
The Design
will also of a plant’s
ensure P and Ioperation.
efficient is not complete
In a without
chemicaltheprocessing
use of
supports. Pipe
industry, thesupports in plant
chemicals used piping helps incan
or produced reducing cost and to
be hazardous
number of or
humans pump required to maintain
the environment line flow
if not properly parameter
handled and thisand
could
safety of personnel
equally through
lead to a lot operation
of damage zone. and financially.
structurally
Below
The is some
best major type are
organizations of support:
those that have come to the realization
that provision of safety is not only the right thing to do for their
I – BEAM Support to carry pipe lines
employees, it is also profitable.
H – BEAM Support above 2m
 Advantages of a safe working environment
U – CHANNEL
1. Ultimately, safety leads to more profit as less money is spent
PLATES taking
TO ALIGN VALVES
care of legal bills, hospital bills, and repair of
equipment.
SHOES TO HOIST PIPE INTO PROPER ORIENTATION
2. It gives the company a good name.
3. Happy employees which increases their job performance.
Safety is usually considered in three classes:
I. Safety of the environment

II. Safety of the personnel
III. Safety of the plant and equipment.
98
The term “engineering safety” covers the provision in the design

of control systems alarms, trips, pressure relief devices, automatic
shutdown system and duplication of key equipment, firefighting
equipment and service; personnel protect equipment and so on.
99
8.1.1 SAFETY OF THE ENVIRONMENT
There are several hazards associated with industrial process.

These hazards need to be prevented and kept in check in order to
protect the environment. Environment in this context refers to the
immediate surroundings around the plant. For the safety of the
environment to be ensured, the following points should be noted
and applied;
1. Flaring of gases should be done minimally.

2. The level of toxicity of effluent should be monitored regularly
and kept in check.
3. Storage tanks should be situated in areas away from vehicle
traffic.
4. The control room should be attended to at all times to
ensure that there is an immediate response if an alarm is
triggered.
5. There should be a way of informing the community around
the facility if there is danger that might affect them e.g Fire.
An alarm is suggested, and this should be tested regularly.
6. Protect pipe racks and cable trays from fire.
7. Fire-fighting system must be provided within the complex.
This consist:
 Fire water pipe network throughout the facility supported by
necessary hydrants. Hoses should be permanently placed
near these hydrants.
 The system should have a suitable water pump. It is advised
that there be at least 2 pumps. One big one to fill the lines or
pump large volume of water into it (when the water is being
depleted very fast like in a case of fire) and a smaller jockey
100
pump to maintain the pressure in the line. It would start

more frequently than the big pump.
 It is suggested that the system should have its own separate
standby generator.
 Fire entry suits and other protective clothing, compressed air
breathing apparatus and fire blankets should be made
available in every building.
8.1.2 SAFETY OF THE PERSONNEL
The personnel of a company refers to the operators and staff of

that company who ensure that the production process move on
smoothly. Their safety can be ensured in the following was.
1. Provision of personal protective equipment (PPE) and

ensuring that they are properly used.
2. Pipes and equipment that contain very hot liquids for
example the heater must be lagged to make sure it does not
cause injury to personnel.
3. All chemicals in the plant must be properly label with its
chemical hazard identification chart and their Material
Safety Data Sheet (MSDS) must be available and updated
regularly also.
4. First aid kits must be provided in all buildings.
5. Emergency means of transportation must be provided in
case of any accident.
6. Emergency exit doors must be provided and these exits
clearly marked for all to see.
7. Cleanliness of the facility must be ensured at all times to
avoid unnecessary risk or accident.
8. Smoking should be avoided in process area.
101
9. Fire extinguishers must be made available at strategic

points within the facility.
10. All ladders must have hand rails and personnel encouraged
to use them whenever climbing.
11. Safety signs and symbols should be placed at hazardous
area.
8.1.3 SAFETY OF THE PLANT AND EQUIPMENT
A plant includes any machinery, equipment (including scaffold),

appliance, implement or tool and any associated computer or
fitting used in the production process of a material or substance.
There are different types of risks associated with using different
types of equipment. To mitigate this risk, the following must be
done:
1. As Nitric acid is known to be highly corrosive, regular

pigging of the pipelines with both smart and scraper pigs
should be conduct so as to check this.
2. Corrosion protection is achieved by the well proven use of
suitable austenitic stainless steel where condensation can
occur and by regular monitoring of the conditions.
3. Regular maintenance of equipment should be carried out.
4. Check to ensure that equipment and machineries meet
health and safety standards before it is purchased.
 REACTOR
Reactor is a vessel in which chemical transformation takes place.
The converter, oxidizing unit and absorber are the reactors in this
design. The catalytic reactor is designed to give a uniform
distribution of the air/ammonia mixture over the catalyst gauzes.
102
Maintenance of the catalyst operating temperature is very

important for the NO yield. This is achieved by adjusting the
air/ammonia ratio and ensuring that the lower explosive limit for
ammonia in air is not exceeded. The following safety steps should
be followed in the design and operation of the reactor.
 The materials going into the reactor must be purified. This is

done to remove impurity that will affect the reactor.
 The reaction condition i.e. temperature, pressure etc must
be monitored closely.
 The reactor should be cleaned accordingly during periodic
maintenance.
 COMPRESSOR
While operating the compressor, the following precautions should
be observed.
 The air must be dried properly to avoid water entering into

the compressor which could damage it.
 The air must be filtered properly to avoid foreign particle
from entering into the compressor.
 The proper operating pressure should be maintained at all
times.
 Coolant must be checked regularly and topped.
 In case of shut down, the shut down and start up procedures
should be strictly adhered to.
 HEAT EXCHANGERS
For heat exchangers to work effectively and safely, the following
must be implemented.
103
 Ensure that the heat exchanger is pressure tested as

designed.
 Ensure that it is cleaned periodically and faults and leakage
rectified if found. Inspect after cleaning before coupling
back.
 The water must be purified especially the one going into the
boiler to remove chlorine because ignition occurs when
chlorine is passed into ammonia forming nitrogen and
hydrochloric acid and if chlorine is present in excess, then a
highly explosive nitrogen trichloride (NCl3) is formed. As we
cannot guarantee 100% conversion of ammonia in the
converted and no leak in the boiler, the water should be
purified.
 PUMPS
For the pumps to work effectively and safely, the process
operators should ensure that;
 The right operating temperature and pressure must be used.

 There should be a minimum flow line that helps to maintain
a certain rate of flow in the pump preventing it from going
into cavitation.
 Lube oil to gland bearings is available, bottle filled and ready.
The lube oil should be changed at regular intervals.
 The vents should be properly cleaned and capped
 There should be no particle or foreign body in both the
suction and discharge lines.
 TANKS
Nitric acid is normally stored in flat bottomed, roofed tanks, made
from low carbon austenitic stainless steel, installed in areas
104
provided with suitable containment facilities. The acid level in the

tank is monitored by means of a level indicator. A vent to the
atmosphere allows the escape of gas which comes from liquid
movement and thermal effects. It is normal to earth the tanks. For
the life span of the tanks to be preserved, the following should be
done:
 The tank should be cleaned regularly

 Periodically, the tanks should be checked for corrosion and
the affected part could be painted.
 The right operating conditions for the tanks must be
maintained.
8.1.4 GENERAL SAFETY PRECAUTION
Generally, precaution is taken to prevent accidents or hazards (a

potential danger). Hazards can either be intrinsic or extrinsic.
Intrinsic hazards are naturally occurring hazards caused by wind,
earthquake, lighting and water. The effects of intrinsic hazards
include leakage in pipes, explosion of pipes, collapse of
production buildings, rupture of welded joints etc. the following
precautions can be taken to mitigate the dangers posed by
intrinsic hazards:
 Lightning rods should be installed at strategic points.

 Drainages should be wide and deep enough, and should also
be channeled properly to prevent flooding with the facility.
 Explosive substances have to be stored in a cool dry place
away from sunlight and ultraviolet rays.
105
 The floor around the industry should be properly cast around

with concrete or other weather resistant covering and the
road networks properly tarred
Extrinsic hazards are man-made hazards caused by man due to

carelessness.They may include dropping of an oil filter on the
floor, igniting flame close to a flammable substance, not knowing
how to operate a machine or equipment, ignoring procedure for
starting or using equipment, using wrong tools. They can be
prevented by the following measures:
 Personnel coming into the facility for the first time must be
given a proper safety orientation on the do’s and don’ts of
the company policy on safety and regular safety talks on
safety and maintenance of plant must be conducted.
 Regular training of personnel on safety issues should also
take place.
 Good housekeeping practice by all employees should be
encouraged.
8.2 HAZARD OPERABILITY (HAZOP) STUDY

Hazard and operability study sometimes simply referred to as
operability Studies, provide a systematic and critical
examination of the operability of a process. They indicate
potential hazards due to deviations from the intended design
conditions.
8.2.1 BASIC PRINCIPLES

106
A formal operability study is the systematic study of the design,

vessel by vessel, and line by line, using “guide words” to help
generate thought about the way deviations from the intended
operating conditions can cause hazardous situations.
The following words are also used in a special way, and have
the precise meanings given below:
• Intention: the intention defines how the particular part of

the process was intended to operate; the intention of the
designer.
• Deviations: these are departures from the designer’s

intention which are detected by the systematic application of
the guide words.
• Causes: reasons why, and how, the deviations could occur.

Only if a deviation can be shown to have a realistic cause is it
treated as meaningful.
• Consequences: the results that follow from the occurrence

of a meaningful deviation.
• Hazards: consequences that can cause damage (loss) or

injury.
107
108
Table 8.1 HAZOP STUDY: Weak-acid condensate stream
Deviation Possible consequences Consequence Action Required

No Flow 1.Pump Failure Deficient quality product a) Install LOW LEVEL ALARM
and high NOx tail gas on LIC at the base of the
emission levels. absorption column.
2. Valve fails shut. As for I Covered by a).
Valve overheats. b) Install kick-back on pumps
3. Line fracture As for I and 2. Covered by a) and b).
c) Regular inspection and
patrolling of weak-acid
transfer lines and seals.
More Flow 4. Higher humidity in Higher make but weaker d) Install a HIGH LEVEL
feed air. product acid. ALARM on LIC at the base of
the absorption column
More Temperature 5. high feed rate causing Possible higher NOx See Table 8.6.
larger heat of reaction emission.
More Pressure 6. Isolation valve is Lines subject to full Covered by b)
closed in error while delivery pressure f) Perhaps worthwhile
pump running. installing a pressure gauge
upstream of the delivery
pump
7. Thermal expansion on Possible line fracture or g) Provide thermal expansion
the isolation. flange leakage relief in the
Valve section.
Less Flow 8. Flange leakage or Decreased absorption. Covered by a), c), and d).
valve Lower product make
stub blanked but leaking
Less Temperature 9. Reaction gas Increased dissolved NOx See Table 8.6.
temperature in oxidation concentrations in
109
unit lower. product acid.

Maintenance 10. Equipment failure, Process stops. Ensure all pipes and fittings
flange leak, catalyst are constructed of the right
changeover in reactor, materials and arc stress
etc. relieved.
Table 8.2 HAZOP study: Make-up water feed stream.
Deviation Possible causes consequences Action Required

No Flow 1.Pump Failure Deficient quality product a) Install LOW LEVEL ALARM
and high NOx tail gas on LIC at the base of the
emission levels. absorption column.
2. Valve fails shut. As for I Covered by a).
Valve overheats. b) Install kick-back on pumps
3. Line fracture As for I and 2. Covered by a) and b).
c) Regular inspection and
patrolling of weak-acid
transfer lines and seals.
More Flow 4. Control valve fails open Dilute acid product is d) Install a HIGH LEVEL ALARM
formed on
LIC at the base of the absorption
column
More Temperature 5. Higher feed temperature Possible higher NOx See Table 8.6
to the emission due to lower
Refrigeration unit. absorption. e) Ensure refrigeration unit is
6. Failure in the As for 5. well
refrigeration unit. maintained with adequate
110
control
More Pressure 7. Isolation valve is closed Line subject to full delivery Covered by b).
in error whilst pump pressure. IJ Perhaps worthwhile installing a
running. pressure gauge upstream of the
delivery pump.
Possible line fracture or g) Provide thermal expansion
8. Thermal expansion in flange leakage relief in the valve section.
the isolation valve section
(fire).
Less flow 9. Flange leakage or valve Decreased absorption. Covered by a),c) and d)
stub blanket but leaking Higher operating cost in
lost water
Less Temperature I0. Reaction gas Increased dissolved NOx See Table 8.6
temperature in oxidation concentrations in product
unit lower. acid.
Maintenance 11. Equipment failure, Process Stops Ensure all pipes and fittings are
flange leak, catalyst constructed of the right
changeover in reactor, etc . materials and are stress relieved.
Table 8.3. HAZOP study: Gas-inlet stream

111
No Flow 1.Flow stopped upstream No absorption in column. a) Ensure liquid feeds to

Entire process stops as tail- absorber and other process
gas Row stops. unit shut down.
b) Install LOW FLOW
ALARM on FIC.
2. Line blockage or the As for I. Covered by a) and b).
isolation valve shut in error. Pressure buildup in pipe c) Install kick-back on
and secondary upstream pumps and
3.Line fracture As for I. ensure pressure relief
Gases escape into the system is adequate
surroundings. d) Ensure regular patrolling
of feed transfer lines.
e) Plant emergency
shutdown procedures
More Flow 4. Increased feed Possible reduction in F) Ratio control on the
absorption liquid feed streams should
Efficiency. be sufficient.
May cause flooding. g) Install HIGH LEVEL
ALARM on the FIC.
More Pressure 5.Flooding Unit subject to high Covered by c).
pressure, bursting discs h) Ensure correct sizing on
may rupture, tail gas pressure relief system.
6. Isolation valve release. Covered by b) and c).
accidently closed As for 2. i) Provide for thermal
7. Thermal expansion in Line fracture or flange expansion relief in the
isolation. leakage. design of the isolation
valve section
More Temperature 8. Insufficient cooling Decreased absorption, j) Ensure accurate
higher pollution. temperature control on the
internal cooling circuit.
Less flow 9. Leaking inlet range As for 3. Covered by b), and d)
Less Temperature 10. Overcooling. Increased dissolved gasses Covered by j)
112
in acid.
H i g h NOx composition 11. Improved yield from Higher tail-gas emission k) Manually increase make-
reactor. levels possible. up water Composition flow
rate.
Table 8.4. HAZOP study: Gas – Outlet stream.

No flow I. No inlet gas flow. No tail gas for expansion. See Table 8.1.
Pressure build up in column a) Install LOW LEVEL
and line ALARM on PIC.
2. Flooding in column. As for I. b) Install pressure relief
valve with bursting disc.
Covered by b).
3. PCV fails shut, line As for 2. c) Install HIGH LEVEL
blockage or isolation valve ALARM on PIC.
closed in error. Covered by a)
As for 1. d) Institute regular
4. Line fracture or flange inspection of all transfer
failure lines.
More flow 5. Increased gas feed at Transfer line subject to Covered by b) and c).
inlet. higher pressures. Covered by b) and c).
As for 5. d) Look to altering make-up
6. Decreased NOx Tail-gas emission levels up. water feed rate in
absorption response.
More Temperature 7. Higher feed gas or liquid Decreased absorption and e) Install HIGH LEVEL
inlet temperature. higher NOx emission. ALARM on TIC
More pressure. 8. All of 5, 6, and/or 7. As for 5, 6, and 7. Covered by b) and c).
9. Thermal expansion in Line fracture or flange f) Install thermal expansion
isolation valve section leakage. relief in isolation valve
(fire). section.
10. PCV fails shut or As for 3 Covered by b) and c).
isolation valve shut in error.
113
Less flow 11. Leaking flange or valve Less tail gas for expansion Covered by a) and d).
stub not blanked and and release of NOx to the
leaking. environment.
12. Flooding.
Liquid Carryover 13. The entrainment device Condensation is down, Replace entrainment
ineffective. steam lines (corrosion). device.
Maintenance 14. Equipment failure, Process stops. Ensure all pipes and fittings
flange leak, catalyst are
changeover in reactor, etc . constructed of the right
materials and are stress
relieved
Table 8.5 HAZOP study: Liquid-outlet stream.

No flow. I. No liquid inlet from either See Tables 9.6 and 9.7
make-up water or acid a) Covered by control and
condensate. alarms specified in Tables 8.1,
2. Flooding in column. Increase in column pressure. 8.2 and 8.3.
Liquid level in column Covered by a).
increases adding to flooding b) Install HIGH LEVEL ALARM on
problems. LIC.
3. LCV fails shut. c) Regular patrolling and
Discharge of acid into the inspection of transfer lines.
4. Line fracture.4. Line fracture. surroundings. d) Install suitable alarms to
Loss of feed to the stripping stripping
column column to indicate loss of flow
More flow 5. LCV fails open. Gas begins to bypass the e) Install LOW LEVEL ALARM on
plates causing higher NOx LIC.
emissions.
114
More temperature 6. Higher inlet temperatures Less dissolved NOx in acid Covered in Tables 8.1, 8.2 and
but higher NOx tail-gas 8.3.
emissions
More pressure 7. LCV fails shut or isolation Line subject to full surge or Covered by a)
valve close in error. delivery pressure.
Less flow 8. Leaking flange or valve stub Loss to surrounding. Covered by d) and e)
not blanked and leakage.
Less temperature 9. Lower inlet stream Higher concentrations of See Tables 8.1, 8.3 and 8.4.
temperatures or over capacity dissolved NOx in product
from cooling circuit. acid.
NOx dissolved 10. Lower steam temperature. Higher downstream See Tables 8.1,8.3 and 8.4
operating costs.
Same as 9.
maintenance 11. Equipment failure, flange Process stops Ensure all pipes and fittings are
leak, catalyst changeover i n constructed of the right
reactor, etc. materials and are stress
relieved
115
Table 8.6: HAZOP study: cooling-water circuit.

No Flow 1.Pump Failure High emissions of NOx in a) Install HIGH LEVEL ALARM on
tail gas. TIC on the tail-gas outlet line to
indicate high emissions.
2. Valve fails shut. Covered by a).
As for 1 b) Install kick-back on pumps.
3. Line fracture Valve overheats. Covered by a) and b).
As for 1 and 2 c) Regular inspection and
patrolling of
cooling-water circuit lines and
associated
More flow 4. Control valve fails open. Product acid is at lower d) Install a LOW LEVEL ALARM on
temperature therefore, TIC on the tail gas outlet line
higher dissolved NOx.
More temperature 5. Higher feed temperature Possible higher NOx Covered by a)
to the refrigeration unit. emissions due to lower e) Ensure refrigeration unit is
absorption. well
As for 5. maintained with adequate
control
More pressure 7. Isolation valve is closed Lines subject to full Covered by b).
in error while pump delivery pressure. f) Perhaps worthwhile installing a
running. Possible line fracture or pressure gauge upstream of the
8. Thermal expansion in flange leakage. delivery pump.
the isolation valve section g) Provide thermal expansion
(fire). relief in the valved section
Less flow 9. Flange leakage or Decreased absorption. Low Covered by a), c), and d).
valve stub blanked but quality product and high
leaking emissions.
Less Temperature 10. Higher duty from Increased dissolved NOx Covered by a), c), and d).
116
refrigeration unit. concentration in product

acid.
Maintenance 11. Equipment failure, Process stops Ensure all pipes and fittings
flange leak, catalyst are constructed of the right
changeover in reactor , etc materials and are stress relieved
117
8.3 ENVIRONMENTAL IMPACT ASSESSMENT (E.I.A)
This is the assessment of the possible positive and negative

impact that a proposed project may have in the environment,
together consisting of the environmental, social and economic
aspect. It is a systematic process of identification, prediction
evaluation, mitigating and presentation of possible
consequences on the environment of proposed actions at a
stage in decision making process so that environmental
damage can be minimized or avoided.
8.3.1 WHAT EIA DOES
• Describes the project or operation
• Describes the environment that will be affected
• Predicts the impact on the environment
• Adopts options, techniques and controls to reduce negative

impact.
• Monitors the project or operation to ensure that identified

key impact is minimized.
8.3.2 GOAL
• To ensure that decision makers consider the ensuing

environmental impacts when deciding whether to proceed with
a project or not.
118
8.3.3 BENEFITS OF ENVIRONMENTAL IMPACT

ASSESSMENT
• May be prerequisite for permit approval by government or

international agencies.
• Required by financiers of the proposed projects
• Help to prevent environmental problem, risk or costly-time

working liabilities.
• Boosts Proponent Company’s image.
• Repose confident /assurance in Proponent Company.
8.3.4 ENVIRONMENTAL IMPACT ASSESMENT (EIA) OF A

NITRIC ACID PLANT.
 Negative impact
The major negative impact of a nitric acid plant is NOx emissions
of the tail gas from the absorption tower especially during start up
and shut down before the plant stabilizes. Others include:
 Risk of fire/explosion hazard.

 Reduced soil and marine water quality.
 Increase in water and electricity demand.
 Noise pollution.
 Positive impact
 Provide skilled and unskilled job opportunities.
 Make available nitric acid in the country, thereby encouraging the
production of fertilizer as it is a major chemical used in its
production.
119
 Bring development to the area where the plant is sited.

8.3.5 NOx EMISSION FROM NITRIC ACID PRODUCTION.
Nitric acid production is one of the larger chemical industry

sources of NO. Unlike NOx found in combustion flue gas, NOx from
nitric acid production is part of the process stream and is
recoverable with some economic value. Vent gas containing NOx
is released to the atmosphere when the gas becomes too impure
to recycle or too low in concentration for recovery to be
economically practical.
The chemical reactions for each of the nitric acid production

process steps demonstrate that NOx must first be created before
nitric acid can be produced. The first reaction,
4NH3 + 5O2 ⇌ 4NO + 6H2O + heat
Eq. 1
Shows NO forming from the reaction of NH and air. The NO is then

oxidized in the second step,
2NO + O2 ⇌ 2NO2 + heat

Eq. 2
Producing NO2. The NO2 is subsequently absorbed in water to

produce nitric acid. However, as the absorption reaction,
3NO2(g) + H2O(l) ⇌ 2HNO3 (aq) + NO(g) + heat,
Eq. 3
120
Shows, one mole of NO is produced for every three moles of

NO2absorbed, making complete absorption of the NOx impossible.
The unabsorbed NOx, if not controlled, is emitted in the absorber
tail gas.
8.3.6 FACTORS AFFECTING NOx EMISSION LEVELS.

 Re-oxidation of NO into NO2 is a very slow reaction. As more
air is added, the reaction becomes increasingly slower as the
reactants become diluted with excess nitrogen.
 Increased temperatures due to exothermic absorption tend
to reverses eq. 3 producing more NO2.
 Low temperature (less than 38 0C [1000F]) is a key factor
forhigh absorption efficiency but is also one that is difficult
and expensive to control.
 Completion of the absorption process which reduces NOx
emission is aided by increased pressure (800 to 1,400 kPa)
 Increasing acid strength beyond design specification
typically increases the NOx emission rate.
 Good maintenance practices and careful control ofoperations
play important roles in reducing emissions of NOx.
8.3.7 CONTROL TECHNIQUES FOR NOx EMISSIONS

FROM NITRIC ACID PRODUCTION.
 Extended absorption
Extended absorption reduces NO emissions by increasing
absorption efficiency and is achieved by either installing a single
121
large tower, extending the height of an existing absorption tower,

or by adding a second tower in series with the existing tower.
Increasing the volume and the number of trays in the absorber
results in moreNOx being recovered as nitric acid (1-1.5% more
acid) and reduced emission levels.
 Non-selective catalytic reduction (NSCR).

Nonselective catalytic reduction uses a fuel and a catalystto
1. Consume free oxygen in the absorber tail gas.

2. Convert NO2 to NO for decolorizing the tail gas.
3. Reduce NO to elemental nitrogen.
The process is called nonselective because the fuel first depletes

all the oxygen present in the tail gas and then removes the NOx.
It can be operated at any temperature, heat used to operate it
can be recovered and it can achieve higher NOx reduction than
extended absorption but it is expensive due to the cost of fuel.
 Selective catalytic reduction (SCR)

Selective catalytic reduction uses a catalyst and ammonia in the
presence of oxygen to reduce NOx to elemental nitrogen. The
process is called selective because the ammonia preferentially
reacts with NOx in the absorber tail gas. The following sections
discuss SCR used as a NO control technique for nitric acid plants.
Proper operation of the process requires close control of the tail
gas temperature.
 Chilled Absorption.
122
Chilled absorption provides additional cooling to the absorption

tower. This process is frequently used in addition to other control
techniques such as extended absorption. The principal advantage
of chilled absorption is improved absorber efficiency due to lower
absorption temperature. However, chilled absorption by itself
typically cannot reduce NOx emissions to the level that any of the
three primary control techniques can achieve.
8.3.8 ENVIRONMENTAL MANAGEMENT PLANT
The following are actions taken to mitigate the negative impacts

of the plant sited above.
1. Use extended expander and chilled absorption to increase

absorber efficiency and thus reduce NOx emission.
2. Site the plant far away from residential area so as to reduce
noise pollution effect and risk of fire.
3. Update on site emergency response plan.
4. Have a generator to provide the electrical needs of the plant
and own water supply system.
5. Monitor stack gas emissions.
6. Test liquid waste to make sure the level of chemical in it is
acceptable before discharging to sea.
123
CHAPTER 9
ECONOMIC ANALYSIS
9.1 OVERVIEW
Chemical processes have been harnessed to transform resources,

and raw materials into more useful and hence more valuable
products to improve the living standards of people. This principle
is at the core of chemical engineering, and there industries have
matured over the last 100 years, and have been very successful
at creating wealth. The means of establishing which products to
make and how to optimize the process required for the
manufacture have been based on economic principles.
Approaches to accounting for the risks to the economic value of
projects are also considered to ensure that they deliver the
expected benefits.
9.2 ECONOMIC CONSIDERATION
The following are considered under economic evaluation;
1. Cost and Assets Accounting: This provides a survey of

accounting procedures for the analysis of cost and profits as
used for industrial applications.
2. Cost Estimation: This provides information regarding the
estimation of fixed capital cost and also recurrent operating
expenditure.
124
3. Interest and Investment costs: This discusses the

concept and calculation of interest, i.e payment as
compensation for the use of borrowed capital.
4. Taxes and Insurance: Taxes represent a significant
payment from a company’s earnings and although insurance
rates are only a small fraction of annual expenditure cover
for a plant is essential.
5. Depreciation: This is the measure of the decrease in value
of an item, with respect to time and can be considered as a
cost incurred for the use of the equipment.
6. Profitability, Alternatives, Investments and
Replacements: The profitability of an investment is a
measure of the amount of profit generated. It is important to
assess the profitability accurately and also the profit that
could be obtained from alternative investments.
10.4 TYPES OF COST
X.4.1 INDIRECT COST

1. Design and engineering cost; which cover the cost of
design and the cost of “engineering” the plant: purchasing,
procurement and construction supervision. Typically 20% to
30% of the direct capital cost.
2. Contractor’s fees: if a contractor is employed his fees
(profit) would be added to the total capital cost and would
range from 5% to 10% of the direct cost
3. Contingency allowance: this is an allowance built into the
capital cost estimate to cover for unforeseen circumstances
125
(labor disputes, design errors, adverse weather) typically 5%

to 10% of the direct cost.
Table 9.1: typical factors for estimation of project fixed capital

cost
MAJOR EQUIPMENT , TOTA; PCE

PURCHASE COST (F1 TO F9)
Equipment erection 0.40
Piping 0.70
Instrumentation 0.20
Electrical 0.10
Building process 0.15
Utilities 0.50
Storage 0.15
Site development 0.05
Ancillary buildings 0.15
9.4.2 Total physical plant cost (PPC)
PPC = PCE (1 + ∑factors ) = PCE × 3.4
Ranging from f10 to f12
Design and engineering 0.30

Contractors fee 0.05
contingency 0.10
Fixed capital = PPC (1 + f10 + f11 + f12) = PPC × 1.45
126
9.4.3 OPERATION COSTS
An estimate of the operating costs, the cost of producing the

product, is needed to judge the viability of a project and to make
choices between possible alternative processing schemes. These
costs can be estimated from the flow sheet, which gives the raw
material and service requirements, and the capital cost estimate
The cost of producing a chemical product will include the items

listed below. They are divided into two groups.
1. Fixed capital cost: Costs that do not vary with production

rate. These are the bills that have to be paid whatever the
quantity produced
2. Variable operating cost: Costs that are dependent on the
amount of product produced.
9.4.4 FIXED COSTS

1. Maintenance (labor and materials)
2. Operation labor
3. Laboratory costs
4. Supervision
5. Plant overhead
6. Capital charges
9.5 COST ESTIMATION
9.5.1 THE RATIO METHOD

127
The ratio method is a simple technique whereby known capital

cost data for an existing chemical plant are adjusted to provide a
cost estimate for the desired plant capacity. This method is also
able to update figures to account for inflationary effects of past
years. Finally the capital cost figure is adjusted for exchange rate
differences between countries .The method is centered around
the use of key cost estimation indices such as the CE plant cost
index and the Marshall and Stevens (M&S)index.
 Ratio method calculations;

n
capacity of designed
Cost of Designed plant ¿ Cost of previous plant ( Capacity of previous plant )
1200 tons 1200 0.6

Cost of =Costof 280 tons/day ×( )
day 280
cost of 280tons /day =¿ $ 60 million
Therefore;
0.6
1200
cost of 1200 / day=$ 60 million ×( ) = $143.66 million
280
= ₦22.7 billion
9.5.2 STEP COUNTING METHOD
Step counting estimating methods provide a way of making a

quick order of magnitude estimate, of the capital cost of a
proposed project. The technique is based on the premise that
the capital cost is determined by a number of significant
128
processing steps in the overall process. Factors are usually

included to allow for the capacity, and complexity of the
process: material of construction, yield, operating pressure and
temperature.
 step counting method calculations;

C=14000 NQ 0.615
Where Q=plant capacity, tonne per year.
N=number of functional units
C=capital cost.
Q=400,000tons/yr
N=13
0.615
C=14000× 13 ×( 400,000)
= $ 507 million equivalent ¿ 79.8 billion naira .
9.5.3 FACTORIAL METHOD
Capital cost estimates for chemical process plants, are often

based on an estimate of the purchase cost of the major
equipment items, required for the process, the other costs being
estimated as the factors of the equipment cost .The accuracy of
this type of estimate will depend on which stage the design has
reached at the time.
129
ECONOMIC ANALYSIS CALCULATIONS
ESTIMATION OF FIXED CAPITAL COST
 Rough Estimate
Cf = Fl Ce
Ce = ₦ 824.43 million
Cf = 4.7 × 828.43 = ₦ 3.89 billion
 Detailed Estimate
PPC = Ce ( 1 + ∑factors )
∑factors = 3.3
PPC = 824.43 (1 + 3.3) = ₦3.55 billion
Total Fixed Capital = 3.55 ( 1 + 0.45) = ₦ 5.15 billion
Working capital = 5% × 5.15 = ₦258 million
Total Capital Investment Cost = Total Fixed Capital + Working

Capital
Total Capital Investment Cost = 5.15 + 0.258 = ₦ 5.41billion
OPERATING COST ESTIMATION
Variable Cost ₦ million
1) Raw materials 0.25

130
2) Miscellaneous 0.24
3) Utilities Cost
Cooling water Negligible
Steam Negligible
Power 0.4
4) Shipping $ Packaging 1.15
Total 2.04
FIXED COST
₦ Million
1) Maintenance 1.21
2) Operating Labor 7.26
3) Laboratory Cost 2.18
4) Plant Overhead 3.63
5) Insurance 387.15
6) Royalties Not applicable
Total 401.43
Annual Total Operating Cost = 2.04 + 401.43 = ₦ 403.47

million
Annual Operating Cost Rounded = ₦ 403.5 million
ANNUAL PROFIT CALCULATION
Total Expenses = operating cost + capital finance cost

131
Total fixed capital investment = ₦ 5.15 billion
Working capital = ₦ 258 million
Total capital cost = ₦ 5.41 billion
(Assuming 5% compound interest rate annually and 2 years

investment)
Total interest = p (1 + r )n
= 5.41 (1 + 0.05)2
= ₦ 5.96 billion
Operating cost for 2 years = 2 × 0.403 = ₦ 806 million
Total Expenses = ₦ (0.806 + 5.96) billion
= ₦ 6.77 billion
Cost of Nitric acid per ton = ₦ 10500
Annual total cost of Nitric acid = 7100 × 400,000
= ₦ 4.2 billion
Total cost of Product for 2 years = ₦8.4 billion
Annual total cost of steam =
10500 kg 8000 hours ₦ 7.5

hour 1 year 454kg
132
Annual total cost of steam = ₦ 1.39 million
Total income before tax = ₦ (5.68 billion + 2 × 0.00139 billion)
= ₦ 8.4 billion
Total income after tax (based on 2.5% tax) = ₦ (8.4 – 0.025 × 8.4)
billion
= ₦ 8.19 billion
Profit after tax = ₦ (8.19 -6.77) billion = ₦1.42 billion
Payback period (no interest) = Depreciable FCI / Total profit
= 5.15 / 1.42 = 3.63 years
Therefore, payback period = 3years 8 months rounded.
BREAK EVEN ANALYSIS
On the assumption that market price of nitric acid will remain

constant for a reasonable length of time. The breakdown period
for the plant will simply be the inverse of the rate return on the
investment
Total capital investment

∴ Break even time (yrs) = annual net profit
5.41
¿ =3.81 yrs
1.42
Break even time= 3yrs 10 months.

133
RATE OF RETURN ON INVESTMENT
R O R = yearly profit / total initial investment × 100%
= 1.42/5.41 × 100/1 = 26.25%
CHAPTER TEN
134
STARTUP AND SHUTDOWN PROCEDURES
Shutdown is that period of time during which a boiler, gas

turbine, process heater or nitric acid production unit is allowed to
cool from its normal temperature range to a cold or ambient
temperature.
The shutdown philosophy is based on the nitric acid plant process

control and safeguarding philosophy reference and adapted to
suit the developments in the design. High nitric acid supply
availability is of paramount importance. The level of safeguarding
reflects the need for the plant to operate safely whilst ensuring
maximum availability.
Shutdowns of the main process will be avoided as much as

possible within the constraints of safer operation. Additional time
is given to the operator to correct process upsets by intentionally
accepting cascading events. This in turn will result in fewer
disruptions in the process
For all separators, low low liquid level will cause the
corresponding liquid outlet SDV (Shut down Valves) to close rather
than generating an OSD (Operational Shut Down)
 On high liquid level and high pressure in the main nitrous

gas stream, gas flow is stopped by closing the inlet
shutdown valves. This is to avoid liquid carry over to the
absorption column and stripper.
 Gas compressor unit.
135
 In the absorption column, a high liquid level and a high

pressure will close the corresponding inlet SOV.
 Trips in the off air compressor package will stop the
compressor and the air flow will be directed to the flare.
10.1 EMERGENCY SHUTDOWN (ESD) AND

EMERGENCY DEPRESSURIZATION (EDP)
Emergency Shutdown and Depressurization of pressurized vessels

and piping is the acknowledged way to reduce the likelihood of
escalation from accidental hydrocarbon release incidents.
An ESD will be automatically initiated on confirmed low

instrument air pressure and manually initiated on confirmed gas
detection via ESD push button. The aim of an ESD is to bring the
plant to a safe condition by;
1. Isolate the plant from the flow lines, stopping all

hydrocarbons containing streams from coming in and going
out of the plant.
2. Depressurization the plant.
3. Starting down the fired heaters
10.2 NOTIFICATION
Prior notification of scheduled shutdowns and scheduled start-ups
following scheduled shutdowns shall be made in a timely manner
and form. Shutdowns and start-ups must be scheduled in pairs
with scheduled dates for each. Notification of scheduled start-ups
and shutdowns is required only if an exemption from the
136
emissions limit is required. This notification shall contain the

following information:
1. Dates and times of the scheduled start-up and shutdown and
its duration, and
2. Any other process variable that is appropriate as
determined.
10.3 RECORD KEEPING

Records shall be maintained and kept on-site and made available
for two years indicating hour-by-hour firing rates, flue gas
temperatures, NOx emissions and such process variables that are
appropriate.
Once all of these equipment checks are performed, the complete
unit is disassembled, all parts and bearings are rechecked and
oiled, the lubrication system is drained and flushed, and the train
is re-assembled. A time-consuming aspect of the drive train
checkout involves plotting of the unit’s surge curves. Once the
unit is operational, the air compressor can be used to blow out
downstream air and stream lines.
Other equipment debugging procedures are performed according

to individual “punch lists” and are summarized as follows:
 Liquid piping and coded vessels: Pressure tested with

water at maximum working pressure.
 Gas lines: cannot be checked until plant is operating
 Relief valves: bench tested with required pressure—if
serious problems exist, they are sent out for repairs.
137
 Heat exchanger: flushed with water or a cleaning solution.

 Waste Heat Boiler: undergoes a hydrostatic check followed
by pre-treatment with chemicals to prevent corrosion due to
oxygen or water prior to plant start-up. A final procedure before
production starts consists of filling the boiler with water and
warming with steam to prevent shock to the system
 Absorber column: shipped to the plant as a complete
package and can be of either a bubble cap or sieve tray
arrangement. The column is prepared by flushing with water to
clean and check flow and level indicating instruments. Sieve
tray columns are more sensitive to gas versus liquid flow and
may require 1hr to seal properly whereas a bubble cap unit
may take about 20mins
 Instrumentation: Cannot be installed until all other
equipment is in place. A critical component is ammonia/air ratio
control system which must be accurately calibrated to read
concentrations of about 9-11 Percent ammonia in air.
10.4 STARTUP OPERATIONS
Once all equipment is installed and thoroughly checked for proper

mechanical operation (this may take from 2 to 6 months), the
plant is ready to undergo initiation of nitric acid production.
Preliminary startup operations consist of the following steps:
1. Startup of air compressor system
2. Initiation of water flow to absorber tower

138
3. Platinum gauze lit by hydrogen torch to initiate burning of

ammonia (flame is self-sustaining)
4. Ammonia flow is begun
Within 2 to 3 weeks of this initial startup, the plant is ready for a
test or demonstration run. Test runs usually last 3, 7, or 14 days
depending on the contract. During this time, the plant must
achieve its peak efficiency, of maximum design rate, and meet all
applicable emission regulations. A violation of any of these
conditions or other equipment mal-functions results in a cessation
of the test run. The conclusion of a successful test run results in
the “legal acceptance” of the plant from the contractor.
The best point in time to define plant startup is when the

ammonia flows to the converter is initiated. Barring no usual
problems, the completion of a successful test run and the
achievement of maximum production rate should be about one
month or less from this starting point. An important point with
respect to nitric acid facilities is that the summer months are the
most critical for proper operation due to cooling requirements for
the exothermic reaction involved. For this reason, most new
plants try to come online during the hotter periods when a
successful test run would be most meaningful. Because of the
requirement for performance testing within 180 days of startup, it
is conceivable that testing could be required during the cooler
months when a plant would find it easiest to meet applicable
emission limitations. In this instance, regulatory agencies might
want to conduct testing as soon after startup as possible, consider
139
postponement of tests until the following summer, or consider

winter testing and subsequent summer testing.
CHAPTER 11
CONCLUSION AND RECOMMENDATION
11.1 CONCLUSION
From the design procedures followed and results obtained, it can
be concluded that a plant can be set up to produce 400,000
tonnes of Nitric acid per annum from ammonia oxidation. The
excess steam generated in the process can be gathered and sold
to increase the total income to be realized from sale of products.
Also, the exhaust gases from the turbine is reduced to the lowest
minimum (<1000ppm). This is to reduce the NOx emission from
the plant which is in line with the Federal Environmental
Protection Agency (FEPA) regulations. The produced acid will be
sold mainly to fertilizer manufacturing plants and oil servicing
companies in Nigeria, and can be exported as well.
Finally, an economic evaluation of the plant showed that the rate
of return on investment is about 26.25% and the payback time is
about 3years and 7 months. Therefore the project can be said to
be economically feasible.
140
11.2 RECOMMENDATION
Additional control schemes should be put in place to ensure very
low nitrous oxide emission; this will contribute to the global
objective in reducing environmental degradation. There should be
considerations for a two stage air compression to supplement the
fluctuations in air requirement due to the anticipated increase in
the demand of nitric acid. There should be provisions for
preventive maintenance, as this will help to reduce frequent
shutdowns due to repairs. It is also anticipated that this plant will
be part of a larger chemical complex. Ammonia will be produced
by steam reforming of natural gas. The nitric acid plant will take a
portion of the ammonia product, and nitric acid and ammonia will
then be used to produce ammonium nitrate.
141
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Publishers, Sydney.
Aneke, L. E. 2009, Principles of chemical engineering process

design,
De-adroit innovation, Enugu.
Anon, A. 1979 ‘Nitric Acid rolls on’ Chemical Engineering 29

June, pp. 24-25.
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networks for heat exchangers by systematic methods’
Chemical Engineering, London 22 April, pp. 25-27.
Brown, K. J. 1989 Process integration initiative (review of the

process integration initiatives funded under the Energy
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Harwell Laboratory, Didcot United Kingdom, pp. 221-236.
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Rein hold, New York, pp.201-203.
Cheremisinoff, N. P. 2000, Chemical process equipment,

Butterworth Heineman, New Delhi.
Chilton T.H. ‘The manufacture of nitric acid by oxidation of

Ammonia : the Du pont pressure process’ Chemical Engineering
Progress, Monograph Series Vol. 56, AIChe, New York.
Coulson J. M. & Richardson J. F. 2004 Coulson & Richardson’s

Chemical engineering, 6th Ed. Vol. 1, Elseiver publishers
London.
Durilla, M. 2009, NOx and NO2 control in nitric acid plants,

Queens Publishing House, U.S.A.
Felder R. & Rousseau R. 2000, Elementary principles of

chemical processes, 3rd Ed. John Wiley & sons, New York.
Gregory T.C 1999, Uses and Applications of chemicals and

related materials, Reinhold Publishing, New York.
Harvin R.L, Leray D.G & Roudier L.R 1979, ‘Single pressure or
dual pressure nitric acid: an objective comparison’, Ammonia
Plant Safety, Vol. 21, pp.173-183, AIChe, New York.
143
Himmelblau, D. M. 2003, Basic principles and calculations in

chemical engineering, 6th Ed. Prentice Hall, India.
House, F. F. 1969 ‘Engineers guide to plant layout’ Chemical

Engineering, NY 76 July 28 p.120.
Kent J.A, 1983, Reigel’s Handbook of Industrial Chemistry, Van

Nostrand Ranhold Publishing, New York.
Kirk B.E & Othmer D.F (Eds) 1981, Encyclopedia of Chemical

Technology 3rd Ed. Vol.15 Wiley-Interscience, New York, pp.853-
871.
Linnhoff, B, Dunford, H & Smith, R 1983, Heat integration of

distillation columns into overall processes, Chem. Eng. Sc.,
38(8), pp. 1175-1188.
Martyn, S.R. & David, W. J. 1989, Chemical engineering design:

a case study approach, Bell and Bain Ltd, Glasgow.
Max, S.P, Klus, D. T. & Ronald, E.W 2003, Plant design and
economics for chemical engineers; 5th Ed., McGraw-Hill, New
York.
Ohrue T., Ohkubo K. & Imai O. 1999, Technological

improvements in strong nitric acid process, Vol. 21 pp.164-170,
AIChe, New York.
144
Perry R. H., Green D. W. & Maloney J. O 2008, Perry’s Chemical

Engineers’ Handbook, 8th Ed. McGraw-Hill, New York.
Sinnot, R.K 2005, Chemical engineering design, 4th Ed.,

Butterworth-Heinemann, London.
145
APPENDIX I
TABLES AND CHARTS
Table A.1: Conversion factors for some common SI units

146
Table A.2: Typical Overall Coefficient

147
Table A.3: Typical Design stress for Plates

148
Figure A.1: Temperature correction factor: for one Shell; two or

more even tube passes Heat exchange
APPENDIX II
MATERIAL BALANCE CALCULATION
Basis: 1hour
4000000tons HNO3 1 year

1 year 8000 hours
=50tonsHNO 3
solutions/hour
149
ABSORBER AND STRIPPER
3NO2+H2O ⇌ 2HNO3+NO
50tons HNO3 solution 0.6 tons HNO3

1 ton HNO3 solution
=30 tons HNO3 Produced
30 tons 3 tons 1 ton mole 46 tons NO2 100 tons

HNO3 moles NO2 HNO3 NO2 fed
2 ton moles 63 tons 1 ton mole 98 tons NO2
HNO3 HNO3 NO2 converted
=33.528 tons NO2 fed
1 ton mole NO 30 tonsHNO3 1 ton mole 30 tons NO

HNO3
2 ton moles 63 tons HNO3 1 ton mole NO
HNO3
= 7.143 tons NO Produced
OXIDISING UNIT
2NO+O2 ⇌ 2NO2
33.528 tons 1 ton mole O2 1 ton mole NO2 32 tons O2

NO2 fed
2 ton moles 46 tons NO2 1 ton mole O2
NO2
150
=11.662 tons O2 converted
11.662 tons O2 1 ton mole O2 2 tons moles 30 tons NO

NO
32 tons O2 1 ton mole O2 1 ton mole NO
=21.866 tons NO converted
11.662 tons O2 1 ton mole O2 2 tons moles 30 tons NO

NO fed fed
32 tons O2 1 ton mole O2 1 ton mole NO
fed fed
=21.866 tons NO fed
CONVERTER
4NH3+5O2 ⇌ 4NO+6H2O
23.197 tons 5 tons moles 1 ton mole NO 32 tons O2

NO O2 converted converted
4 tons moles 30 tons NO 1 ton mole O2
NO converted
=30.929 tons O2 converted
Quantity of O2 fed to the converted= (11.662+30.929) =42.591

tons O2 fed.
23.197 tons 4 tons moles 1 ton mole NO 17 tons NH3

NO NH3
4 tons moles 30 tons NO 1 ton mole
NO NH3
=13.145 tons NH3 converted.
151
13.145 tons NH3 1 ton NH3 fed

0.98 ton NH3 converted
=13.413 tons NH3 fed.
Quantity of NH3 leaving converter= (13.413-13.145) =0.268 tons

NH3.
23.197 tons 6 tons moles 1 ton mole NO 18 tons H2O

NO H2O
4 tons moles 30 tons NO 1 ton mole H2O
NO
=20.877 tons H2O Produced.
0.005 tons H2O 13.413 tons NH3

0.995 tons NH3
0.0679
Total Quantity of H2O leaving Converter= (20.877+0.0679) =

20.95 tons.
Make up H2O is added to ensure efficient chemosorption.
Quantity of makeup water= 7.059
Quantity of H2O fed to Absorber= (7.059+21.582) = 28.641 tons

of H2O.
30 tons HNO3 1 ton mole 1 ton mole H2O 18 tons H2O

HNO3
63 tons HNO3 2 tons moles 1 ton mole H2O
HNO3
=4.286 tons H2O Required.
=0.64 tons O2
152
O2 left to react=6.32 tons O2 {6.96 – 0.64}
Assume 50% conversion of NO
Amount of NO reacted = 0.5 × 8.6 =4.3tons NO
0.27 tons NH3 5 mols O2 1 mol NH3 32 tons O2

4 mols NH3 17 tons NH3 1 mol NH3
4.3 tons NO 1 mol O2 1 mol NO 32 tons O2

2 mol NO 30 tons NO 1 mol O2
=2.29tons O2 reacted
Amount of leaving stripper: 6.32 – 2.29 = 4.03 tons O2
Amount of NO left unreacted: 8.6 – 4.3 = 4.3 tons
=0.48 tons NO
Total amount of NO leaving stripper = 4.3 + 0.48 =4.78 tons NO
0.27ton NH3 6 mols H2O 1 mol NH3 18 tons H2O

4 mols NH3 17 tons NH3 1 mol H2O
153
=0.43 tons H2O

Total amount of water vapor leaving the stripper = 23.83
+ 0.43 -20 =4.26 tons
NB: Amount ofH2O in HNO3 solution =20 tons.
4.3 tons NO 2 mols NO2 1 mol NO 46 tons NO2

2 mols NO 30 tons NO 1 mol NO2
=6.59 tons NO2
Total NO2 leaving stripper =6.59 + 0.672 = 7.262 tons
NO2
COMBUSTION CHAMBER AND PURIFICATION REACTOR.

COMBUSTION CHAMBER
CH4 + 2O2 CO2 + 2H2O
2C2H6 + 7O2 4CO2 + 6H2O
2H2 + O2 2H2O
2NO + O2 2NO2
Assume 10 tonnes of natural gas supplied to combustion
chamber with composition in wt %
CH4:85.7, C2H6: 4.8, N2: 3.2, H2: 6.3
8.75 tons CH4 2 mols O2 1 mol CH4 32 tons O2
1 mol CH4 16 tons CH4 1 mol O2
=34.28 tons O2 required
8.57 tons CH4 1 mol CO2 1 mol CH4 44 tons CO2
1.02 1 mol CH4 16 tons CH4 1 mol CO2
=23.10 tons CO2
8.57 tons CH4 2 mols H2O 1 mol CH4 18 tons H2O
1.02 1 mol CH4 16 tons CH4 1 mol H2O
154
=18.9 tons H2O
0.48 tons 7 mols O2 1 mol C2H6 32 tons 02

C2H6
2 mols C2H6 30 tons C2H6 1 mol O2
=17.92 tons O2
0.48 tons 4 mols CO2 1 mol C2H6 44 tons CO2
C2H6
1.02 2 mols C2H6 30 tons C2H6 1 mol CO2
=1.38 tons CO2
0.48 tons 6 mols H2O 1 mol C2H6 18 tons H2O
C2H6
1.02 2 mols C2H6 30 tons C2H6 1 mol H2O
=0.847 tons H2O
0.3 tons H2 2 mols H2O 1 mol H2 18 tons H2O
2 mol H2 2 tons H2 1 mol H2O
2.7 tons H2O
N/B: Assume 50% conversion of H2, 90% conversion of
CH4 and C2H6,30% conversion of NO
Amount of CH4 leaving combustion chamber = 8.57(0.1)
= 0.857 tons
Amount of C2H6 leaving combustion chamber = 0.48(0.1)
=0.048 tons
APPENDIX III
ENERGY BALANCE CALCULATION
Unit 3: THE COMPRESSOR
Tin= 20°C Tout=155°C

155
T2
Heat, Q = n∆H = ∫ CpdT

T1
Components involved N2 an O2
Specific heat capacities;
N2 = 1.04 KJ/KgK and O2 = 0.6486 KJ/KgK
Enthalpy, H;
H1= 1.04(428 −293 ) = 140.4 KJ/Kg
H2 = 0.64886(428− 293) = 87.56KJ/Kg

H3 = 0.6486 (428 – 293) = 87. 56KJ/Kg
Q= Heat output from the Compressor;

Q = n∆H = ∑ nHOut −∑ nHIn
187030(140.4) + 49720 (87.56) −49720 (87.56)
Q = 2625901 KJ/hr
Let q = Volumetric flowrate of air
q = Fair// Dair
Fair = Flow rate of air, Dair = Density of air
q = 236750 Kg/m3/1.178Kg/m3 = 200976.23 m3/hr
Theoretical Power of the Compressor= P1Q1ln (P1/P2)
= 1 ×200976.23 ln (7.3/ 1) = 399515.49 KJ/hr
Theoretical power
Actual Shaft Work required = Efficiency
= 399515.49/ 0.84 = 475613.68KJ
Unit 5: AIR HEATER

156
Tin = 155°C T 0ut = 250°C

Enthalpy, H;
533
H1 and H3 = ∫ 0.9454+1.315 ×10 -4

T −5897.46 T-2
428
=
152.484KJ/Kg
H2 = 0.973504T + 1.76 ×10 -4
T2 −1187.2T-1
=
80.79 KJ/Kg
Heat Duty of the Air Heater, Q = n ∆ H = ∑ nHOut − ∑ HIn
Q = 187030(80.7782) + 49720(152.484) – 49720(152.484)

= 15107946.75 KJ/hr
Unit 8; THE CONVETER
Reactions involved in the Converter

4NH3 + 5O2 4NO + 6H2 ∆Hr = −907 KJ/K
Balance with reaction;
Q = ∆H = ξ∆Hr + ∑nOut HOut− ∑ninHin
ξ = extent of reaction
ξ= (270 − 13500)/ -4 = 3307.50 KJ/hr
Specific Heat capacity of NH3
Cp/R =( 3.578 + 3.020 ×10 -3
T + (-0.186 ×10 5
T-2)) ×
0.488
Calculating the enthalpies

H1 and H5 = 1.0142(1163 −523) = 615.58 KJ/Kg
H2 and H7 = 1.0838 (1163 – 523) = 693.632 KJ/Kg
157
1163
H4 = ∫ 1.7461+1.47376× 10 -3
T – 9076.8T2
523
=
3035.09 – 1132.10 = 1902.99 KJ/ Kg
1163
H6 = ∫ 0.9385+0.173 ×10 T + 387.94T-2)

-4
523
= 610.38 KJ /Kg
Heat outlet, Q = 3307.5(-907.3) + (270
427 (612.58)+160860 (693.632)+65(1305.98)

×1902.99+1160 ( 612.58 ) +21060 ( 1305.98 ) – ¿
Q = 20579273.85 KJ/hr
Unit 9; WASTE HEAT BOILER
Inlet Temperature = 890 ° C and Outlet Temperature=
250°C
Enthalpies of the compositions
0.9454+1.315 ×10
¿
T −5897.46 T-2)
523
H1 and H3 = -4
∫¿
1163
= 523.70 – 1193.50 = -669.8 KJ/Kg
H2 and H4 = =-719.25 KJ/Kg
H5 = -685.088 KJ/ Kg
Q= (1160 (-669.8) + 16080( -719.25) + 23320(-685.088) –

1160(-669.8) + 160860(-719.25)
158
Q = -15976252KJ/Kg
Temperature of Steam coming out from the Waste Heat

Boiler
Q = mCp (TST – TCW)
m= 1000Kg/hr
TCW=30°C, Cp = 4.2 KJ/hr
TST -30 = 15976252/1000 × 4.2
TSteam=410°C
Unit 13: STACK GAS HEATER
Tin = 200°C TOut =

150°C
H1 and H3 = 0.973504T + 8.8 ×10 -5

T2 −¿ 1187.2T
= -52.909 KJ/Kg
H2 and H 5 = Cp ∆ T = 1.31(-50) = -65.5KJ/Kg
H4= -50.906KJ/kg
Q = 160860(-52.909) + 1460(-50.906) + 33530(-65.5) –
160860(-52.909) + 335030(-65.5)
Q= -74322.76 KJ/Kg
¿
-74322.76 = 13565 ×2.15 ×¿ TST -30)
159
TSteam= 118.48
Unit 12: WASTE HEAT BOILER

Inlet Temperature = 150°C = 423K
Outlet Temperature = 50°C = 323K
Enthalpies, H
H1 and H3 = 0.97350T + 8.8 ×10 T – 1187.2T-1
-5
= -102.59 KJ/Kg
H2 and H5 = 131 KJ/Kg
Q = 160860(-104.734) + 1460(-102.59) + 33530(-131)
Q=-149781.4 KJ/hr
TSteam=103°C
AMMONIA VAPORIZER
Q + ƛ =13565 × 2.15(T +33.4)
ƛ=Latent heat of Steam= 1910.3
Q=149781.4
T = 15169.14/ (13565×2.15) -33.4= -28.199°C
AMMONIA SUPERHEATER
Q= -1596252KJ/hr, ƛ=3300
Q + ƛ = 13565×2.15(T + 28.2)
T = (1596252+3300)/ (13565×2.15) -28.2
T=26.65°C
160
APPPENDIX IV
EQUIPMENT DESIGN CALCULATION
STACK GAS HEATER
Q = 74322.76KJ/h, Th in =2000C, Th out = 1500C, Tc in = 300C,Tc out

=118.480C, U =0.102Kw/m2
Converting Q = 74322.76KJ/h to KJ/s
74322.76/3600 =20.6452KJ/h
Tm=( Th ¿−Tc out )−( Thout −Tc ¿ )

Th −Tcout
ln ⁡[ ¿ ]
Thout −Tc ¿
( 200−118.48 )−(150−30)
(200−118.48)
ln ⁡[ ]
(150−30)
81.52−120
81.52
ln
120
38.48
0.387
o
∆ T m=99.43 C
Q
A=
U ∆Tm
20.6452
0.102× 99.53
A = 2.03m 2
161
AMMONIA VAPORIZER
149781.4 KJ 149781.4
Q= ,∈ KJ / sec= =41.606 KJ /S
hr 3600
Tc ¿ =−33. 4 o C
out =¿−28.19 9o C
Tc ¿
Th¿ =208
(Th¿ −Tc out )−(Thout −Tc ¿ )

Thout =167.2 ∆ T m=
Th¿−Tc out
ln ⁡[ ]
Thout −Tc¿
(208+28.199)−(167.2+ 33.4)
208+28.199
ln ⁡[ ]
167.2+33.4
236.199−200.6
236.199
ln ⁡[ ]
200.6
35.599 35.599 o
= =218. 4 C
ln 1.177 0.163
U = 0.102KW/m2
Q 41.606
A= = =1.868 m2
U ∆ Tm 0.102 ×218.4
WASTE HEAT BOILER 1

162
(Th¿ −Tcout )−(Thout −Tc¿ )

∆ T m=
Th¿ −Tcout
ln ⁡[ ]
Thout −Tc ¿
(890−410)−(250−30) 480−220
=
890−410 480
ln ⁡[ ] ln
250−30 220
∆ Tm=333.76
Q 4437.8 4437.8
A= = = =130.73 m2
U ∆ Tm 0.102 ×333.76 34.04
WASTE HEAT BOILER 2

(208−150)−(50−32) 58−18 40
∆ Tm= = = =34.48
208−150 58 ln3.2
ln ⁡[ ] ln
50−32 18
Q
A=
U ∆ Tm
Q = 149781.4KJ/hr, converting to KJ/s
= 41.61KJ/S
41.61
=11.83 m2
0.102×34.48
NH3 SUPERHEATER.
163
(Th¿ −Tcout )−(Thout −Tc¿ )

∆ T m=
Th¿ −Tcout
ln ⁡[ ]
Thout −Tc ¿
( 410−26.65)−(330−28.2) 81.55
∆ Tm= = =340.9 5o C
410−26.65 ln 1.2702
ln ⁡[ ]
330−28.2
Q = 4437.85KJ/S.
U = 0.102KW/m2
4437.85
A= =127.6 m2
0.102 ×340.95
AIR HEATER
Q = 14881486.75KJ/hr = 4133.7KJ/S.
(350−250)−(200−155) 100−45 55 55
∆ Tm= = = = =68.8 4 o C
350−250 100 ln 2.22 0.799
ln ⁡[ ] ln ⁡( )
200−155 45
Q 4133.7
A= = =588.7 m2
U ∆ Tm 7.02
164
APPENDIX V
EQUIPMENT COSTING CALCULATION
IN 1998
A m2 0.6
Cost ∈ A m2=cost of 500 m2 ×( )
500 m2
IN 2013
2013 index
Cost ∈2013=cost∈1998 ×( )
1998 index
Index in 1998 = 390
Index in 2013 = 683.6
AMMONIA VAPORIZER
165
Cost of 500m2 = N1.84 million
A = 1.87m2
0.6
1.87
Cost ∈1998=N 1.84 million ×( ) =N 0.06 million
500
683.6
Cost ∈2013=N 0.06 million ×( )
390
N 0.11 million.
WASTE HEAT BOILER 1
IN 1998
2 2 A m 2 0.6
Cost ∈ A m =cost of 500 m ×( )
500 m 2
IN 2013
2013 index
Cost ∈2013=cost∈1998 ×( )
1998 index
Index in 1998 = 390
Index in 2013 = 683.6
WASTE HEATER BOILER 2
In 1998
11.8 0.6
Cost ∈ A m2=N 1.84 million ×( )
500
166
N 1.84 million ×(0.0236)0.6
N 1.84 million × 0.106

cost of A m2=
N 0.19 million
In 2013
683.6
cost of 2013=N 0.19 million × =N 0.33 million
390
AMMONIA SUPERHEATER
A = 128m2
Cost in 1998
2 128 0.6
Cost of 128 m =N 1.84 million ×( ) =N 0.8214 million
500
Cost in 2013
683.6
390
WASTE HEAT BOILER 1
A = 130.5m2
In 1998
2 0.6
Am
Cost ∈ A m2=cost of 500 m2 ×( 2
)
500 m
0.6
130.5
Cost of 130.5 m2=N 1.84 million ×( ) =N 0.8219 mi llion
500
683.6
390
FOR AIR HEATER

167
IN 1998
2 2 A m 2 0.6
Cost ∈ A m =cost of 500 m ×( )
500 m 2
IN 2013
2013 index
Cost ∈2013=cost∈1998 ×( )
1998 index
Index in 1998 = 390
Index in 2013 = 683.6
588.7 0.6
Cost of A m2=N 1.84 million ×( ) =N 2.1 million
500
683.6
390
STACK GAS HEATER
1998
2.03 0.6
Cost ∈ A m2=N 1.84 million ×( ) =0.068 million
500
683.6
390
CONVERTER
Cost index 2013 = 680.1
Cost index 1990 = 390

168
Volume = 600 gallon
Cost for 600 gallon in 1990 = 17000

0.6
1000000
Cost of 1 million gallon∈1990=17000 ×( ) =$ 1.457 million
600
680
Cost ∈2013=$ 1.457( )=$ 2.541million
390
COMPRESSOR
In 1990
cap 1
( )
Cost of eq1 = cost of eq2 cap 2
0.6
7294
×( )
Cost of eq1 = $2100 447.8
0.6
Cost of eq1 = $ 11203.4

cost index 2013
Cost in 2013 = cost in 1990 ×( cost index 1990 )
928.1
cost in 2013 = 11203.4 ( 756.3 )
=$ 13748.4
= # 2.2 million
Cost for nitric acid storage tank
Given volume of the tank at 1990 = 12 × 1606 gallons
Cost at 1990 = $170000
Cost index at 2013 = 683.6
Cost index at 1990 =395

169
Volume of storage tank =28.3m3 to liters =23800l
For 5000 gallons

5000
( )
Cost at 1990 = 170000 12 ×10
6 0.6
1637.96 = $2830.56
= #447228
683.6
¿
Cost in 2013 = 1593.39( 395
= $2830.56
= N447228.00
For year 2006

capacity of equipment 1
( )
Cost of equipment 1 = cost of equipment 2 capacity of equipment 2
For year 2006

cost∈2006 CPE ∈2006
cost∈2013 = CPE ∈2013
RATIO METHOD
Cost of designed plant = cost of previous plant

capacity of designed plant
( ) n
capacity of previous plant
1200
( )
Cost of 1200tons per day =cost of 280 per day 280
0.6
= $60 million ( 1200

280 )
0.6
= $144 million
170
=#23 billion
STEP COUNTING METHOD
C = 14000 N Q0.615
N = 13(number of functional units)
Q = 400000 tons/yr (capacity of plant)
C = 14000 ×13 ×(400000) 0.615

= $507 million
= # 79.8 billion

Design Project On Nitric Acid Production

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Design Project On Nitric Acid Production

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1

PLANT DESIGN FOR THE PRODUCTION OF

400,000 METRIC TONNES OF NITRIC ACID

PER ANNUM FROM AIR OXIDATION OF

FEDERAL UNIVERSITY OF TECHNOLOGY,

This report describes the detailed design of a plant to produce

estimated capital investment is ₦5.41 billion. The rate of return

2.3 Emission and

3.0 Material balance ------------------------------------------------------42

3.1 Conservation of mass -----------------------------------------------42

3.2 Methods of material balancing -----------------------------------43

3.3 Materials balance assumptions-----------------------------------44

3.4 Summary of material balance calculations-------------------44

3.5 Material balance for each unit------------------------------------44

6.0 Equipment design and specification ---------------------------66

6.1 Problem specification------------------------------------------------67

6.2 Analyzing the problem solution----------------------------------68

6.6 Summary of design and equipment specification

7.0 Process control and instrumentation----------------------------73

7.2 Plant control instrumentation-------------------------------------74

7.3 Alarms and safety trips --------------------------------------------77

7.4 Lining, piping, valves and pumps -------------------------------78

7.5 Pipe support------------------------------------------------------------81

8.0 Safety and environmental

8.2 Hazard and Operability (HAZOP)

8.3 Environmental impact

9.2 Economic Consideration--------------------------------------------103

9.6 Economic analyses calculation-----------------------------------108

10.0 Start up and shut down procedure----------------------------113

10.1 Emergency shut down and emergency depressurization

10.3 Record keeping -----------------------------------------------------115

10.4 Startup operation---------------------------------------------------116

1.1 BACKGROUND INFORMATION

Nitric acid is a strong acid and a powerful oxidizing agent with

Nitric acid is now produced commercially using the stepwise,

The traditional methods are:

(a) Extractive distillation with dehydrating agents such as

(b) Reaction with additional nitrogen oxides.

The latter technique has the greatest application in industry.

The chemistry of ammonia oxidation is remarkably simple with

1.1.1 PROPERTIES AND USES

Nitric acid is an oxidizing mineral acid with physical and chemical

aluminum. A compilation of many of the physical and chemical

Nitric acid has enormously diverse applications in the chemical

Nitric acid has a number of other industrial applications. It is used

An important point is that for most uses concerned with chemical

chemical grade is to be produced, additional process equipment

There is a potential health hazard when handling, and operating

1.2 DESIGN JUSTIFICATION

At present, there is no Nitric acid plant in Nigeria. The little Nitric

1.3 DESIGN OBJECTIVES

 To design a plant that will deliver 400000 metric tonnes of

2.1 HISTORY OF NITRIC ACID PRODUCTION

In 1903 the electric-arc furnace superseded this primitive original

Gregory (1999, p.40) argues that ‘Although the process benefitted

According to Ray (1989, p.8) Researchers returned to the

acid. This achievement began the search for an economic process

By 1908 the first commercial facility for production of nitric acid,

During World War 1, the intense demand for explosives and

Many new plants were constructed, all of which employed the

(a) The development of chrome-steel alloys for tower

(b) The improved design of feed preheaters enabled higher

(c) Early developments in automatic process control improved