ADAMSON UNIVERSITY

Ermita, Manila

College of Engineering
Chemical Engineering Department

Laboratory Report # 4: Production of

Nitric Acid

Process Dynamics and Control Lab

Submitted by:

Vanessa Denise C. Aguilar

Kathrine Faye M. Aquino

Cedric Q. De Guzman

Monique Rae G. Lugartos

Hannah T. Rapanan

Submitted to:

Engr. Rugi Rubi

March 15, 2017

Introduction

Under the Dual Pressure process, liquid Ammonia (NH3) entering the plant is
vaporized in ammonia vaporizer I E-101 and ammonia vaporizer II E-102 by
circulating chilled water and warmed cooling water from cooler condenser. Water
and oil accumulated in evaporator E-101 and E-102 are discharged into ammonia
stripper E-103 when required. The remaining ammonia stripped by steam heating
batch wise. The residual solution, consisting of water, oil and ammonia,, should be
passed to a neutralization unit. Gaseous ammonia is fed back to the ammonia
evaporator E-102. Finally, vaporized ammonia is superheated with steam in
preheater E-104. The ammonia vapor is filtered in ammonia filter F-101 before
reaching ammonia air in mixer M-101.

Atmospheric air is filtered in air intake filter F-102 and compressed by air
compressor C-101 to approximately 0.46 MPa absolute. During cold season, if
necessary, atmospheric air is mixed with the ventilation air of the compressor house
prior to filtration F-102.

The compressed air i split into two stream. One is the primary air is fed to
ammonia air mixer M-101 and mixed with ammonia gas from E-104. Secondary air
flow to bleaching tower T-102.

Air and ammonia gas flow rates are monitored, and the proper mixture is
obtained by ratio control. The mixed gas stream is filtered in mixed-gas filter F-103
and enters burner R-101/R-102, where the ammonia oxidation reaction takes place
on platinum-rhodium catalyst gauzes.

The NO gas, heated to 890 degree Celsius from burner R101-R-102 passes
through the waste, heat recovery train, which consist of the following units: La
Mont-type forced circulation waste - heat boiler (evaporator and super heater coils)
E-105, tail-gas heater IV E-113, economizer E-106, tail-gas heater III E-112, and feed
water preheaters E-114A and E-114B.

In waste-hat boiler E-105, reaction heat is used to generate superheated

steam for steam turbine Y-101 and other plant users.
 Boiler feed water required for the system is fully thermally degassed. The
undegassed water is fed to tank D-102 and delivered by pumps P-106A and P-106B
via feed water heaters E-114A and E-114B to feed water tank D-106 with degasser
D-106. Feed water tank D-106 functions as a suction vessel for boiler feed water
pumps P-104A and P-104B, which deliver boiler feed via economizer E-106 into
steam drum D-105.

The mixture of steam and water in the evaporator section for the waste-heat
boiler is forced into circulation by pumps P-103A and P-103B. Separation of
saturated steam and water takes place in team drum D-105. Saturated steam laves
the steam drum and is superheated in the superheater coils of waste heat boiler E-
105.

The cooled NO gas, after passing feed water preheater E-114A and E-114B, is
partly oxidized to nitrogen dioxide and enters cooler condenser I E-107.

In cooler condenser I E-107, water formed during ammonia combustion is

condensed as a weak acid of approximately 40 weight percent concentration.

The NO gas from cooler condenser I E-107 is fed into cooler condenser II E-
108, where it is cooled down again. After entering mist separator D-108, the NO gas
is combined with secondary air from bleaching tower T-102 and compressed by NO
compressor C-102 to approximately 1.08 MPa absolute.

The compressed NO gas is cooled in tail-gas pre-heater II E-111 and cooler

condenser III E-109. The acid condensate from cooler condenser I E-109, is pumped
into the sieve tray of absorption tower T-101 having the corresponding
concentration. The cooled NO gas from cooler condenser III E-109 enters the
absorption tower at the lower part of the oxidation section, where the complete
oxidation of the NO gas and the absorption of NO2 in water takes place on sieve
trays. Water-cooled oils for selected sieve trays removed the heats of reaction and
absorption.

Process water is pumped to the top of the absorption tower T-101. That water
can be cooled steam condensate, demineralized water, or process condensate from
AN (ammonium Nitrate) plant.
 The raw acid is bleached in bleaching tower T-102 in contact with secondary
air. The operating pressure for the bleaching system is approximately 0.45 MPa
absolute. The acid finally produced is transferred to and stored in a nitric storage
tank.

The tail-gas leaving absorption tower T-101 contained less than 200 ppm NOx
that has not been absorbed. The tail-gas is lead through tail-gas preheater I E-110
and tail gas preheater II E-111, where is it heated first in contact with secondary air
and afterwards with NO gas from NO compressor C-102. Finally the tail-gas is
heated in tail-gas heaters III E-112 and IV E-113 by NO gas from waste-heat boiler E-
105 to the designed temperature for the tail-gas expander Y-102, which is the prime
mover of the compressor set (air compressor C-101 and NO compressor C-102) the
exhaust tail gas is discharged to the atmosphere through a stack.

Steam turbine Y=101 supplies the rest of the power that is necessary to drive
the main compressor set. The steam is generated in waste-heat boiler E-105 by the
recovery of heat from the reaction gas. Steam produced in excess of steam turbine
T-101's needs is fed to the plant user.

Lastly, the commercial yield of the dual-process produces an overall yield of

96% per metric ton of 100% HNO3.

While for High Pressure Process, anhydrous NH 3 is evaporated continuously

and uniformly in an evaporator, using steam to supply the necessary heat of
evaporation. Air for reaction is compressed in a power-recovery compressor and in a
steam driven compressor to 110 psig and passed through heat exchanger and air
filler. NH3 gas is oxidized with air to NO at a pressure of 105 psig in a converter by
passing through platinum 10% rhodium gauze at 907C. Then NO with the excess
air necessary for the succeeding oxidizing steps is cooled in a waste-heat boiler
(W.H.B) and a waste cooler and conducted at the bottom of the absorber.
Successive oxidation and hydrations of the NO are carried out with continuous water
cooling in the absorbing unit. The aid (60% to 65% HNO 3) is drawn off through an
acid trap. The waste gas and expanded through a compressor for part of the air,
before being exhausted to atmosphere.
 In high-pressure nitric acid plant, the ammonia oxidation reaction is
maintained at 900-930C. With air and ammonia supply, temperature held constant,
the gauze temperature is adjusted by the slight changes in the proportion of
ammonia to air. Since the explosive limit of ammonia is approached at the
concentrations greater than 12% plant operation normally is obtained at 9.5-10.5
mol%. For high pressure plant, therefore a preheat temperature of 225-275C is
required.

The higher operating temperature and the higher mass velocities that
normally are used in high pressure plants lead to appreciably greater losses of
catalyst gauze.

Nitric acid is formed when nitrogen dioxide dissolves in water and releasing
nitric oxide.

Weak nitric acid is produced coming from the condenser, as soon as by

product water from the ammonia oxidation undergoes condensation and absorbs a
portion of the nitrogen dioxide. Nitric oxide at 95% efficiency at 930C from the
oxidation of ammonia.

On the other hand, the by-products of the process are the following:

Nitric oxide ammonia is oxidized by air on the surface of solid catalyst such
as platinum will gauze or furic oxide at a temperature of about 650-700C.
Nitrogen Pentoxide most of the nitrogen being oxidized to nitric acid which
upon cooling with more oxygen to form pentoxide.
Nitrogen Dioxide the nitric oxide is oxidized to nitrogen dioxide with
secondary air. The nitric oxide (nitrogen monoxide) produced reacts faster
with atmospheric oxygen to give nitrogen dioxide.

Objectives

1. To increase the efficiency of nitric acid manufacturing with the super heater
2. To yield a homogeneous product with the use of the mixer
3. To produce nitric acid from ammonia with lesser equipment and cost
Diagrams

Legend: A Alarm
TR Temperature Recorder
TC Temperature Controller

Legend: FRC Flow Recorder

Controller
Discussion

Over-all Control

Ammonia, which is the raw material in the production of Nitric Acid is being stored

in a 3-month tank and will be supplied to a daily tank. From this tank, 20% by uz.

Ammonia will enter on the shell side of the vaporizer. Temperature recorder (TR) will

send a signal to Temperature Control (TC) if the desired temperature is not met,

sending a signal to the valve, either to increase or decrease the flow of the

vaporizing medium. The vaporized ammonia and the unvaporized liquid enters the

and the thick liquor tank where the complete separation of vapor and liquid occurs.

The liquid remains in the tank while the NH 3 vapor enters the superheater.

Temperature recorder will send a signal to temperature controller if the desired

temperature is not met, sending a signal to the valve, either to increase or decrease

the flow of the superheating medium. If too much heat is recorded, there will be an

emergency alarm, sending signal to close the valves (superheating medium,

superheater) and to open the valve where the ammonia vapor will flow, bypassing

the superheater. When the temperature decreases and the alarm will stop, the

valves (superheating superheater) will open and the valve in the bypass will close.

Compressed air enters the mixer depending on its exit on the superheater. The flow

rate of the air is being controlled by tbe Flow Rate Recorder and Controller,

maintaining the ratio of the entering gas (1:15; NH 3; air) or ammonia should have at

least 14-16% by weight in the mixture. The mixture of the NH 3 and air enters the

burner where oxidation of NH3 to NO and N2 takes place while maintaining the

temperature. The temperature recorder sends signal to the Temperature controller

in case the desired temperature is not met, sending signal to the flow rate controller

(FRC) whether to increase or decrease the opening of the pipe where the steam
from the economizer enters. This steam serves as the cooling medium of the waste

heat boiler. Gases (NO, N 2, H20, O2) enters to the series of heat exchangers (tail gas

heater, economizer, feed water preheater, cooler, condenser) where the

temperature is being controlled. In case, the desired temperature is not met, the

Temperature controller sends signal to the flow rate controller (FRC) either to

increase or decrease the opening of the valve connected to it. In the case of feed

water preheater, cooler, and condenser, the cooling medium is water entering at

25C and coming from water basin. And for tail gas heater 1, 2 and 3, the tail gases

coming from the absorber serves as the cooling medium since these gases leave

the absorber at a lower temperature (90F). Gases enter the absorber together with

the weak acid formed in the condenser. The absorbers pressure is controlled by the

Pressure Recorder Controller (PRC) and in a sudden increase of pressure, PRC will

send a signal, opening the valve that will allow the increase of flow rate of Nitric

Acid formed to the Nitric Acid storage tank. Liquid level indicator (LLI) monitors the

level in the absorber (HNO3, H20 now formed) sending a signal to the LLC which the

LLC controls the flow rate (FRC) of the processed water entering the absorber. Nitric

Acid with 95.65% by weight leaves the absorber and enters the HNO 3 storage tank.

Conclusion and Recommendation

Both of the unit operations presented, the superheater and mixer, have
significant impacts on the yield of nitric acid from ammonia economically and
efficiently speaking. The temperature controller in the superheater will have a big
influence on the manufacturing process where the temperature recorder will signal
whether the desired temperature is being met. In addition, the flow recorder
controller in the mixer will dictate the consistency of the product. With the critical
roles of the super heater and mixer it is suggested that this unit operations should
be constantly managed and developed for better nitric acid production in a way that
it can be sufficient enough to reduce the cost and equipment in the plant.