Ind. Eng. Chem. Res.

2009, 48, 2705–2712 2705

Equilibrium and Kinetic Studies of in Situ Generation of Ammonia from Urea in

a Batch Reactor for Flue Gas Conditioning of Thermal Power Plants
J. N. Sahu, A. V. Patwardhan, and B. C. Meikap*
Department of Chemical Engineering, Indian Institute of Technology (IIT), Kharagpur, P.O. Kharagpur
Technology, West Bengal, 721302, India

Ammonia has long been known to be useful in the treatment of flue/tail/stack gases from industrial furnaces,
incinerators, and electric power generation industries. In this study, urea hydrolysis for production of ammonia,
in different application areas that require safe use of ammonia at in situ condition, was investigated in a batch
reactor. The equilibrium and kinetic study of urea hydrolysis was done in a batch reactor at reaction pressure
to investigate the effect of reaction temperature, initial feed concentration, and time on ammonia production.
This study reveals that conversion increases exponentially with an increase in temperature but with increases
in initial feed concentration of urea the conversion decreases marginally. Further, the effect of time on
conversion has also been studied; it was found that conversion increases with increase in time. Using collision
theory, the temperature dependency of forward rate constant developed from which activation energy of the
reaction and the frequency factor has been calculated. The activation energy and frequency factor of urea
hydrolysis reaction at atmospheric pressure was found to be 73.6 kJ/mol and 2.89 × 107 min-1, respectively.

1. Introduction But, unfortunately, ammonia presents significant danger to

Ammonia is a colorless gas with a pungent, suffocating odor.
Ammonia is corrosive and exposure will result in a chemical-
type burn. Since ammonia is extremely hygroscopic, it readily
migrates to moist areas of the body such as eyes, nose, throat,
and moist skin areas. Exposure to liquid ammonia will also result
in frostbite since its temperature at atmospheric pressure is 2.2
°C. Specifically, upon sudden release to the atmosphere, as might
occur in a train wreck or a traffic accident, the ammonia forms
a cloud of aerosol fog of liquid ammonia droplets. Unlike
gaseous ammonia, which, though toxic, is lighter than air and
quickly dissipates to harmless concentrations, the cloud can
persist for a while before it disappears. The cloud is typically
heavier than air and tends to drift along the surface of the earth,
i.e., the ground or the surface of a body of water. The cloud
moves with the wind and can sweep over a total area, i.e., a
“footprint”, much larger than the area covered by the cloud at
any one moment. Contact with the cloud is instantly incapacitat-
ing, and a single breath can be fatal.1
The Occupational Safety and Health Administration (OSHA)
issues permissible exposure limits for ammonia of 50 ppm, or
35 mg/m3, time-weighted average, and 35 ppm, or 27 mg/m3,
short-term exposure, and also ammonia is a highly hazardous
chemical under the Process Safety Management Standard.2,3
Many industrial plants require the supply of large quantities
of ammonia, which frequently must be transported through and
stored in populated areas. Important users among these are
industrial furnaces, incinerators, and electric power generation
industries.4 All of these are faced with a lowering of the amount
of nitrogen oxides being discharged to the atmosphere in the
combustion gases being emitted from their operations, as
required by environmental regulations.5 Another important use
is for the so-called “conditioning” of flue gas by which an
improved collection and removal of particles matter (fly ash) is
obtained. 6,7
human health as a hazardous chemical. Its transportation,
storage, and handling triggers serious safety and environmental
regulatory requirements for risk management plans, accident
prevention programs, emergency response plans, and release
analysis. An alternative approach to ammonia supply suggested
in the late 1980s includes using urea feedstock to generate
ammonia on site.8 The method of urea to ammonia conversion
is by hydrolysis process; urea is an ideal candidate for the
manufacture of ammonia.4 Urea is an environmentally safe
material used primarily as fertilizer. Urea is a nontoxic chemical
compound and presents essentially no danger to the environ-
ment, animals, plants life, and human beings. It is solid under
ambient temperatures and pressures. Consequently, urea can be
safely and inexpensively shipped in bulk and stored for long
periods of time until it is converted into ammonia. It will not
leak, explode, be a source of toxic fumes, require pressurization,
increase insurance premiums, require extensive safety programs,
or be a concern to the plant, community, and individuals who
may be aware of the transportation and/or storage dangers of
ammonia. It has been determined that using urea thermal
hydrolysis is the preferred process for converting urea/water
solution into a gaseous mixture containing ammonia, carbon
dioxide, and water vapor.9
The published information in the literature about hydrolysis
of urea for production of ammonia is very little detailed and is
patented.4,5,8-14 However, there is no information available in
the literature regarding the equilibrium and kinetic study of urea
hydrolysis for production of ammonia in a batch reactor, and
also in our early study in semibatch reactor at atmospheric
pressure it shows very slow rate of reaction.15,16 Therefore, we
decided to study more thoroughly the phenomenon of urea
hydrolysis for production of ammonia in situ in a batch reactor
for different applications.
2. Method of Experiment

* Corresponding author. Tel.: +91 3222 283958(O)/2283959 (R). 2.1. Process. The schematic of experimental setup is shown
Fax: +91-3222-282250. E-mail: bcmeikap@che.iitkgp.ernet.in, in Figure 1 and a photographic view is shown in Figure 2. The
bcmeikap@iitkgp.ac.in. experimental setup mainly consists of a high-pressure (100 kg/
10.1021/ie801286h CCC: $40.75  2009 American Chemical Society
Published on Web 02/09/2009
2706 Ind. Eng. Chem. Res., Vol. 48, No. 5, 2009
Figure 1. Schematic of the experimental setup for urea hydrolysis.
Figure 2. Photograph of the experimental setup of a high-pressure reactor.
cm2) reactor, heat exchanger, condenser, metering pump, feed
tank, control panel, and product storage tank. The reactor is of
2000 mL capacity and is made of stainless steel-316 to prevent
corrosion. A metering pump was used to feed the urea solution
to the reactor at high pressure at controlled flow rate against a
positive differential head between pump suction and discharge.
The shell and tube type condenser was used to exchange heat
between the products (NH3, CO2, H2O(V)) and cooling water.
The system has a heat exchanger to cool the unreacted urea for
recycle to the reactor where tap water at room temperature
without any pressure is used for cooling purpose. Apart from
above, it also has two storage vessels, one for urea solution
and another for product storage. The reactor has two openings:
one is for feeding urea solution and the other for withdrawing
the product to condense the gaseous product from the reactor
where tap water is used for the purpose of condensation. To
measure the temperature and pressure of the reactor, a thermo-
couple and pressure gauge were attached to the reactor through
the control panel. Cooling coil was placed inside the reactor to
cool the reactor when required; tap water was used here also as
a coolant. There is a control panel to control the required
temperature and speed of the stirrer. To supply the necessary
heat, electrical heating by coil outside the reactor wall was
provided at a controlled rate by means of control panel. The
control panel consists of several controllers and instruments.
The control panel consists of indicators that are connected by
electrical wire, mains on/off switch, stirring motor on/off switch
with variable speed inverter drive and speed indicator, electrical
heater on/off switch, alarm system, fuses, and PID temperature
controller. The whole setup is placed on a stand with moving
arrangement.
2.2. Experimental Technique. IFFCO make urea sample
was used to conduct the experiment which has been collected
from market. First, urea solutions of different concentration (10,
20, 30, and 40 wt %) were prepared. In each case the volume
of water was taken as 450 mL. Then the solution of particular
concentration was fed into the feed tank. A metering pump was
used to feed the urea solution to the reactor at high pressure at
controlled flow rate against a positive differential between pump
suction and discharge. The experiments are conducted without
stirrer. Heat was supplied by heating electrical coil outside of
reactor wall at a controlled rate by means of the control panel.
The decomposition of urea takes place slowly starting around
at 110 °C. As the reaction starts, the product, which is a gaseous
mixture of ammonia, carbon dioxide, and water vapor, goes
through the condenser. In the condenser the gaseous product
mixture gets condensed where tap water at room temperature
without any pressure was circulated through the condenser. Then
the product was stored in the product storage tank and was
collected in a beaker with boric acid solution as it is an absorbing
material for ammonia solution. Boric acid solution is prepared
by dissolving 4 g of boric acid in 100 mL of warm distilled
water. Then the absorbing ammonia solution was taken out and
its volume was measured. After it gets absorbed with boric acid,
three samples each of 10 mL volume were taken for titration.
Three drops of methyl orange indicator is mixed in each sample.
Then it is titrated with hydrochloric acid. Boric acid is so weak
that it does not interfere with acidimetric titration. Then by
comparing the initial concentration and final concentration the
equilibrium conversion was found out. Finally, the rate of
reaction was found out from the slope of the line in the graph
which was plotted between time versus concentration data. A
graph was plotted between ln(CA) and ln(rA). The slope and
intercept give the values of order of the reaction and rate
constant, respectively.
2.3. Characterization of Urea. Urea and biuret were
detected and quantified using HPLC (high performance liquid
chromatography).The HPLC equipment consisting of a Perki-
nElmer chromatograph series 200 UV/vis LC detector (Perki-
nElmer, USA) equipped with an isocratic pump series 200 and
 Ind. Eng. Chem. Res., Vol. 48, No. 5, 2009 2707
a rheodyne injector with a 20 µL loop with variable-wavelength
ultraviolet /visible detector was used. The equipment was
controlled by Total chrome software that controlled the solvent
gradient, data acquisition, and data processing. The column was
a reversed-phase Agilent column. Separation was in a C-18
column (250 mm × 4.6 mm dia.), 5 µm pore size, and a UV
detector set at a wavelength of 199 nm. The mobile phase used
here 0.1 M phosphate buffer pH 6.7 at flow rate 1 mL/min, and
the column temperature was 25 ( 1 °C. HPLC provides the
following features: high resolving power, speedy separation,
continuous monitoring of the column effluent, accurate quantita-
tive measurement, repetitive and reproducible analysis using the
same column, and automation of the analytical procedure and
data handling.
2.4. Reagents. All the chemicals used in the study were from
Merck (India) Ltd. and Qualigens Glaxo (India) Ltd. analytical
grade.

3. Results and Discussion

3.1. Reaction Pathway. The basic chemistry employed in
the hydrolysis of urea is a reverse of that employed in the
industrial production of urea from ammonia and carbon dioxide
and employs two reaction steps, as follows:17
NH2CONH2 + H2O f NH2COONH4 (1)

NH2COONH4 f 2NH3 + CO2 (2)

The reaction in eq 1 where urea hydrolyzes to form am- Figure 3. HPLC analysis of the urea feed solution.
monium carbamate is mildly exothermic, while eq 2, in which
ammonia and carbon dioxide are produced, is strongly endo-
thermic, with the result that the reaction to release ammonia
and carbon dioxide requires heat and quickly stops when the
supply of heat is withdrawn. Excess water promotes the
hydrolysis reaction, the overall reaction for which is as follows:
xH2O + NH2CONH2 f 2NH3 + CO2 + (x - 1)H2O (3)

3.2. Physical and Chemical Characterization of the

Urea Samples. IFFCO make urea samples were collected from
near the local market in Kharagpur, India. It is a common
nitrogen fertilizer used by Indian farmers. The physical appear-
ance is of granular structure, white in color, and it is highly
soluble in water. The pH of the urea solution of 10 wt % urea
to water was 7.84. The urea sample was characterized to the
known purity before conducting the experiment. Urea samples
were characterized by HPLC to find out the impurities. The
HPLC analysis of the feed urea sample is shown in Figure 3.
The chromatographs show the presence of urea and biuret in
the inlet feed solution of urea. It has been observed that IFFCO
urea contains 2.05% biuret and its purity is 91.21.
3. 3. Study of Equilibrium Conversion. Experiment was
conducted for hydrolysis of urea at high pressures in a batch
reactor at different temperatures, pressures, and concentrations;
both equilibrium and kinetic studies were done. From the initial
concentration and final concentration, the conversion was found
out and the equilibrium study of hydrolysis reaction without
stirring was studied. Here the effect of equilibrium conversion
on temperatures, pressures, and concentrations was studied.
Effect of Temperatures on Conversion. It can be seen from Figure 4. Effect of temperature on conversion at different concentrations.
Figure 4 that the conversion is a function of temperature. It
increases exponentially with increase in temperature. For 10%
urea solution, the conversion increases from 3% to 30% when solution and the conversions are 27, 25, and 23%, respectively,
temperature increases from 110 to 160 °C in 10 °C intervals. at 160 °C. It was observed that the initially conversion is slower
Similar trend has been observed for 20, 30, and 40% feed at lower temperature and it becomes rapid at around 130 °C.
2708 Ind. Eng. Chem. Res., Vol. 48, No. 5, 2009

Figure 6. Temperature evolution of reactor products for initial feed

concentration of 40 wt % urea to water.

Figure 5. Effect of initial feed concentration on conversion at different

temperatures.

At this temperature the production of ammonia is higher than

that at lower temperature.
Effect of Initial Concentration on Conversion. The conver-
sion was slightly affected by the initial concentration of urea
that is feed to the reactor. It can be seen from Figure 5 that
with increases in initial concentration of urea the conversion
decreases marginally. For each initial concentration the tem-
perature was varied from 110 to 160 °C. Keeping temperature
constant at 160 °C, the conversion decreases from 30% to 23%
when concentration varies from 10% to 40%. Similarly for 120,
130, 140, and 150 °C the equilibrium conversion decreases from
7% to 2.5%, 9% to 4%, 11% to 7%, and 20% to 11%,
respectively, when the initial concentration of urea increases
from 10% to 40%. This is due to the fact that higher weight %
of urea possesses less pressure in comparison to the lower weight
% urea solution as shown in Figure 8. Hence, during the
decomposition the solution, this has less urea content and will
give more ammonia, carbon dioxide, and water vapor as Figure 7. Effect of temperature on reaction pressure at different concentrations.
products from the reactor.
3.4. Vapor-Liquid equilibrium. The operating temperature
and pressure of the reaction of the reaction vessel along with 900 kPa and 100 to 950 kPa with temperature increases from
the excess water added (over the stoichiometric amount needed 110 to 160 °C, when 10 and 40 wt % urea solution, respectively,
to hydrolyze urea) will determine the concentration of water in is feed to the reactor. The benefits of operating at a pressure
the mixture at equilibrium. The gas discharging from the reactor uniquely related to the operating temperature for a specified
will leave saturated with water vapor. Figure 6 depicts the concentration of aqueous urea feed can be seen from Figures 7
measured concentration of product composition (moles of and 8. From Figure 8 we can seen that with increase in reaction
product/total moles of products) obtained from the reactor with pressure the conversion increases from 2.5 to 22.5% and 4 to
40 wt % of urea to water feed inlet solution at different 30% with increase pressure from 50 to 900 kPa and 100 to 950
temperatures. It can be seen from the figure that the production kPa, respectively, when at 10 and 40 wt % urea solution,
of ammonia and carbon dioxide increases markedly as the respectively, is feed to the reactor.
temperature increased and the production of excess water At an operating temperature of 110-160 °C and operating
decreased. pressure in the 50-950 kPa range, the concentrations of
Figure 7 depicts the measured reaction pressure of the urea ammonia and carbon dioxide held in the reactor liquid solution
hydrolysis reaction mixture at steady state for various temper- are relatively low. Assuming ideal gas behavior, we can make
atures at different initial feed concentrations of urea. It can be use of Raoult’s law and Dalton’s law to understand the
seen from the figure that reaction pressure increases from 50 to equilibrium of the solution.

Figure 8. Effect of reaction pressure on conversion at different initial feed
concentrations.
Raoult’s law is written as follows:
pi ) Pixi
and Dalton’s law is
pi ) Pyi
where pi is defined as the partial pressure of the component i,
Pi is defined as the vapor pressure of component i at the
operating temperature of the system, xi is the mole fraction of
component i in the liquid phase, yi is the mole fraction of
component i in the vapor phase, and P is the total pressure,
which is equal to the sum of the partial pressures of all
components in the vapor phase.
Theoretically determined reaction pressures by using Raoult’s
law and Dalton’s law based on vapor pressure of water in the
same range of temperatures are presented for comparison with
experimental data in Figure 9.
3.5. Study of Reaction Kinetics. Experiments were con-
ducted for hydrolysis of urea in a batch reactor at different
temperatures, reaction pressures, and concentrations and kinetic
study was done. From the initial feed concentration and final
concentration, the conversion was found out and the kinetic
study of hydrolysis reaction was studied. Assuming no backward
reaction, the rate constant for forward reaction was calculated.
As in the reaction excess water is used, the concentration of
water is neglected. Let -rA be the rate of reaction, CA0 the initial
concentration, and CA the concentration at any time. The rate
of reaction for forward reaction can be written as
-dCA
-rA ) ) k(CA)n
dt
Ind. Eng. Chem. Res., Vol. 48, No. 5, 2009 2709
Figure 9. Comparison of experimental and theoretically determined reaction
pressures at different temperatures.
Multiplying ln on both sides in eq 6 we have
(4) ln(-rA) ) ln(k) + n ln(CA) (7)
Hence if a graph is plotted taking ln(CA) on the abscissa and
(5) ln(-rA) on the ordinate, a straight line will be obtained whose
y-intercept represents the rate constant.
EffectofTimesonConcentration.Fromtheconcentration-time
data, a kinetic study was done. Figure 10 depicts that the
concentration of urea decrease as time increases at a constant
temperature, and also it depicts that the higher temperature
possesses less concentration of urea compared to the lower
temperature. It is observed from Figure 11 that the conversion
increases with time. For 10 wt % initial concentrations, the
conversion reaches from 0% to 88% at a constant temperature
140 °C when time increases from 0 to 90 min. So 90 min is
required for achieving 90% conversion for 10 wt % solution,
but the time will be high for higher concentration solution as
shown in Figure 11. From Figure 12 it is seen that the time
taken to achieve higher conversion is more at 120 °C and less
at 150 °C temperature.
The effect of rate on concentration at a fixed temperature is
shown in Figure 13. From the figure it is observed that the slope
of the plot is approximately 1. This indicates that the forward
reaction is first-order type. Further, the intercept of the above-
mentioned figure gives the value of forward rate constant which
is a function of temperature. It is observed from the figure that
with increase in temperature from 140 to 150 °C the forward
rate constant increases from 0.013 to 0.22 min-1. The variation
with temperature is very small because of the fact that there
was no stirring and catalyst. Table 1 shows the values of rate
(6)
constant with temperature.
2710 Ind. Eng. Chem. Res., Vol. 48, No. 5, 2009

Figure 11. Effect of time on conversion at different weight percent solutions

for constant temperature 140 °C.

Figure 10. Effect of time on concentration at different temperatures.

From the above result it is observed that the order of the

forward reaction is close to 1 and with increase in temperature
the rate constant increases. So finally the temperature depen-
dency of forward rate constant was explained by Arrhenius
theory. The rate equation can be written as follows:
-rA ) kCA (8)

where -rA is the reaction rate, k forward rate constant, and CA

concentration of urea solution.
According to Arrhenius theory, the temperature dependency
of forward rate constant can be written as

k ) Ae-E/RT (9)
where A is frequency factor and E is activation energy.
From the Figure 14 the activation energy and frequency factor
was found out as 73.6 kJ/mol and 2.89 × 107 min-1, respec-
tively. These values are compared with the values reported by
Aoki et al.18 They reported the activation energy and frequency
factor as 87.78 kJ/mol and 3.753 × 107 min-1, respectively.
3.6. Characterization of the Reactor Liquor Samples. The
detailed analysis of reactor liquid sample was done at 160 °C
and with inlet feed concentration of 10 wt % of urea to water.
The pH of the reactor liquid sample solution was 9.02. The Figure 12. Effect of time on conversion at different temperatures for constant
reactor liquid typically contains 3-4% urea, 0-5% higher urea initial feed concentration 10 wt % solution.
derivatives, and 1-2% ammonia. At temperature above 120 °C, analysis of the reactor liquor sample is shown in Figure 15.
any ammonium carbamate in the liquid formed immediately The HPLC analysis of reactor liquor samples shows the presence
decomposes to ammonia and carbon dioxide and hence very of urea, biuret, and other new products also observed. The
small concentrations (1-2%) of ammonium carbamate will be presence of urea in reactor liquor decreases compared to inlet
present in the reactor liquor, and the rest is water. The HPLC feed urea solution, but the biuret percentage increases, maybe
 Ind. Eng. Chem. Res., Vol. 48, No. 5, 2009 2711

Figure 14. Effect of temperature on rate constant.

Figure 13. Effect of concentration on reaction rate at different temperatures.

Table 1. Kinetic Data for Urea Hydrolysis in a Batch Reactor

temp (°C) k (min-1) n(calcd) n(av) R2
140 0.0134 0.947 0.947
145 0.0198 1.120 0.979
150 0.0220 1.110 1.0 0.970
155 0.0344 1.058 0.893
160 0.0350 0.913 0.935

due to the formation of higher urea derivatives as new peaks

also observed.

4. Conclusions
The objective of this work was to study the hydrolysis of
urea for generation of ammonia in a batch reactor. A number
of experiments were carried out in a batch reactor at different
temperatures taking different concentrations of urea solution
from 10 to 40% by weight, and both equilibrium and kinetic
studies were done. From equilibrium study it is concluded that
with increase in temperature and pressure the equilibrium
conversion increases and a maximum conversion of 30% is
possible with 10% concentration and at 160 °C temperature and
896.32 kPa reaction pressure. The equilibrium conversion
decreases with increase in concentration. It has also been found
that the forward reaction is a pseudo-first-order reaction with Figure 15. HPLC analysis of the precipitated solids from the reactor
rate constant varying from 0. 013 to 0.035 min-1 within the solution.
temperature range of 140 and 160 °C, respectively. The
activation energy and frequency factor of urea hydrolysis
reaction are found to be 73.6 kJ/mol and 2.89 × 107 min-1, order reaction with respect to urea. Also it can be concluded
respectively. Finally, it can be concluded that the hydrolysis of that the initial reaction rate is slower and it becomes rapid at
urea to form ammonia and carbon dioxide behaves as a first- around 130 °C. At this temperature the production of ammonia
2712 Ind. Eng. Chem. Res., Vol. 48, No. 5, 2009
is higher than that at lower temperature. Further the reaction
rate constant is function of temperature.
Acknowledgment
The authors gratefully acknowledge the financial support to
the National Thermal Power Corp. (NTPC), New Delhi, India,
has extended toward them for this work.
Nomenclature
A ) frequency factor (min-1)
CA ) final concentration of urea solution (mol/L)
CA0 ) initial concentration of urea solution (mol/L)
E ) activation energy (kJ/mol)
k ) forward rate constant (min-1)
n ) order of forward reaction
P ) total pressure (Pa)
pi ) partial pressure of the component i at the operating temperature
of the system (Pa)
Pi ) vapor pressure of component i at the operating temperature
of the system (Pa)
R ) ideal law gas constant (kJ/kgmol · K)
Ra ) rate of reaction
T ) reaction temperature (K)
t ) reaction time (min)
xi ) mole fraction of component i in the liquid phase
yi ) mole fraction of component i in the vapor phase
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ReVised manuscript receiVed September 22, 2008
Accepted November 21, 2008
IE801286H