100 Years of Ammonia Synthesis

Technology
This paper is a review of 100 years of development of an important industry – the synthesis of ammo-
nia from synthesis gas comprising nitrogen and hydrogen. In this development the name Topsøe is
important, and the year 2013 incidentally marks the 100th birthday of Dr. Haldor Topsøe, who as a
person has contributed significantly to the on-going development of this industry over more than 70
years.

The paper starts with a short review of the early development from Haber-Bosch to around 1960.
Thereafter follows a discussion of important recent developments in the following three areas: am-
monia synthesis catalysts, ammonia synthesis converter design, and ammonia synthesis process con-
cepts.

Ib Dybkjær
Haldor Topsøe A/S

In Oppau, near Mannheim, Germany, the first

Introduction industrial plant for production of ammonia from
hydrogen and nitrogen started operation. This

I
n the year 1913 a lot of important events
took place. While true for every year and
for every perspective, from the perspective
of our industry, the ammonia industry, 1913
was truly remarkable. Three events are espe-
cially noteworthy.
The Danish physicist Niels Bohr published a se-
ries of 3 papers entitled, "On the Constitution of
Atoms and Molecules" (1). This work laid, to-
gether with work by others, the foundation for
quantum mechanics and thus for the tremendous
development in physics and chemistry. Today
this development allows us to understand on the
atomic scale complex phenomena such as cata-
lytic reactions between gases adsorbed on solid
surfaces.
facility was also the first high pressure catalytic
unit ever constructed. The plant was based on
the invention of the ammonia synthesis reaction
by Fritz Haber, the identification of the most
suitable catalyst by Alwin Mittasch, and the pi-
oneering engineering developments by Carl
Bosch. This event has been described as "Deto-
nation of the Population Explosion" (2), which
through application of synthetic fertilizers for
food production, facilitated the growth in the
number of human beings on Earth from about
one billion in 1900 to about seven billion in
2000. It has been stated that a world without
synthetic fertilizers would only sustain a world
population of about four billion (3).

2013 101 AMMONIA TECHNICAL MANUAL

 In Denmark, Haldor Topsøe was born on May
24, 1913. Through the foundation of his com-
pany “Haldor Topsøe” in 1940, and through his
personal inspiration and leadership for 73 years,
Haldor Topsøe had a tremendous influence, not
only on his employees, but worldwide on the
development of the ammonia industry for at
least 50 years. A side note about Haldor Topsøe
is that as a young man, he worked with Niels
Bohr.
Historical Background and Early
Developments
At the end of the 19th century, it became evi-
dent that the known resources of nitrogen,
which were primarily ammonium sulphate (as a
by-product from coke and town gas production
from coal) and natural deposits of saltpeter
(Guano) from Chile, were not sufficient to meet
the demand for fertilizers required to increase
the agricultural yield to satisfy the world’s food
requirements. Small scale industrial production
of synthetic nitrogen compounds was developed
based on the Birkeland-Eyde process (produc-
tion of nitrogen oxides in an electric arc) and the
Frank-Caro process (production of calcium cy-
anamide, CaCN2, from calcium carbide and ni-
trogen), but these processes were inefficient,
expensive, and not well suited for large scale
production.
On this background, the history of modern am-
monia synthesis started in Germany shortly after
1900, when Fritz Haber and his co-workers
from BASF developed and patented the process
concept which forms the basis for all ammonia
production today. Their contributions are as fol-
lows: Fritz Haber developed the synthesis pro-
cess and demonstrated it in laboratory scale, Al-
vin Mittasch tested literally thousands of
catalysts and identified the promoted iron cata-
lyst, and Carl Bosch did the engineering devel-
opment of what was to become the first indus-
trial high pressure catalytic unit in history.
AMMONIA TECHNICAL MANUAL
The plant, located at Oppau/Ludwigshafen near
Mannheim, Germany, was commissioned in
1913 with a capacity of 30 MTPD (33 STPD).
The capacity was rapidly increased to 250
MTPD (275 STPD) in 1916. In 1917, a second
plant was started at Leuna, near Leipzig, Ger-
many, which after further expansion produced
240,000 MTPY (265,000 STPY)) at the end of
the First World War.
Soon after the First World War, others started
development work, partly on the basis of the
German pioneering effort. A plant was started
at Terni, Italy, in 1920 based on synthesis tech-
nology developed by Luigi Casale. In France, a
plant was constructed in 1921 at Montereau,
based on developments by M.G. Claude. Both
the Casale and the Claude technologies used ex-
tremely high pressures. Additionally, early de-
velopments in Europe synthesis technology de-
veloped by Giacomo Fauser were adopted by
the Italian company Montecatini, and Friedrich
Uhde GmbH constructed a plant to operate on
coke oven gas from the Mont Cenis Company.
This plant used a special synthesis technology
later known as the Mont Cenis process. The
features of this process were very low operating
temperature and pressure and a special catalyst
based on iron cyanide.
In parallel, independent development work took
place in the USA. In 1918 a plant called “US
Nitrate Plant No. 1” was constructed in Ala-
bama. The plant was, however, not very suc-
cessful, but the developments continued in the
1920’s with the construction of several success-
ful plants. In 1928, an American company (Ni-
trogen Engineering Corporation, NEC) was
commissioned to construct a plant in Europe,
thereby entering the worldwide competition.
In spite of these developments, Germany still
dominated the industry. In 1937, the annual
world production of ammonia was
755,000 MTPY (830,000 STPY), of which 72%
was still concentrated in Oppau and Leuna.
102 2013
 During the Second World War, the preferred
feedstock changed, especially in the USA, from
coke to natural gas, and the worldwide produc-
tion capacity increased rapidly. In 1945 about
125 ammonia plants existed with a total capaci-
ty of 4.5 million MTPY (5.0 million STPY).
The most important processes were: Haber-
Bosch, Casale, Claude, Fauser, NEC and Mont
Cenis.
Already before the war it was the general opin-
ion that the ammonia synthesis technology was
mature, and that no significant further develop-
ments could be expected. This conclusion was
to a certain extent true, since many of the fea-
tures that characterize modern technology – in-
cluding catalyst type, operating conditions and
converter design – were already well proven in
industrial applications. However, the plants
looked very different from what we know today.
The synthesis gas was most often produced
from coke at atmospheric pressure and stored in
large gas holders, which served as the link to the
synthesis section. The synthesis gas was com-
pressed in reciprocating compressors, which had
limited capacity corresponding to 300 – 400
MTPD (330 – 440 STPD) of ammonia.
In the synthesis section, several parallel trains
were often used (in the Leuna plant, which op-
erated until 1990, there were 18 synthesis loops
in parallel). In early plants the effluent from the
ammonia converter was cooled with cooling wa-
ter without any recovery of heat. It soon be-
came evident that the economics of ammonia
production could be improved by recovery of
this waste heat, and steam production and/or
boiler feed water preheating by the reactor ef-
fluent was introduced.
With respect to converter technology, it was an
important factor that the vessel fabrication tech-
nology available before the war limited the size
of the converter pressure shell. Therefore, the
physical dimensions of the converter were limit-
ing the achievable production capacity. As a
consequence, great emphasis was given to the
2013
ammonia production per unit converter volume,
and quite complicated mechanical constructions
were developed to maximize the production ca-
pacity of a given volume.
The overall process scheme for production of
ammonia from light hydrocarbons, i.e. natural
gas, LPG or naphtha, was right from the start
similar to that used in most plants today. In
most cases the plants comprised the following
process steps:
 Feed purification
 Primary and secondary reforming
 Shift conversion
 CO2 removal
 Final purification of synthesis gas
 Compression and ammonia synthesis
 Ammonia recovery and refrigeration
During the period from the war and up to about
1965, significant developments took place with-
in each of these process steps. Detailed descrip-
tions of these developments can be found in the
references (4, 5, 6) listed at the end of this pa-
per. Key steps in the development of this pro-
cess concept were as follows:
 From multi-train units (often with different
number of trains in front-end and synthesis
loop) to single-stream plants.
 From atmospheric pressure to high pressure
(about 30-40 barg or 425-570 psig) in the
synthesis gas preparation.
 From low capacity (about 100 MT per train)
to higher capacity (the first "large" single-
stream unit was a 600 MTPD plant).
 From one stage high temperature CO conver-
sion with a promoted iron oxide catalyst, to
two stage CO conversion – first with two re-
actors with iron-based catalysts; later with
one reactor with an iron-based catalyst fol-
lowed by a second reactor with a copper-
based catalyst operating at low temperature.
The introduction of the low temperature CO
conversion was facilitated by the develop-
ment of effective methods for removal of sul-
fur from the feed stocks.
103 AMMONIA TECHNICAL MANUAL
  Improved energy efficiency – from well
above 60 GJ/MT (or MMBTU/MT) of am-
monia in the pre-war coke based plants to 40-
50 GJ/MT (or MMBTU/ST) in the first natu-
ral gas based plants and 30-40 GJ/MT (or
MMBTU/ST) in the first single-stream
plants.
 Recovery of heat in both synthesis gas prepa-
ration and synthesis loop by steam produc-
tion at increasing pressure.
 Change from reciprocating compressors to
centrifugal compressors.
 Use of quench-cooled converters in the syn-
thesis instead of more complicated types with
internal cooling. Quench converters (10-12
beds) were first used in the natural gas based
plants constructed in U.S.A. during the Sec-
ond World War. Later developments reduced
the number of beds to 2-4, and this type of
converter was predominating in the 1960's
and 1970's.
The "end-product" of this development was the
large capacity, single-stream ammonia plant
which emerged in the early 1960's, and which is
still the dominating concept in the ammonia in-
dustry today (7).
When the large capacity, single-stream ammo-
nia plant was a reality, a veritable explosion oc-
curred in the industry. During the period from
about 1963 to 1975, more than one hundred
plants were constructed, and the installed capac-
ity almost tripled (8). In this period, many dif-
ferent companies offered technology for produc-
tion of ammonia to the market. Comprehensive
surveys may be found in the references (4, 5)
listed at the end of this paper. The most im-
portant technology suppliers were Chemico (the
successor of the Nitrogen Engineering Corpora-
tion), Foster Wheeler, ICI, Kellogg, Topsøe and
Uhde.
AMMONIA TECHNICAL MANUAL
Ammonia Synthesis Catalysts
Traditional industrial ammonia catalysts are
iron-based. They are prepared by fusion of iron
and adjusted with various promoters, predomi-
nantly potassium, calcium and aluminium,
which may be added to the melt as oxides, hy-
droxides, carbonates or nitrates. Upon solidifi-
cation, the product is crushed and sieved to the
desired particle size - today, typically 1.5-3 mm
irregular-shaped particles.
The catalyst is supplied in either the as-
prepared, unreduced form, or in the prereduced,
metallic state. In the prereduced form the cata-
lyst is highly pyrophoric and must be passivated
by controlled oxidation of the iron surface in or-
der to enable safe handling upon exposure to air.
Efforts to develop more active ammonia synthe-
sis catalysts have been on-going. Both catalysts
based on wüstite (9, 10, 11) and cobalt contain-
ing catalysts (12) have been commercialized.
In addition to enhancements to the iron-based
catalyst, alternatives to the iron-based catalysts
have been thoroughly researched. Although the
high activity of ruthenium-based catalysts was
recognized early (13), it was the work by Japa-
nese researchers (14) on alkali promoted, carbon
supported ruthenium catalysts that triggered re-
newed interest and immense research efforts in
identifying and researching alternative catalysts.
Using cesium or barium promoted ruthenium
catalysts, activities about an order of magnitude
higher than seen for the iron catalyst may be
achieved, especially at high ammonia partial
pressure, since the inhibition by ammonia is
significantly less severe than for the traditional
catalyst. Several other supports have been re-
ported including MgO, MgAl2O4 , boron nitride
and zeolites. A barium-promoted ruthenium
catalyst on a special oxide support (15) and a ru-
thenium-loaded electride with high electron-
donating power and good chemical stability (16)
were both reported to have high activity for
ammonia synthesis. Although promoted ruthe-
104 2013
 nium catalysts have been introduced in the in-
dustry (17), it is still an open question whether
limited supply, high cost, and environmental
risks will allow widespread use of ruthenium-
based catalysts. Other alternatives, including
non-iron, non-ruthenium catalysts, have been
researched. Among these a novel class of high-
active bimetallic nitrides have been discovered,
e.g., cesium-promoted Co3Mo3N (18, 19) and
barium-promoted cobalt catalysts (20). Howev-
er, all these alternatives are competing against a
class of traditional low-cost, iron-based catalysts
characterized by high activity and with a dura-
bility which is unsurpassed in industrial cataly-
sis.
Ammonia Synthesis Converters
In text books about chemical reaction engineer-
ing and similar subjects, the discipline “reactor
design” often seems to be interpreted as, “de-
termination of necessary reactor (catalyst) vol-
ume”. However, there are several other factors
to consider in reactor design - at least when this
is interpreted as all information required as an
instruction to a supplier of a reactor for a specif-
ic practical application. Some of the more im-
portant points – with reference to a catalytic re-
actor – are listed below (21):
Chemistry and Thermodynamics
 The reaction, possible side reactions
 Thermodynamics (equilibrium, heat of reac-
tion, properties of reactants and products)
 Possible catalyst poisons
Reaction Kinetics
 Intrinsic kinetics + diffusion parameters
 Pellet kinetics
Properties of Catalyst
 Thermal stability
 Particle size and shape
 Pore system
 Mechanical strength
 Change in properties during activation
and/or operation
2013
Process Optimization
 Operating temperature and pressure, risk of
“run-away”
 Energy recovery
 Pressure drop
 Limitations in volumetric flow
 Gas distribution in catalyst bed
Process Control
 Temperature, pressure and flow control
 Safety aspects, start-up and shut-down
Mechanical Design
 Materials of construction, strength and cor-
rosion resistance
 Workshop manufacture
 Transport restrictions
 Erection
The basic data – chemistry and thermodynamics
– will define a broad range of conditions where
the reaction is possible at all. The reaction ki-
netics and the properties of the catalyst – in
many cases especially the thermal stability –
will narrow the range of possible operating con-
ditions and in some cases dictate choice of reac-
tor type (e.g. cooled vs. non-cooled design).
Process optimization studies, energy and cost
considerations, and safety aspects will finally
determine at what range of conditions the reac-
tor should operate. Mathematical models are
then used to determine dimensions of the reactor
required to obtain the performance (conversion
and pressure drop) selected after process opti-
mization studies. Piping connections and in-
strumentation is then designed, proper materials
of construction are selected, workshop construc-
tion, transport issues and catalyst loading and
unloading are considered, and at last the design
of the reactor is completed.
Ideally, the design of a reactor following the
above principles should lead to one optimal so-
lution – the best design for the specific case.
However, the real world does not work in this
way for a number of reasons including intellec-
105 AMMONIA TECHNICAL MANUAL
 tual property rights. This is clearly shown – if
not by other evidence, then by the multitude of
solutions found for the same problem, in our
case for the design of ammonia synthesis reac-
tors.
Below is given a list of types of converters,
which have been used in ammonia synthesis
loops.
Non-Cooled Reactors
 Axial flow (e.g. C. F. Braun one bed con-
verters in series)
 Radial Flow (e.g. Haldor Topsøe S-50 con-
verter, Uhde one bed converter)
 Axial/radial flow (e.g. Casale converter)
Cooled Reactors
 Quench cooled reactors
o Axial flow, 2-12 beds (e.g. M. W. Kel-
logg early designs)
o Radial flow, 2 beds (e.g. Haldor
Topsøe S-100 converter (1966))
o Horizontal converter (e.g. M. W. Kel-
logg)
 Indirect cooling in catalyst bed
o Axial, counter-current flow (e.g. Ha-
ber-Bosch, Claude, Mont Cenis,
Fauser, TVA-converter)
o Axial, co-current flow (e.g. NEC)
o Radial Flow (e.g. Casale “isothermal”
converter)
 Cooling between catalyst beds
o Axial flow in catalyst beds (e.g. M. W.
Kellogg intermediate designs)
o Radial Flow in catalyst beds (e.g. Hal-
dor Topsøe S-200 and S-300, KBR
KAAP converter, Uhde 2 and 3 bed
converters)
o Casale (axial/radial flow)
o Horizontal converter (KBR)
Several of the converter designs mentioned were
available in several versions, making the total
number of commercialized converter designs
AMMONIA TECHNICAL MANUAL
quite substantial. A review of the different ver-
sions is beyond the scope of this presentation.
Detailed reviews of ammonia synthesis convert-
er designs may be found in references (4-6) at
the end of this paper. Reviews of older types
may be found in reference (22).
Today radial flow converters with indirect cool-
ing between catalyst beds, first introduced by
Haldor Topsøe in the early 1970’s as replace-
ment for the quench cooled S-100 (which was
the first commercial radial flow converter), are
completely dominating the industry. They are
used by all important suppliers of ammonia syn-
thesis technology - Haldor Topsøe, KBR, Uhde
and Casale. The only non-radial flow converter
used by these licensors is KBR’s horizontal
converter, which features most of the ad-
vantages offered by the radial flow designs.
Process Concepts
The operating conditions in the ammonia syn-
thesis loop are described by a number of param-
eters, which in some cases may be independent
variables, and in other cases a function of other
parameters. The most important parameters are
loop pressure, separator temperature, recycle ra-
tio, conversion per pass, and inert level. The re-
lationship between these parameters (and other
parameters such as space velocity, concentra-
tions and temperatures at various points in the
synthesis loop etc.) can be described in mathe-
matical models which are used for design, simu-
lation and optimization. In conventional syn-
thesis technology, used in most modern plants
irrespective of technology supplier, the loop
pressure is typically 150-220 barg (2200-3200
psig) with synthesis gas compression in 2 or 3
stage centrifugal compressors.
In the period from 1975 until now the main de-
velopment has been an increase in the typical
single-stream capacity from 900 MTPD
(1000 STPD) in 1975, to 1500 MTPD
(1600 STPD) in the 1990’s, and to (typically)
2200 MTPD (2400 STPD) today. Even larger
106 2013
 capacities are possible, but have only been se-
lected in very few cases.
Other developments in the ammonia synthesis
technology are as follows:
 Widespread use of hydrogen recovery
from purge gas (in membranes, cryogenic
units, or by pressure swing adsorption).
 Increased interest in co-production of
other products, especially methanol (23).
The competition between suppliers of ammonia
synthesis technology is fierce. Three licensors,
Haldor Topsøe, KBR, and ThyssenKrupp Uhde,
now dominate the market for complete synthesis
units. A very brief description of key elements
in the technology supplied by these three com-
panies is given below. In addition, it may be
mentioned that Ammonia Casale has a strong
position in the market for revamp of ammonia
synthesis converters with their axial/radial flow
converter design.
Haldor Topsøe A/S
Key elements in Topsøe’s synthesis technology
are as follows:
 Proprietary iron-based catalyst
 Proprietary radial flow converters (1-, 2-,
and 3-beds)
 Proprietary waste heat boiler
Recent developments in this technology include
the following:
 3-bed converter (S-300)
 S-350 converter configuration (S-300 +
S-50 (one bed converter)
 New bayonet tube waste heat boiler de-
sign
KBR
KBR is a fusion of M. W. Kellogg and Braun
(original name C. F. Braun, later Santa Fe
Braun, and most recently Brown & Root
Braun).
2013
Key elements in KBR’s synthesis technology
are as follows:
 A conventional concept with iron-based
catalyst in horizontal converter
 A low pressure concept (the KAAP pro-
cess) with ruthenium catalyst in the lower
3 beds in a 4-bed radial flow converter
 A proprietary waste heat boiler design
 A unitized chiller
ThyssenKrupp Uhde (formerly Uhde)
Key elements in Uhde’s synthesis technology
are as follows:
 Conventional with proprietary radial flow
converters (1-, 2-, and 3 beds)
 Dual pressure process with once-through
converter before the last compressor stage
 Proprietary waste heat boiler
For detailed and updated descriptions of these
technologies, reference is made to the respective
company websites (24, 25, 26).
The Future
The ammonia synthesis technology is a mature
technology. The process concept has, in princi-
ple, been unchanged for many decades. Maturi-
ty does not, however, mean that the technology
has not developed over the years, or that it will
not continue to be developed in the future to fur-
ther improve capital and operating cost and to
improve efficiency, safety and reliability of the
production process. Below are some viewpoints
on developments to further improve capital and
operating cost, and to improve efficiency, safety
and reliability of the production process that
may be expected.
Energy Consumption
Over the last 25-30 years the specific energy
consumption for the overall ammonia plant has
been reduced by approximately 30%. The cur-
rent nominal energy consumption is now just
30% above the theoretical minimum. Very like-
107 AMMONIA TECHNICAL MANUAL
 ly, this level represents the “practical theoretical
minimum” for energy consumption, taking una-
voidable losses in unit operations and chemical
processes into consideration. Significant further
reduction can thus not be expected, and any mi-
nor improvements will most probably be
achieved in the synthesis gas generation part of
the ammonia plant, and not in the ammonia syn-
thesis itself, which accounts for “only” 14% of
the theoretical energy loss.
Capacity
Just before the year 2000 the general opinion
was that the size of ammonia plants had reached
a limit imposed by logistics related to storage
and transportation. However, in the first decade
of the 21st century we have seen construction of
the first plant with a capacity above 3000
MTPD (27), and plants with even higher capaci-
ty are discussed (28). If nothing else, this
growth proves that foretelling is difficult, and
that one should be careful when talking about
future limitations in industrial developments.
Break-away Technology
In the early 1990’s, a few ammonia plants using
a heat exchange reformer (29) were constructed.
Later, others have also commercialized heat ex-
change reforming (30, 31). However, only a
few ammonia plants utilizing this concept have
been constructed so far, all in situations where
steam export is undesirable.
Distributed production of ammonia based on
construction of small capacity ammonia plants
is advocated by some. The argument is that
each farm can have its own fertilizer production
facility, possibly with biomass as the raw mate-
rial, and/or that ammonia can be part of a dis-
tributed fuel supply system. The technologies
proposed are new and interesting, but none of
them seem to have potential to compete in any
normal economic environment with the well-
established large scale technology. The industry
prefers construction of large capacity production
facilities near cheap raw material sources and
AMMONIA TECHNICAL MANUAL
transport of the product by ship, rail or pipeline
to the main consumer areas.
Biological fixation of nitrogen is possible and
known from nature (e.g., peas, which host nitro-
gen-fixing bacteria in a symbiotic relationship).
Some may argue that modern genetic engineer-
ing can easily transfer the ability to fix nitrogen
to other crops vital for our food supply, and that
this would be the end of the fertilizer industry as
we know it today. This vision is perhaps possi-
ble, but the timeframe for such a development is
not easy to predict. Certainly it will not happen
in the near future.
Conclusions
The fertilizer industry will be with us more or
less in its present form for decades to come.
The production capacity for synthetic ammonia
- today at about 160 million MTPY (32) - will
continue to grow at 1-2% per year to satisfy the
increasing demands for food from an increasing
number of people enjoying increasing welfare.
Energy consumption will be reduced only mar-
ginally, if at all. The capacity of the typical
plant will slowly increase to 3000 MTPD or
perhaps even higher. A few very small plants,
possibly based on biomass, may be constructed,
but not in numbers which will have any
measureable impact on the market. Ammonia
will continue to be produced mainly in large ca-
pacity plants located near a supply of cheap nat-
ural gas.
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24. www.topsoe.com/business_areas/ammonia
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26. www.thyssenkrupp-uhde.de/technologies/
ammonia

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