2 Manual en Ingles Apendix 1 - Activation of KM1R and KM111 in 3-Bed Radial Flow Converter

Manual
Activation of KM1R/KM111
catalysts in a three-bed
radial flow converter
Making optimal performance possible
Haldor Topsoe A/S | Haldor Topsøes Allé 1 | 2800 Kgs. Lyngby | Denmark
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Manual – Activation of KM1R/KM111 in three-bed radial flow converters
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Table of contents
1 Introduction 4
1.1 The manual 4
1.2 Purpose of manual 4
2 The catalysts 4
2.1 KM1R/KM111 4
2.2 Pre-reduced catalyst 4
2.3 Filling densities 4
3 Catalyst activation 5
3.1 Activation of iron oxide 5
3.2 Heat of reaction 5
3.3 Amount of water formed during the activation 5
3.4 Activation schedule 5
4 Purging 6
4.1 Oxygen removal 6
5 Gas composition 7
5.1 Reducing gas 7
5.2 H2/N2-ratio 7
5.3 Establishing make-up gas addition and purge 7
5.4 Early stage of the reaction 7
5.5 Ammonia concentration at the inlet of the converter 8
5.6 Water concentration at the inlet of the converter 8
5.7 Oxygen equivalents and other poisons 8
6 Cooling 9
6.1 Water/air cooler 9
6.2 Refrigeration chillers 9
6.2.1 Sampling of aqueous ammonia 10
6.2.2 Refrigeration compressor 10
7 Gas circulation 10
7.1 Circulation rate 11
8 Start-up heater (SUH) 11
Information contained herein is confidential; it may not be used for any purpose other
than for which it has been issued, and may not be used by or disclosed to third parties
without written approval of Haldor Topsoe A/S.
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8.1 SUH outlet temperature 11

8.2 SUH maximum load 11
9 Gas distribution 12
9.1 Main inlet 12
9.2 Pressure shell and converter outlet temperature limits 12
9.3 Cold shot and inter-bed heat exchanger (IHE) valve(s) 12
10 Loop pressure 13
11 Temperature of the catalyst 13

11.1 Uniform bed temperatures 13
11.2 Asymmetrical activation 13
11.3 Equalization of uneven temperatures 14
12 Water formation 14
12.1 Analysis of water content 14
12.2 Methods for water determination 14
13 Activation procedure 15
13.1 Activation time frame and data collection 15
13.2 First period 16
13.2.1 Valve positions 16
13.2.2 Pressure 16
13.2.3 Cooling 16
13.2.4 Circulation rate 17
13.2.5 Start-up heater 17
13.2.6 Heating up rate 17
13.2.7 Heat recovery 17
13.2.8 Bi-hourly water analysis 17
13.3 Second period 17
13.3.1 Catalyst temperatures 18
13.3.2 Pressure 18
13.3.4 Heating up rate 18
13.4 Third period 18
13.4.1 First signs of reaction 18
13.4.2 H2/N2-ratio 18
13.4.3 Analyses of ammonia 19
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13.4.4 Cooling with chiller(s) 19

13.4.5 Catalyst temperatures 19
13.4.6 First bed temperature control 19
13.4.7 Second and third beds temperature control 19
13.4.8 Pressure 20
13.5 Fourth period 20
13.5.1 Third bed inlet temperature 20
13.5.2 Pressure 21
13.6 Fifth period 21
13.6.1 Bringing the start-up heater offline 21
13.6.1.1 Reducing the start-up heater load 21
14 Interrupting the activation procedure 22

14.1 Avoid stagnant atmosphere 22
15 Notice and disclaimer 22

15.1 General recommendations 22
15.2 Liability 22
15.3 Advisors 23
15.4 Unclear points 23
16 Contact 23
Appendix 1: Control principles for S-300 without LHE 24
Appendix 2: Control principles S-300 without LHE (S-200 revamped) 25
Appendix 3: Control principles for S-300 with LHE (S-200 revamped) 26
Appendix 4: Log sheet sample 27
Appendix 5: Water vapor in ammonia synthesis gas mixtures 28

I. Gas chromatography method 28
II. Ascarite method 31
III. Calcium carbide method 35
IV. Approximation method 38
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1 Introduction
1.1 The manual
This manual contains Topsoe’s recommendations for the activation of a combined charge of Topsoe
ammonia synthesis catalysts KM1R and KM111 in a radial flow converter.
1.2 Purpose of manual

The aim of this manual is to ensure that the catalyst activation is carried out in a proper way, thereby
achieving the maximum catalyst activity.
Should any deviation from this procedure be necessary, we recommend discussing this with Haldor
Topsoe A/S before starting the activation.
2 The catalysts
2.1 KM1R/KM111
The catalysts installed in beds 1, 2, and 3 respectively are Topsoe ammonia synthesis catalysts
KM1R, KM 111, and KM 111. The standard size for both catalysts is 1.5–3.0 mm.
2.2 Pre-reduced catalyst

KM1R is produced by carefully controlled reduction of KM1 at Haldor Topsoe catalyst manufacturing
facilities. As part of the pre-reduction procedure, the catalyst is skin oxidized, which allows safe
handling during the loading of the catalyst.
2.3 Filling densities

When loaded according to Topsoe guidelines, the filling densities for the catalysts are in the
following range:
- for KM1R from 2,200 to 2,500 kg/m3 (137–147 lbs./ft3)

- for KM111 from 2,800 to 3,000 kg/m3 (175–187 lbs./ft3)
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3 Catalyst activation
This chapter gives Topsoe’s recommendations concerning certain operating parameters during the
activation and concludes with a chronological description of the activation process.
3.1 Activation of iron oxide

The catalyst activation consists of the reduction of the iron oxide in the catalyst to elementary iron
and requires heating of the catalyst. The pre-reduced KM1R catalyst will start reducing at about
225°C (440°F), and the unreduced KM111 catalyst will start reducing at between 380–400°C (715–
750°F).
The reaction taking place during the catalyst activation is:
Fe3O4 + 4H2 ® 3 Fe + 4 H2O *
* Fe3O4 : Iron (II, III) oxide
3.2 Heat of reaction

The catalyst activation does not produce nor consume heat in any noticeable amount. Therefore, in
order to reach temperatures where the catalyst is activated, heat must be supplied by other means,
which in this case will be a start-up heater. Later on, when the activation in the first bed is far
advanced and synthesis of ammonia has commenced, the heat released from the reaction is used to
keep up the temperature.
3.3 Amount of water formed during the activation

The water formed during the activation is equivalent to 20 kg per metric ton (40 lbs. per ST) of pre-
reduced catalyst and about 280 kg per metric ton (560 lbs. per ST) of unreduced catalysts. A large
part of the water will arise as aqueous ammonia.
3.4 Activation schedule

The activation is conveniently considered as consisting of five periods.
- First period: The catalyst is heated to a level where the activation of the pre-reduced catalyst
begins.
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- Second period: The pre-reduced catalyst has been activated and the first signs of ammonia
production are seen. Furthermore, the heating continues to a temperature where the
activation of the unreduced catalyst in the second bed starts.
- Third period: The unreduced catalyst in the second bed is activated and ammonia synthesis
reaction is seen across the bed. At the same time, the activation of the unreduced catalyst in
the third bed has commenced.
- Fourth period: The catalyst in the third bed is active to an extent that no external heat source
is needed to keep the temperature high.
- Fifth period: The start-up heater can be taken out of service and the converter can slowly be
brought into normal operation.
The following sections present Haldor Topsoe’s detailed activation procedure as well as
recommendations concerning certain operating parameters during the activation.
4 Purging
4.1 Oxygen removal
In order to remove oxygen after loading of the catalyst and closing of the converter, it is very
important that the synthesis loop is purged thoroughly with nitrogen.
The purging of the loop is done with nitrogen by pressurizing and depressurizing three to five times.
Particular attention should be paid to the converter as the loaded catalyst may contain some pockets
of air that might be difficult to remove.
Any leftover of oxygen will react with the pre-reduced catalyst when the temperature of the catalyst
approaches 100°C (212°F). Thus, if relatively large amounts of oxygen are present, the activation
will be prolonged unnecessarily.
The oxygen level should preferably be kept below 1,000 ppmv in the loop near atmospheric
pressure.
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5 Gas composition
5.1 Reducing gas
Basically, the activation of the ammonia synthesis catalysts KM1R and KM111 could be carried out
with pure hydrogen. However, it is strongly recommended that the catalysts are activated in
synthesis gas of normal composition, i.e. with a H2/N2 ratio close to 3, as this will give a smooth
transition from activation to normal operation. Furthermore, it is recommended that the activation is
carried out in circulating gas.
5.2 H2/N2-ratio
Throughout the activation, the H2/N2 ratio should be maintained at 3. This allows the reaction to start
as soon as part of the catalyst has been activated. This will further prevent abrupt changes in the
catalyst temperatures and thus diminish the risk of affecting the catalyst and equipment adversely.
5.3 Establishing make-up gas addition and purge

It is recommended that the activation is carried out in circulating gas. The activation is a solely
hydrogen-consuming process. Thereby, in order to maintain the H2/N2 ratio at 3, it may be necessary
to have some make-up gas addition and some purging established from the beginning of the
heating. The purging is mandatory when the reaction starts and is continued throughout the
activation.
5.4 Early stage of the reaction

When the activation is carried out with normal synthesis gas and at a pressure not too low, the
ammonia synthesis reaction will start some time before the activation is complete. This offers two
advantages:
1. The heat produced allows for increasing the circulation rate above what can be supported by
the start-up heater alone. This ensures that the last part of the activation is carried out faster
than would otherwise be the case. At the same time, a gradual transition from activation to
normal operation is obtained.
2. The co-condensation of the produced ammonia and activation water results in a more
efficient removal of water from the synthesis gas before the gas is recycled to the converter.
This is highly important as water is poisonous to the catalyst.
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5.5 Ammonia concentration at the inlet of the converter

When the reaction starts, a low ammonia concentration at the inlet of the converter will give a higher
potential for ammonia synthesis. Therefore, the circulating gas should always be cooled as much as
possible in the water/air cooler and chiller(s) without violating other restrictions, cf. section 6.
The ammonia content in the inlet and outlet gases of the converter should be initiated when
significant signs of ammonia synthesis reaction are seen at temperatures near 380–400°C (740–
780°F).
5.6 Water concentration at the inlet of the converter

Cooling down the gas to the lowest attainable temperature further ensures a more efficient co-
condensation of water with ammonia. This results in a more efficient removal of water from the
synthesis gas before the gas is recycled to the converter, thus resulting in a minimization of the
water concentration at the converter inlet. This is highly important as water is poisonous to the
catalyst. The improved purification is obtained for two reasons, namely:
1. The equilibrium pressure of water vapor above the liquid phase consisting of ammonia and
water is lower than that above a liquid phase consisting of pure water
2. The freezing point of the mixed liquid phase is lower than that of pure water and allows for
the application of a lower condensation temperature.
Low water content further ensures that the highest activity is obtained and enhances the
temperature increment due to a higher degree of ammonia formation.
In the very unlikely event that some catalyst has become unstable and starts heating, the catalyst in
the drum or lifting hopper in question should be discarded.
5.7 Oxygen equivalents and other poisons

The level of oxygen equivalents (CO + CO2) in the make-up gas should be kept as low as possible
(0–10 ppmv). To calculate the number of oxygen equivalents, the following formula should be used:
Oxygen equivalents = (Concentration of CO) * 1 + (Concentration of CO2) * 2
Example: For a make-up gas with a concentration of 1.0 ppmv of CO and 2.5 ppm of CO2, the
oxygen equivalents are:
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Oxygen equivalents = (1.0) * 1 + (2.5) * 2 = 6.0
It should be emphasized that the gas should be free from catalyst poisons such as halogens, sulfur,
phosphorous, and arsenic.
6 Cooling
As described in section 5, low water and ammonia contents at the converter inlet is beneficial. This
can be obtained by cooling the gas to the lowest possible level without violating other restrictions, cf.
description of chiller(s) below.
6.1 Water/air cooler

The water/air cooler should be taken into operation from the moment the circulation of gas is started.
If available, ammonia injection should also be considered part of the start-up procedure. In this case,
the loop chiller(s) may be started almost immediately.
6.2 Refrigeration chillers

The most efficient removal of water from the circulating gas is obtained when the refrigeration
chiller(s) is (are) taken into service. Therefore, it is important that the circulating gas is cooled in the
chiller(s) as soon as this/these can be taken into service without any risk of water freezing in the
chiller(s).
The refrigeration chiller(s) should be taken into service when the condensate collected in the
ammonia separator downstream the chiller(s) constantly exhibits an ammonia concentration high
enough to prevent freezing, even if the temperature in the chiller(s) drops lower than intended.
The condensate can freeze in the chiller tubes even though the gas temperature outlet the chiller(s)
is above 0°C (32°F), since the surface of the cooling coils or tubes submerged in liquid ammonia is
colder than the gas and might be cold enough to cause freezing.
Particularly for this reason, working with a large safety margin is advisable. When the ammonia
separator condensate has a concentration of about 190 grams ammonia per liter of water (1.6 lbs.
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ammonia per gallon), its freezing point is below the boiling point of pure liquid ammonia at
atmospheric pressure.
Furthermore, when analyses of the ammonia water mixture condensed in the separator downstream
the chiller(s) show that the freezing point is sufficiently low, i.e. 25% by weight ammonia or more, a
temperature down to the normal temperature at the outlet of the chiller(s) is allowed.
Nevertheless, the chiller(s) is (are) not commissioned before the catalyst has gained substantial
activity and the ammonia concentration at the inlet of the converter is close to the chemical
equilibrium concentration. In this case, the chiller(s) should be commissioned slowly in order to avoid
a drastic drop in ammonia inlet concentration, which would result in a fast increase of reaction rate
and an uncontrollable development in the catalyst temperatures.
6.2.1 Sampling of aqueous ammonia

The sample of the ammonia/water mixture in the separator should be taken not too long after the
separator has been emptied. This ensures that the sample contains the actual mixture. The strength
of the aqueous ammonia can be measured in several ways, e.g. by evaporation of the ammonia, by
titration, by density measurement.
6.2.2 Refrigeration compressor

If it is possible to run the refrigeration compressor at a stable suction pressure of 4 kg/cm2g (57 psig)
or more, the refrigeration compressor can be put into operation from the very beginning of circulating
gas in the loop.
7 Gas circulation
It is recommended that the activation is carried out in circulating gas from the beginning, as this
allows a better control of the development in catalyst temperatures. When the pre-reduced catalyst
in the first bed starts becoming active, it may gain activity very quickly. Therefore, it will be necessary
to have the circulator in service in order to have proper temperature control. The circulation rate
should be as high as possible, keeping the required heating up rate in mind.
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7.1 Circulation rate

A high circulating rate ensures a proper gas distribution in the beds and thus a uniform heating of the
catalyst. When the catalyst activation starts, the high circulation rate will give a low concentration of
water vapor in the gas leaving the catalyst.
A high circulation rate leads to the highest catalyst activity. It also helps to keep the water content of
the synthesis gas at a low level. The water concentration in the gas should not exceed 3,000 ppmv.
8 Start-up heater (SUH)

8.1 SUH outlet temperature
During the first part of the heating up, when the catalyst temperatures are low, the start-up heater
outlet temperature should preferably be kept to maintain a maximum temperature difference of less
than:
- 150°C (270°F) with respect to the highest temperature in the catalyst section, i.e. typically the
inlet to the first bed and
- 200°C (360°F) with respect to the converter outlet.
The gas flow through the start-up heater should be fairly large. The heating up rate is controlled by
increasing the energy input to the start-up heater.
8.2 SUH maximum load

When the load on the start-up heater is at its maximum, it should be maintained and further
temperature changes should only be carried out by adjusting the gas flow. This will ensure that
maximum circulation is maintained throughout the activation. The minimum flow will be reached just
when reaction starts in the first bed.
At this time, the circulation rate should correspond to a space velocity of at least 1,000 Nm3/h per m3
(1,000 SCFH per ft3), preferably 1,500 Nm3/h per m3 (1,500 SCFH per ft3) of catalyst or even higher.
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9 Gas distribution
For better understanding of this section, we advise to study the sketches of the control principles for
Topsoe’s three-bed converters (S-300) in Appendices 1–3.
9.1 Main inlet

From the beginning of the first period, part of the synthesis gas is introduced through the normal
main inlet in order to ensure that the pressure vessel is cool and – in case of a converter with lower
heat exchanger – to later ensure that the heat content of the effluent from the third bed is recovered
in the internal feed/effluent heat exchanger.
The gas stream passing through the main inlet is combined with the hot gas from the start-up heater
introduced through the cold-shot pipe. After the conditions in the start-up heater have stabilized, the
temperature at the inlet of the first bed is controlled by adjusting the circulation rate, using either the
circulator by-pass and/or the main inlet valve.
9.2 Pressure shell and converter outlet temperature limits

The main inlet valve should, of course, be operated so that the converter outlet temperature and the
pressure shell temperature are kept within the given limits.
9.3 Cold shot and inter-bed heat exchanger (IHE) valve(s)

During the activation, the cold shot valve should be fully closed. This will avoid thermal stress in the
start-up heater and cold shot pipe going to the converter.
The inter-bed heat exchanger (IHE) valve is present in Topsoe’s three-bed converters (S-300 and
revamped S-200 converters) with a lower heat exchanger. Thus, the following section only applies to
these types of converters.
The IHE valve for quench gas, i.e. the gas to be introduced via the second inter-bed heat exchanger,
has to be fully closed at the beginning of the catalyst heating and activation. It is, however,
recommended that the IHE valve is cracked open to avoid thermal shock when quench gas is
introduced later on. This is due to the fact that when the catalyst in the first bed gains activity, the
inlet temperature to the second bed has to be controlled by introducing gas to the tube side of the
inter-bed heat exchanger. Changes in the flow rate through the IHE valve will imply changes of the
main gas flow rate in order to keep the first bed inlet temperature unchanged.
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10 Loop pressure
During the heating period, an operating pressure of 85 kg/cm2g (1210 psig) is recommended, if it is
possible with regard to the recirculation compressor.
Even though the exact value is not critical, it is important that the pressure is maintained constant to
facilitate temperature control. It is important to bear in mind that:
- in order to keep the gas velocity in the beds high, it is advisable not to operate at pressures
above 100 kg/cm2g (1,422 psig)
- at pressures much below 85 kg/cm2g (1,210 psig) water removal in the separators is less
efficient; which has an adverse effect on the final catalyst activity
A pressure of 85 kg/cm2g (1,210 psig) should be maintained until the activation of the second bed is
in progress under stable conditions. The pressure can be then increased to 100 kg/cm2g (1,422 psig)
within a couple of hours. Later on, during the activation of the third bed, the pressure should be
increased to 120 kg/cm2g (1,707 psig).
When the catalyst has gained some activity and the reaction has started, the pressure is maintained
constant by increasing the make-up gas into the loop and by adjusting the purge. The loop pressure
can be raised as the chiller(s) are brought in operation and the heat released from the ammonia
synthesis reaction allows an increment in the circulation rate.
11 Temperature of the catalyst

11.1 Uniform bed temperatures
Throughout the entire activation, it is important that all thermocouples are being read continuously to
ensure that the temperatures are developing symmetrically. Temperature differences should be kept
at a minimum and a careful surveillance is mandatory, particularly in the period when ammonia
synthesis starts and the loop pressure is slowly increased.
11.2 Asymmetrical activation

If significant differences among the individual readings of the temperatures at the outlet of the first
bed occur, i.e. 20–30°C (36–54°F), and these differences tend to increase, the phenomenon is
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probably due to an asymmetrical activation of the catalyst. This will happen when the ammonia
synthesis takes place faster in one part of the bed than in another.
11.3 Equalization of uneven temperatures

To equalize the uneven temperatures, the heating up rate should be reduced by increasing the
circulation rate. If the temperatures have not equalized after a couple of hours, the pressure should
be lowered to further increase the gas velocity and the inlet temperature to the bed increased. These
steps will cause the activation in the not yet activated part to progress faster and simultaneously
cause a slowdown of the reaction in the already activated part. The equalization of the temperatures
should be achieved at constant pressure after which the pressure may be increased further.
The problem is unlikely to occur, but the appropriate corrective measures are stated anyway.
12 Water formation
Most of the water formed during the activation is separated in the loop separators as aqueous
ammonia. The remainder will be found as a small impurity in the ammonia product during the first
days of operation.
12.1 Analysis of water content

We strongly recommend that the activation is followed by means of water analyses at the converter
outlet. These analyses should be initiated when the first bed inlet temperature reaches 225°C
(435°F) and concluded when the converter is lined up for normal operation.
A water analysis should be made at least every two hours, preferably every hour. The water
concentration in the gas leaving the converter should not exceed 3,000 ppmv when the catalyst
temperature is above 250°C (480°F).
12.2 Methods for water determination

Three accurate methods of determination of water in the gas outlet of the ammonia converter are
presented in Appendix 5: Gas chromatography, Ascarite and calcium carbide.
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A fourth and much simpler method is also presented in Appendix 5. This is an approximation that
should only be used if, for some reason, a more accurate method cannot be applied.
13 Activation procedure
This section contains a chronological description of the activation procedure which can be
considered as guidelines.
13.1 Activation time frame and data collection

During the activation, it is important to monitor a number of parameters such as temperatures,
pressures, flows, compositions, and water content. An example of the log sheet is given in Appendix
4.
The expected duration of the activation will be in the order of 95 hours divided among five periods as
specified in the tables below:
Table in metric units:

Hot spot temperature, Heating up rate, Pressure, Expected
Period
°C °C/h kg/cm2g duration, h
1 First bed inlet: Ambient®250 First bed 50®25 85 6
2 First bed inlet: 250®380 First bed 25®15 85 10
3 First bed outlet: 380®480 First bed max 10
Second bed outlet: 380®440 Second bed max 1-2 85®120 35
Third bed inlet: 375®420
4 First bed outlet:®500
120®Design
Second bed outlet®480 Second bed max 1-2 40
pressure
Third bed outlet®450 Third bed max 1-2
5 SUH taken out of service 4
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Table in British units:

Hot spot temperature, Expected
Period Heating up rate, °F/h Pressure, psig
°F duration, h
1 First bed inlet: Ambient®480 First bed 90®45 1210 6
2 First bed inlet: 480®720 First bed 45®30 1210 10
3 First bed outlet: 720®895 First bed max 20
Second bed outlet: 720®825 Second bed max 3-5 1210®1707 35
Third bed inlet: 710®815
4 First bed outlet:®930
1707®Design
Second bed outlet®895 Second bed max 3-5 40
pressure
Third bed outlet®840 Third bed max 3-5
5 SUH taken out of service 4
13.2 First period

The aim of this period is to heat up the catalyst to a temperature level where the activation of the
pre-reduced catalyst begins.
13.2.1 Valve positions

Before taking the start-up heater into service, the valves controlling the flow to the converter should
be adjusted as follows:
- isolation valves on the piping to the start-up heater should be fully open
- cold-shot valve should be fully closed, cf. section 9
- IHE valve(s), if present, should be cracked open, cf. section 9
- main inlet valve should be open to an extent that does not apply any restrictions in the flow
going to the converter
13.2.2 Pressure
The loop pressure should be around 85 kg/cm2g (1,210 psig) and kept at this level throughout the
heating up period.
13.2.3 Cooling
The water/air coolers should be in operation from the beginning.
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13.2.4 Circulation rate

From the beginning, the flow of the circulating gas in the loop must be kept at the highest possible
level allowed by the operation of the circulator and the above mentioned valve positions. Later on as
the heating progresses, the flow may be adjusted to match the desired heating up rate
13.2.5 Start-up heater

When the valves have been adjusted and the circulation has started and it is at its maximum, the
start-up heater can be taken into service. The start-up heater should be brought up to maximum
capacity as quickly as possible, keeping a maximum difference described in section 8.1.
13.2.6 Heating up rate

The heating up rate will be 50°C/h (90°F/h) just after taking the start-up heater into service and is
foreseen to decrease to 25°C/h (45°F/h) when approaching 250°C (480°F). The heating up rate is
controlled by adjusting the flow of the gas circulating in the loop. The flow rate is reduced by opening
the circulator by-pass valve and by closing the main inlet valve, and vice versa.
13.2.7 Heat recovery

The effluent from the converter should be kept as hot as possible until the gas has passed the hot
feed/effluent exchanger in order to maximize the recovery of the heat content of the effluent.
Therefore the boiler/BFW preheater should be operated at minimum load or even bypassed, if
possible, in the initial stages of the activation. If feasible, the boiler/BFW preheater could be kept
preheated by hot steam.
13.2.8 Bi-hourly water analysis

Water content analysis at the outlet of the converter should be started once the catalyst bed has
reached 225°C (437°F) and will continue throughout the activation.
13.3 Second period

In this period, the activation of the pre-reduced catalyst in the first bed begins and the catalyst starts
giving off water.
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13.3.1 Catalyst temperatures

The catalyst hot spot temperature will be 250°C (480°F) at the beginning of this period, increasing to
380°C (720°F) at the end of the period. The temperatures should be monitored carefully in order to
detect any asymmetrical development. If severe asymmetrical temperatures develop, these should
be corrected before the end of this period, cf. section 11.
13.3.2 Pressure
The loop pressure must be kept unchanged at 85 kg/cm2g (1,210 psig) in this period.

The circulation rate is maintained at the highest possible level and may be reduced to increase the
catalyst bed temperatures. The circulation rate is controlled primarily by the circulator by-pass and
when/if this is fully open, it may also be adjusted using the main inlet valve.
13.3.4 Heating up rate

The heating up rate is foreseen to decrease from 25°C/h (45°F/h) to 15°C/h (25°F/h) in this period.
Heating up rate must always be subordinated to the water content at the converter outlet, which
should not be allowed to exceed 3,000 ppmv.
13.4 Third period

13.4.1 First signs of reaction
When the inlet temperature to the first bed approaches 380°C (720°F), some sign of reaction in the
first bed will probably appear, evidenced by a small temperature increase across the bed. If no sign
of reaction in the first bed has been observed after a couple of hours with 380°C (720°F) at the inlet
of the first bed, the bed inlet temperature should be slowly increased towards 400°C (750°F).
13.4.2 H2/N2-ratio
During this period, the catalyst might have gained sufficient activity to start synthesizing ammonia. It
is thus important to maintain the H2/N2-ratio around 3 in order to get a stable operation without
rapidly increasing or decreasing catalyst bed temperatures. Purging well and keeping the H2/N2-ratio
of the make-up gas at 3 can ensure this.
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13.4.3 Analyses of ammonia

When ammonia formation has started, we recommend starting analyzing for ammonia at both the
inlet and outlet of the converter.
13.4.4 Cooling with chiller(s)

During this period, the strength of the aqueous ammonia will increase. When the ammonia
concentration is found to be more than 25%, the chiller(s) can be taken into operation without risking
ice formation in the chiller tubes.
13.4.5 Catalyst temperatures

The catalyst hot spot temperature will be 380°C (720°F) at the beginning of this period increasing to
480°C (900°F) at the end of the period. The catalyst temperatures in the first and second beds
should not be allowed to increase by more than 10°C/h (20°F/h) and 1-2°C/h (3-5°F/h), respectively.
At the end of this period, the first bed outlet temperature may reach 480°C (900°F), whereas the
second bed outlet temperature may be around 440°C (825°F).
13.4.6 First bed temperature control

The catalyst temperatures in the first bed are controlled by the circulation rate. When the
temperatures tend to increase too fast, the circulation rate is increased and vice versa. Typically, the
first bed inlet temperature will be maintained at around 400°C (750°F) in this period.
13.4.7 Second and third beds temperature control

The catalyst temperatures in the second bed are controlled by the flow going to the inter-bed heat
exchanger. For Topsoe’s three-bed converters (S-300 and revamped S-200 converters) with lower
heat exchanger, this is done by operating the IHE valve(s), and for Topsoe’s three-bed converters
(revamped S-200 converters) without lower heat exchanger by means of the main inlet valve. The
inlet temperature to the second bed will be 380-400°C (715-750°F) at the beginning of this period.
The inlet temperature is brought to and maintained at 410°C (750°F) for 8–10 hours.
If no sign of reaction is observed in form of an increasing bed outlet temperature, the second bed
inlet temperature may be raised to 430°C (800°F) in small steps.
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It should be kept in mind that when changing the valve positions the gas going to the converter is
diverted differently. This means that adjusting the heating up rate in one bed may also affect the
heating up rate in the other beds.
For Topsoe’s three-bed converters that are reusing the existing pressure shell from the S-200
converters, the inlet temperature to the second and third beds cannot be controlled independently,
cf. Appendices 2 and 3. In this case, one should aim at controlling the inlet temperature to the
second bed, but the inlet temperature to the third bed should not exceed 420°C (790°F).
13.4.8 Pressure
The pressure is slowly increased towards 120 kg/cm2g (1,707 psig). The pressure should be
increased stepwise by 5 kg/cm2 (71 psi). After each increase in the pressure, the operating
parameters should be allowed to stabilize. The pressure should not be increased by more than 5
kg/cm2 (71 psi) every half an hour.

The circulation rate is still maintained at the highest possible level. Simultaneously with the pressure
increase, the circulation rate may be increased in addition to what is connected with the pressure
increase. Furthermore, in order to control the first bed temperatures, it may be necessary to lower
the inlet temperature to the first bed.
13.5 Fourth period

13.5.1 Third bed inlet temperature
The inlet temperature to the third bed should be increased slowly towards 420°C (790°F), and
maintained until the first sign of reaction is observed in the third bed. At the first sign of reaction, the
inlet temperature should be slowly decreased towards the design inlet temperature, resulting in a
higher temperature increase across the third bed.
For Topsoe three-bed converters that are reusing the existing pressure shell from the S-200
converters, one should aim at controlling the inlet temperature to the third bed while being careful not
to lose the reaction in the second bed. This could happen when the inlet temperature to this bed has
dropped too much.
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13.5.2 Pressure
The pressure is slowly increased towards design pressure. The pressure should not be increased by
more than 5 kg/cm2 (71 psi) every half an hour.
13.6 Fifth period

13.6.1 Bringing the start-up heater offline
In the beginning of this period, the catalyst has gained sufficient activity to permit taking the start-up
heater out of service.
The circulation rate will be close to the maximum, the pressure about that of normal operation and
the production rate approximately 25% or more of design rate.
When taking the start-up heater out of service the temperature variations should be kept at a
minimum
13.6.1.1 Reducing the start-up heater load

The start-up heater load should be reduced in small steps to ensure that the catalyst bed
temperatures are maintained stable. No further reduction in the start-up heater load should be made
until the converter conditions are stable after each step.
The following measures may be taken to compensate for the reduction of the start-up heater load:
- raise the first bed inlet temperature slightly in order not to lose reaction
- reduce the circulation flow slightly by just opening the circulator bypass valve
- change the gas distribution at the inlet of the converter, namely in direction of more flow
through the main inlet and less flow through the start-up heater
- increase the load on the refrigeration if not already done.
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14 Interrupting the activation procedure

14.1 Avoid stagnant atmosphere
It is strongly emphasized that from the moment the catalyst starts giving off water until it has been
completely activated, it is very important to avoid a stagnant atmosphere of synthesis gas in the hot
converter. In such an atmosphere, the activation will continue, and a rather high concentration of
water vapor will cause poisoning of the part of the catalyst already completely activated. Therefore, it
is very important that a continuous forward gas flow through the converter is maintained during the
whole activation period. This gas flow carries along the water vapor resulting in the maintenance of a
low level in the converter.
If the activation has to be interrupted and flow cannot be maintained, it is necessary to lower the
temperature by 50°C (100°F) below the level reached before discontinuing the circulation. This will
cause the activation rate to slow down to a very low level so that the circulation can be stopped
without jeopardizing the catalyst activity.
If a sudden fall out of the circulation causes interruption of the flow through the converter before
temperatures have been lowered by 50°C (100°F), the synthesis should be bled off gas downstream
the converter by purging. This will create a small flow through the catalyst in the normal flow
direction, and the activation water will be carried away from the already activated part of the catalyst.
15 Notice and disclaimer

15.1 General recommendations
Haldor Topsoe engineers and scientists having knowledge of the catalyst have prepared the
recommendations contained in this manual. However, any operating recommendations should be
considered to be of a general nature, given without detailed knowledge of the customer’s plants and
with the understanding that such recommendations shall not be relied upon by the customer without
the customer’s independent verification of their accuracy and validity.
15.2 Liability
The recommendations are given without any liability on the part of Haldor Topsoe for upset or
damage to the customers’ plants or personnel. Nothing herein is to be construed as recommending
any practice or any product in violation of any patent, law or regulation.
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15.3 Advisors
Haldor Topsoe representatives present at site are solely to be considered as advisors, who are in no
way responsible for the operations manager’s duties or responsible for operating customer’s facility
in a careful and safe manner. These responsibilities remain with the customer.
We wish to underline the importance of the operating recommendations issued by Haldor Topsoe
being carefully reviewed by the plant personnel before their adoption.
15.4 Unclear points

Unclear points, if any, should be discussed and clarified with Haldor Topsoe before start of
operation.
16 Contact
For contact information, please visit our website on www.topsoe.com.
August 2016 ALEP/CADT
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Appendix 1: Control principles for S-300 without LHE
The above Control Principle is based on an S-300 converter in which it is possible to control the inlet
temperature to the first and second beds independently.
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Appendix 2: Control principles S-300 without LHE (S-200 revamped)
1st bed
TIC
1st IHE Cold bypass Valve Start-up Heater
2nd bed
2nd IHE Main Inlet Valve
3rd bed
TIC
BOILER BFW Preheater HOTEX
The above Control Principle is based on an S-200 to S-300 revamp reusing the existing pressure
shell. It is not possible to control the inlet temperature to the second and third beds independently.
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Appendix 3: Control principles for S-300 with LHE (S-200 revamped)
1st bed
TIC
1st IHE Cold bypass Valve Start-up Heater
2nd bed
2nd IHE IHE Inlet Valve
3rd bed
Main Inlet Valve
LHE
BFW Preheater HOTEX
The above Control Principle is based on an S-200 to S-300 revamp reusing the existing pressure
shell. It is not possible to control the inlet temperature to the second and third beds independently.
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Appendix 4: Log sheet sample
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Appendix 5: Water vapor in ammonia synthesis gas mixtures
I. Gas chromatography method

Scope and field of application
During catalyst activation water vapor is found in the gas leaving the ammonia synthesis converter.
Below a gas chromatographic method for determining the concentration of water vapor at the
converter outlet is described. The method is suitable for sampling and analyzing in the water
concentration range 100-10,000 ppmv in synthesis gas. The detection limit is approximately 100
ppmv of water vapor.
In Appendix 1 the Ascarite absorption method is described, which is applicable for determination of
500-5,000 ppm water vapor in a gas containing 0-25 mol % NH3.
Principle
The analysis for water vapor in gas mixtures is difficult when ammonia is present in significant
concentrations (percent). Usually columns exhibit severe tailing of ammonia, thus preventing
analysis of water in the ppm range.
This method is based on the use of Chromosorb 103 porous polymer (Johns-Manville). The unique
feature of this material is its ability to separate amines and ammonia without tailing. Since the
retention of water is greater than that of ammonia, slight tailing of water is permissible.
Apparatus
a) Sample Container: Stainless steel cylinder of a minimum volume of 500 ml (30.5 in3). Cylinders
of this type are available with a pressure range of 125 kg/cm2 g (1778 psig). The cylinder must
have two axially directed valves to facilitate flushing
b) Gas Chromatograph, using the following conditions:
Column: Chromosorb 103, 80/100 mesh, packed in 2 m long 1/8" OD, stainless
steel tubing. The column is packed with Chromosorb 103 and conditioned
at 250°C (480°F) for 8 hours with a helium flow of 18 ml/min. The column
is then carefully vibrated as the packing shrinks by the conditioning, and
the empty space is filled with Chromosorb 103. After 1 hour at 250°C
(480°F) the column is ready for use.
Carrier gas: Helium, flow 18 ml/min
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Injection: Gas sample valve (stainless steel) at 125°C (257°F), 1 ml loop
Oven: Isothermal at 140°C (284°F)

Detector: TCD at 200°C (392°F) (Hewlett Packard modulated flow type is preferred)
Sample tubing: All sample tubing for transferring the gas sample from the sample
container to the gas chromatograph must be heated to 80-100°C (176-
212°F) (using "heating tape"). The sample tubing must be made from
stain-less steel or glass (polymers absorb ammonia and water).
Procedure
Preparation
Before sampling, the cylinder must be entirely free from condensed water which would be very
difficult to remove by a mere flushing.
Initially, the cylinder is dried by heating it to 60-80°C (140-176°F) and evacuating (oil vacuum pump)
or flushing it with a dry gas for one hour at this temperature level. The cylinder can be checked for
dryness by analyzing a dry gas by the present method.
During use, as long as no water condenses in the cylinder, no further drying out is necessary. If the
sample gas contains a maximum of 3,000-5,000 ppmv of water vapor, there will be no risk of
condensation in the cylinder down to around 20°C at the normally used sampling pressure (up to
around 3.5 kg/cm2 g [498psig]).
If higher water concentrations than the above are found, if gas has been sampled at higher
pressures and/or lower temperatures than the above, or if humid air has entered the cylinder, a
recheck for dryness must be made and, if necessary, the drying process must be repeated.
Sampling Procedure
The analysis method comprises the following steps:
1. Flush the cylinder with sample gas at a high flow rate for several minutes
2. Pressurize with sample gas to around 3.5 kg/cm2 g (498 psig)
3. Disconnect the cylinder and take it to the laboratory
4. Transfer the sample gas to the gas chromatograph via heated tubing
5. Analyze by gas chromatography
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Precaution:
Always check the cylinder for dryness before use or if condensation of water is suspected, by
analyzing a dry gas.
Calibration
For sufficient accuracy of the analyses made during the activation of ammonia synthesis catalyst, the
calibration is done by means of nitrogen saturated with water vapor at a temperature of 0°C (32°F).
The calibration gas is prepared by bubbling nitrogen through a gas wash bottle containing water at
ambient temperature and thereafter passing the gas through a spiral wound glass condenser kept in
an ice bath at 0°C (32°F) before directing the calibration gas to the gas chromatograph. If a
condenser is not available, a narrow gas wash bottle may be used instead. The gas outlet from the
condenser is coupled directly to the gas chromatograph via heated tubing. A suitable flow rate of the
calibration gas is 25 ml/min (0.85 oz/min) and the pressure at which the saturation takes place can
be considered atmospheric
(PH2O = 6.11mbar [8.9psig] a at 0°C [32°F]).
Note: The water vapor percent should be independent of the nitrogen gas flow in the range 10-50
ml/min (0.34 - 1.70oz/min), if not then the condenser is insufficient. A long and narrow bottle
completely immersed in ice is necessary.
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Figure 1 GC plot for 7% mol NH3 and 1000 ppmv H2O in H2/N2
II. Ascarite method

Scope and field of application
During catalyst activation water vapor is found in the gas leaving the ammonia synthesis converter.
Below a method for determining the concentration of water vapor at the converter outlet is described.
The method is applicable for determination of 500-5000 ppm water vapor in a gas containing 0-25
mol% NH3.
Principle
The determination is made by passing a certain volume of the gas over a water absorbing agent
which is strongly alkaline and does not absorb ammonia and then weighing the amount of water
absorbed.
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Apparatus
1. Two glass U-tubes with stopcocks (see Figure 2).
Reagents
1. Ascarite-II (8-20 mesh); sodium hydroxide coated silica. It is manufactured by The Arthur H.
Thomas Company, Philadelphia, Pa., USA. An alternative reagent is Carbosorp AS (6-12
mesh), BDH Laboratory Supplies, Poole, BH15 1TD, England.
2. Paraffin oil (or any non-reactive oil, e.g. silicone oil).
3. Sulfuric acid, 2 mol/l H2SO4.
Sampling
The sample point should be placed immediately after the converter. It is important to try to keep the
sample line hot enough to prevent condensation of water vapor in it. The temperature of the gas inlet
sampling tubes should, however, not exceed 40°C (104°F).
On Figure 2 is shown a set-up for the absorption procedure. Gas from the sample connection is
passed through a rubber or polymer hose to a series of two U-tubes containing Ascarite as water
absorbing agent. The second U-tube is inserted to control the efficiency of the first U-tube. Between
the sample point and the U-tubes a line is branched off and inserted into 25-50 cm (10-20in) of
paraffin oil (this arrangement serving as a pressure controller) or the branch-off line may end in a
rubber hose clip for control of the flow. The latter arrangement, where a large by-pass flow can be
taken, is to be preferred, especially if the sample line under pressure is long and it is difficult to keep
it hot.
The gas flow is measured downstream of the U-tubes. For the protection of the gas flow meter, an
ammonia absorption bottle with 1 liter (33.8oz) 2mol/l sulfuric acid may be inserted.
Procedure
Fill the two glass U-tubes with 10-15ml (0.34-0.51oz) of Ascarite. The tubes should be equipped with
stopcocks and cleaned and dried before use. Place a layer of glass wool over the Ascarite surface to
avoid that dust is carried out of the tubes. Grease and close the stopcocks. Keep outside of tubes
absolutely clean.
Purge the line from the sample point to the U-tube connection point effectively so that a
representative gas mixture is found in the line. Retain flow and connect the two U-tubes. This will
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cause gas to go through the branch line and bubble up through the liquid. Open stopcocks. The four
stopcocks should always be opened from upstream and closed in the opposite order. Tubes are now
being purged.
Continue purging for about 10 minutes. The valve of the sample connection should be opened so
that a gas stream is going out through the pressure controller while gas is passed through the tubes,
whether this is done for purging or for absorption. The branch line should be inserted into the liquid
so as to give a flow through the U-tubes of about 2 l/min (67.6oz/min).
Then close stopcocks. Disconnect and separate the tubes. Keep flow through the sample line.
Weigh the tubes. Tubes are now ready for absorption. Purging of the tubes before weighing is done
in order to have gas of the same density in the tubes when weighing before and after absorption.
Again connect tubes to sample line. Open stopcocks. Pass gas through tubes for about 30 minutes,
corresponding to about 60 liters (2029 oz) of gas. If the gas flow rate is not high enough, increase
level in the pressure controller (4). The exact amount of gas passed through the tubes should be
measured and converted to standard conditions.
Close stopcocks. Disconnect and weigh U-tubes.
The tubes can be used a number of times without changing the Ascarite. When the amount of water
absorbed in the second tube becomes 20% or more of that absorbed in the first tube, the Ascarite
should be renewed.
If the tubes exhibit a weight loss instead of gain the Ascarite may be too humid to be used. In some
cases purging of the tubes for several hours with a dry gas re-stores the absorption properties.
As a rule the Ascarite should be procured in small packages and kept unopened until use. The
absence of color change is no indication of low humidity of the Ascarite, the color changes when
CO2 is absorbed. If, however, CO2 is absorbed, the Ascarite is definitely unfit for use.
Expression of results
The increase in weight gives directly the amount of water absorbed. Convert the amount of water
into mol water vapor and calculate the mol% of water in the gas.
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m 2 - m1
c= 18.02 × 100 mole %
B × (V2 - V1 ) m 2 - m1
+
83.14 × (273 + T ) 18.02
Where
c water vapor (mol% wet) (NH3 free basis)
m1,m2 total weight of the two U-tubes before (m1) and after (m2) the absorption (g)
B barometric pressure (mbar abs)
V1,V2 gas meter reading before and after the absorption (l)
T mean temp of the sample gas outlet the gas meter during the absorption (°C)
18.02 molecular weight of water
83.14 gas constant (mbar · l · mol-1 · K-1)
Figure 2. Set-up for the Absorption Procedure
1. Ascarite 2. Glass wool 3. Gas meter

4. Oil 5. Metal wire 6. Sulfuric acid bottle
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III. Calcium carbide method

Scope and Field of Application
This method is an alternative for the gas chromatographic determination of water in exit gas during
activation of ammonia catalyst. It is suited for determination in the range 100-5000 ppm(v/v) water in
gases containing percent amounts of ammonia.
Principle
Calcium carbide reacts with water and produces acetylene and heat. This reaction has been the
basis for several analytical applications as e.g. determination of moisture in concrete, CRD 154-77
(pressure of acetylene measured) and trace moisture in liquid ammonia, ISO 7104 (acetylene is
measured by gas chromatography).
298
CaC2 + 2 H2O(l) ¾® C2H2(g)+ Ca(OH)2 DH = – 128.4 kJ/mol
298
CaC2 + H2O(l) ¾® C2H2(g)+ CaO DH = – 62.5 kJ/mol
In this method the heat of reaction is basis for estimation of water content.
Reagents and Materials

Calcium Carbide, CaC2 0,8-1,8 mm (Merck/BDH product 979935G Calcium Carbide GPR)
Apparatus
1. Glass U-tube, as shown in figure 1
2. 2 thermometers 0-50°C (0-122°F), 0.1°C (1.8°F) graduation
3. Insulated box for U-tube
4. Flowmeter calibrated for synthesis gas.
Sampling procedure
The sample is taken from a high-pressure regulation valve close to the converter outlet. The
temperature of the valve must be sufficiently high to prevent condensation of water during expansion
of the gas for analysis. The gas then passes a cooler for conditioning to a temperature of 15-40°C
(59-104°F). After the cooler, plastic tube is used to connect to the U-tube via a flowmeter. In order to
have a quick response it is advantageous to split the gas stream before the flowmeter in a main
stream to vent and a smaller (1/10) stream to the flowmeter and analyzer.
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Procedure
1. Approximately 30 ml (1oz) of calcium carbide is added to the reaction chamber of the U-tube.
2. The two thermometers are mounted on the U-tube and the assembly placed in the insulated
box (protected from rain and direct sunlight).
3. A gas flow from the converter of 300 l/h (10145oz/h) equivalent to 5 l/min (169oz/min) is
directed through the U-tube in the direction as shown in figure 1.
4. The temperatures of the two thermometers are monitored and after 20 minutes the
temperature difference should be stable. Note: The input temperature must be below 40°C
(104°F) and appropriate cooling of the gas may be necessary.
5. The water content is calculated from the temperature difference of the thermometers, see
paragraph 7.1.
6. The carbide will change color to white when it reacts with water. Furthermore the granules
will disintegrate. The calcium carbide will last for approximately 8 hours at 3000 ppm water
content and longer at lower levels.
Expression of Results
Method of Calculation
The water content is calculated form the temperature difference:
(TEXIT-TINLET )×300 = PPM H2O
The factor 300 is empirical and depends on heat balance between the produced heat and the heat
removed by the gas and to the surroundings.
Precision
The accuracy and precision is not known as it depends on several factors in the design of the U-tube
and insulation.
Bibliography
BASF: Determination of steam content in ammonia containing gases.
ISO 7104: Liquefied anhydrous ammonia for industrial use - Determination of water content - Gas
chromatographic method.
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Figure 3 Apparatus for measurement of water
Specifications:
- Height 17cm (6.7 in)
- Diameter of reaction chamber 4 cm (1.6 in)
- Support of CaC2 layer: glass filter porosity 0
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IV. Approximation method

Following approximation should only be used if for some reason an accurate method cannot be
applied.
æ XH2O ö æ YH2O, out ö

ç ÷ = çç ÷÷
è XNH3 ø è YNH3, out - YNH3, in ø
æ XH2O ö
YH2O, out = ç ÷ * (YNH3, out - YNH3, in ) , where
è XNH3 ø
XH20 = Mol-% H2O in separator liquid*
XNH3 = Mol-% NH3 in separator liquid*
YH20, out = Mol-% H2O in converter outlet gas
YNH3, in = Mol-% NH3 in converter inlet gas
YNH3, out = Mol-% NH3 in converter out gas
*empty separator, take sample, when enough fresh liquid is available

2 Manual en Ingles Apendix 1 - Activation of KM1R and KM111 in 3-Bed Radial Flow Converter

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2 Manual en Ingles Apendix 1 - Activation of KM1R and KM111 in 3-Bed Radial Flow Converter

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8 Start-up heater (SUH) 11

8.1 SUH outlet temperature 11

11 Temperature of the catalyst 13

13.4.4 Cooling with chiller(s) 19

14 Interrupting the activation procedure 22

15 Notice and disclaimer 22

Appendix 1: Control principles for S-300 without LHE 24

Appendix 2: Control principles S-300 without LHE (S-200 revamped) 25

Appendix 3: Control principles for S-300 with LHE (S-200 revamped) 26

Appendix 4: Log sheet sample 27

Appendix 5: Water vapor in ammonia synthesis gas mixtures 28

1.2 Purpose of manual

2.2 Pre-reduced catalyst

2.3 Filling densities

- for KM1R from 2,200 to 2,500 kg/m3 (137–147 lbs./ft3)

3.1 Activation of iron oxide

The reaction taking place during the catalyst activation is:

Fe3O4 + 4H2 ® 3 Fe + 4 H2O *

* Fe3O4 : Iron (II, III) oxide

3.2 Heat of reaction

3.3 Amount of water formed during the activation

3.4 Activation schedule

5.3 Establishing make-up gas addition and purge

5.4 Early stage of the reaction

5.5 Ammonia concentration at the inlet of the converter

5.6 Water concentration at the inlet of the converter

5.7 Oxygen equivalents and other poisons

Oxygen equivalents = (Concentration of CO) * 1 + (Concentration of CO2) * 2

Oxygen equivalents = (1.0) * 1 + (2.5) * 2 = 6.0

6.1 Water/air cooler

6.2 Refrigeration chillers

6.2.1 Sampling of aqueous ammonia

6.2.2 Refrigeration compressor

7.1 Circulation rate

8 Start-up heater (SUH)

8.2 SUH maximum load

9.1 Main inlet

9.2 Pressure shell and converter outlet temperature limits

9.3 Cold shot and inter-bed heat exchanger (IHE) valve(s)

11 Temperature of the catalyst

11.2 Asymmetrical activation

11.3 Equalization of uneven temperatures

12.1 Analysis of water content

12.2 Methods for water determination

13.1 Activation time frame and data collection

Table in metric units:

Table in British units:

13.2 First period

13.2.1 Valve positions

13.2.4 Circulation rate

13.2.5 Start-up heater

13.2.6 Heating up rate

13.2.7 Heat recovery

13.2.8 Bi-hourly water analysis

13.3 Second period

13.3.1 Catalyst temperatures

13.3.3 Circulation rate

13.3.4 Heating up rate

13.4 Third period

13.4.3 Analyses of ammonia

13.4.4 Cooling with chiller(s)

13.4.5 Catalyst temperatures