Tenth Stamicarbon

Urea Symposium 2004

Paper 3

Safurexâ : A dream comes through

Authors:
Maria Hugosson, Sandvik Materials Technology
Jo Eijkenboom, Stamicarbon
10th Stamicarbon Urea Symposium
10 - 13 May 2004, Scheveningen

Table of Contents
Page:
1. Abstract .......................................................................................................................2
2. Introduction..................................................................................................................3
3. Development of several Duplex grades ending in Safurexâ ........................................4
4. Quality requirements ...................................................................................................5
5. Mechanical properties .................................................................................................7
6. 475°C embrittlement....................................................................................................8
6.1 Base Materials .......................................................................................................8
6.2 Weld deposits ........................................................................................................8
7. Safurexâ welding .........................................................................................................9
8. Design consequences ...............................................................................................10
8.1 Liners ...................................................................................................................10
8.2 Heat Exchanger tubes..........................................................................................12
8.2.1. HP Stripper, HP Carbamate Condenser and HP Scrubber tubes.................12
8.2.2 Heat exchanger tubes for Pool condenser / Pool reactor ..............................14
9. Side effects when using SafurexÒ..............................................................................15
9.1.Tubesheet thickness ............................................................................................15
9.2. Bellows design ....................................................................................................15
10. HP piping .................................................................................................................16
11. Miscellaneous products ...........................................................................................19
11.1 Forgings .............................................................................................................19
11.2 Plates .................................................................................................................19
11.3 HP Piping bends ................................................................................................19
11.4. HP Pipe flanges ................................................................................................20
11.5 Valves and accessories .....................................................................................21
12. In plant test results of Safurexâ ..............................................................................23
12.1 HP Carbamate Condenser in the El Delta Urea Plant........................................23
12.2 The HP Carbamate Condenser in the Police Urea Plant, Poland. .....................23
12.3.1. HP Stripper in the UF-2 DSM Urea plant....................................................24
12.3.2. Liquid distributors in Ultrafertil, Brazil Stripper............................................24
13. Practical experience with equipment fabricated in Safurexâ...................................25
14. Safurexâ in oxygen free carbamate solution...........................................................26
15. Safurexâ in oxygen reduced carbamate solutions ..................................................27
15.1 Shiraz Urea Plant, Iran.......................................................................................27
15.2 Profertil’s urea plant, Argentina..........................................................................27
15.3 HP Stripper in the Shiraz Urea plant ..................................................................29
15.4 Exposure test of SafurexÒ in a Snamprogetti designed plant.............................30
16. Future developments...............................................................................................31
17. Economical consequences ......................................................................................32
18. Conclusions .............................................................................................................33

All technical and other information contained herein is based on general Stamicarbon/DSM experience and within this limit is
accurate to the best of our knowledge. However, no liability is accepted therefor and no warranty or guarantee is to be inferred.

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1. Abstract

In 1992 Stamicarbon and Sandvik met to discuss a new material to be developed for
use in urea plants. Following goals were set:

· Good corrosion resistance to carbamate solutions containing little or no oxygen.

· At least the same corrosion resistance to oxygen containing carbamate solutions as

X2CrNiMoN 25 22 2 (A4-18005 BC.05).

· High resistance to Chloride stress corrosion cracking (S.C.C.).

· Good microstructure stability.

· Good weld ability.

10 years later, after successful research and development and elaborate experiments
and in plant experiences, the conclusion is that all goals have been realized and that
this material has even gone beyond our expectations. SafurexÒ (Stamicarbon A-4
18005 type BE.06) is a duplex stainless steel grade exclusively developed by Sandvik
for the Stamicarbon urea and melamine process.
This paper reviews the development and shows the success of SafurexÒ. Since 1997
several SafurexÒ HP heat exchangers have been fabricated successfully. At this
moment a plant is under construction whereby the complete synthesis is made from
SafurexÒ.

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2. Introduction

In 1992, both Stamicarbon and Sandvik met for their annual meeting in which ongoing
developments with respect to material, weld deposits and corrosion aspects in the field
of urea were discussed and experiences were exchanged.
In that particular meeting, the idea to use a duplex as alloy protection was discussed.
Stamicarbon indicated that it should be possible to design a urea plant that could run
without oxygen using duplex material as alloy protection.

In practice, it was already proven that duplex alloys in urea application showed good
corrosion resistance and that it should in theory be possible to develop a Duplex
Stainless Steel that would meet that demand.

A fore cast of the needed alloying elements was indicated and goals were set. The
development of the material should finally result in a material that would show following
objectives:

· Good corrosion resistance to carbamate solutions containing little or no oxygen.

· At least the same corrosion resistance to oxygen containing carbamate solutions as

X2CrNiMoN 25 22 2 (A4-18005 BC.05).

· High resistance to Chloride stress corrosion cracking (S.C.C.).

· Good microstructure stability.

· Good weld ability.

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3. Development of several Duplex grades ending in Safurexâ

In order to find the right material composition and to ensure the reproducibility of the
material some 20 different heats were made in a laboratory high frequency furnace. The
first discrimination was done on bar and tube samples.
In first instance, it was agreed to check the quality from corrosion point of view with the
Huey test and the Streicher test.

Laboratory examinations and field tests led to the following conclusions:

· Several heats contained too many slag inclusions, resulting in an inferior
microstructure. The sulphur and oxygen concentrations were too high as a result
of the steel making procedure and there was no optimum tuning of the ferrite and
the austenite-forming alloying elements in combination with inadequate heat
treatment. As a result, the reproducibility was inadequate.

· Low-nitrogen grades showed precipitation of intermetallic phases. No

intermetallic phase was found in the high-nitrogen (0.40%) grades.

· The heats that had a homogeneous microstructure and a low level of impurities
exhibited good corrosion resistance in the Huey test, the Streicher test and in
field tests

· Samples, selectively attacked in the Streicher test also showed selective attack
in the field test. The Huey test was not showing any selective attack in parallel
samples. These observations were for us reason to use the Streicher test as the
quality test.

· Stress corrosion cracking experiments showed superior resistance to all other

duplex material.

· A field test in a HP Stripper of a urea plant indicated that the corrosion

performance of SafurexÒ is at least comparable with that of BC.05 material.

· Weld ability proved to be good, microscopic examination revealed an acceptable

microstructure of the welds and the heat-affected zones.

· The structure stability was tested and confirmed to be stable under critical
conditions.

Out of the test results, the optimum alloy composition was selected; this material was
named SafurexÒ. In the subsequent years only slight improvements in the composition
were made. To date, SafurexÒ does not differ from the heat produced in first instance.
The first produced commercial SafurexÒ heat is now present in urea equipment and
proves to be of excellent quality in urea/carbamate solutions.

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4. Quality requirements

SafurexÒ should meet the following requirements:

· Homogeneous ferrite-austenite microstructure consisting of a ferrite matrix with

austenite islands fully enclosed by ferrite. Its homogeneity to be tested with help of a
eddy current test developed by Stamicarbon, see photo 1.

Photo 1. Homogeneity record Photo 2. Typical microstructure.

· Ferrite content to ASTM E 562, Point Counting.

o Base material: 40-60%

o Weld deposit and HAZ: 30-70%

The use of a Ferrite scope appears not to be practical. Unreliable figures will appear.
The philosophy is that in case of base materials Point counting will be done and when
welding, the Ferrite content of the Procedure Qualification Welding (PQR) will be
checked for its ferrite content by Point Counting and in the mean time also the correct
microstructure will be ensured.
Subsequent, welding should be done in accordance with the weld parameters as used
in the procedure qualification welding.

· Streicher test to Stamicarbon Specification A4-71112

o Overall attack: ≤ 0.7 gr/m2/hr

o Selective attack: ≤ 100 µm

It was learned that the execution of the standard ASTM Streicher test gave rise to many
discussions. For that reason, we have developed our own Specification for Streicher
testing.

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In order to have comparable results, the test should only be executed as per this
specification. The quality of the various SafurexÒ products proves to be very stable.

The material is recognized in the ASME system under UNS 32906 and applied as per
ASME Code Case 2295.

Following product standards are applicable:

· Tubes A-789
· Plate A-790
· Bar A-479
· Pipe A-240

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5. Mechanical properties

The mechanical properties are unambiguously better than any other alloy protection in
use in urea plants so far.

Table 1. Mechanical properties

Material Yield strength Tensile strength Elongation A5 Thermal Module of

Temp. °C Rp 0.2 (Mpa) Rm (Mpa) (%) Expansion* Elasticity
20 / 225 20 / 225 20 / 225 10-6/°C N / mm2 at
20 / 225 225°C
20 / 225
â
Safurex 650 / 465 800 / 717 > 25 11.5 / 11.5 184
BC.01 190 / 135 490 / 412 > 40 16.5 / 16.5 184
BC.05 270 / 195 580 / 495 > 30 16.5 / 16.5 184
C. Steel 248 / 202 482 / 482 > 16 12.5 / 12.5 190

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6. 475°C embrittlement

6.1 Base Materials

The susceptabity of SafurexÒ against
475oC has been further examined.
Known is that the structure stability of
duplex stainless steels at
temperatures around 475oC is limited
due to decomposition of the ferrite phase
and thus the toughness declines. This is
not a problem that will occur during urea
production but, it means that precautions
have to be taken when fabricating
SafurexÒ equipment.

Figure 1. 475°C embrittlement base metals

6.2 Weld deposits

Weld deposit has also been reviewed.
In order to check its ductility at plant
operating temperature, overlay welded
Safurex® was exposed to a heat treatment
of 4000 C for 20 hours. After that impact
testing was done at subsequently ambient
temperature, 100°C, 200°C, 240°C
and 280°C.
The conclusion from these experiments
is that the weld metal is embrittled after
a heat treatment of 400°C during 20 hours
at ambient temperature. As was confirmed Figure 2. Toughness of Safurexâ weld deposit
in the tests executed at base materials.

At 100°C, the toughness is on the low side while at operating conditions the ductility is
secured as can be learned from figure 2; the toughness is fully OK using 27 Joule is
applied as the lower limit.
Besides the mechanical aspects, also the corrosion resistance is of importance.
Investigations show that the corrosion resistance of Safurex® decreases if the material
is exposed to temperatures of 4000 C for more than 15hours.

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7. Safurexâ welding

Safurex® can be welded with the commonly

known and commercial available welding
processes. Welding is less critical than
welding austenite materials.
To maintain the microstructure in overlay welds,
a welding flux has been developed for
Electro Slag Welding (ESW)

In the mean time it is proven that Safurex®

can be welded without the addition of filler
wire, while maintaining the mechanical
properties and showing excellent corrosion
behavior. This proof is essential for Photo 3. Internal bore weld
Stamicarbon since welding of Safurex®
without filler wire is a must; it allows internal
bore welding (IBW) to connect the U-bundle
to the tubesheet crevice free.

The experience with the first ever Pool Condenser in SafurexÒ welded confirms this
statement. This Pool condenser has 1,202 U-tubes. In total 2,404 IBW weld were made,
after some initial fine tuning, the number of repairs did not differ from IBW welds made
in BC.05 materials.
It is also important to recognize that, in spite of the fact that this was the first time that
SafurexÒ IBW welds were made in production, the welding was completed in 41 days.
This figure is in line with IBW welds in BC.05 material.

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8. Design consequences

The use of Safurex® as construction material has a positive impact on the design of the
equipment. Due to the lower corrosion rates and the higher mechanical properties the
following main items have been changed in detail but with large consequences.

8.1 Liners
Liners in Stamicarbon Urea plants were typically specified in A4-18005 BC.01
(316 L Urea Grade) material. Since the liner is not part of the pressure vessel, its
thickness should be enough to obtain a reasonable life time and to operate the
equipment in a practical way. Stamicarbon specifies that the limitation with respect to
the lifetime of the liner is the risk for buckling (as a result of difference in thermal
expansion between the construction materials used) in combination with the overall
corrosion during operations.

Figure 3. Advised liner thickness in relation to equipment diameter

Liner thickness v. Equipment diameter

Liner thickness [mm}
14
BC.01
12

10
BC.05
8

4
Safurex®
2

0
1,000 1,500 2,000 2,500 3,000 3,500 4,000 4,500

Diameter [mm]

On top of the strength calculation, a corrosion allowance of 2-mm was added in order to
obtain an acceptable lifetime of a BC.01 liner. Finally, the thickness was adapted to
commercial available thicknesses.

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Subjecting SafurexÒ to the design criteria, taking in mind the high mechanical properties
in combination with the good corrosion resistance of Safurex® and the fact that the
thermal expansion coefficient of SafurexÒ is identical to that of Carbon steel, allowed us
to specify a liner thickness of 4-mm for all conditions resulting in a corrosion allowance
of plus 3-mm.
Table 4 shows the difference in liner thickness comparing two materials.
A corrosion rate of 0.1-mm per year on stream for BC.01 liner while for the SafurexÒ
liner a corrosion rate of 0.05-mm was taken into account.
The diameter of the reactor in this example was 3,000-mm.

Lifetime in relation to minimum liner thickness

Expected
Thickness inclusive
Minimum required Thickness liner
Materials corrosion allowance,
thickness, mm advised, mm life time,
mm
years

6.63 8.63 9 34
BC.01

0.34 4 4 > 50
Safurexâ

The consequence is a reduction in material cost for the liner of some 35%, while the
lifetime of the liner is more than doubled. This is made visible in figure 4.

Figure 4. Liner thickness versus lifetime

4
BC.01 BE.06
3
Over thickness liner, mm

0
Year

11

14

17

20

23

26

29

32

35

38

41

44

47

50

53

56

59
2

-1

-2

-3
Year Onstream

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8.2 Heat Exchanger tubes.

The minimum wall thickness of the heat exchanger tubes is specified by the applicable
design code. The chosen wall thickness of heat exchanger tubes is defined by the
corrosion rate in relation to the expected life time of the heat exchangers. When
selecting the wall thickness, also the reliability of tube-to-tubesheet welding has been
considered.

8.2.1. HP Stripper, HP Carbamate Condenser and HP Scrubber tubes.

Was in the past a wall thickness of nominal 3-mm for a HP Stripper and nominal
2.5-mm for a HP Carbamate Condenser and HP Scrubber specified, with the arrival of
SafurexÒ the thickness of the Stripper tubes has been adapted. The use of SafurexÒ
has serious but positive consequences for the life time of the heat exchangers .

For plant operations the minimum design wall thickness is not of interest. Important are
the actual operating pressure and temperature in order to determine when a tube
should be plugged.
Such calculation method has however to be accepted by the local authorities. This
method can only be used if, in its lifetime no pressure test conditions based on design
conditions are mandatory by the authorities.

The following tables show the difference.

Table 2. Miminum tube wall thickness in relation to the materials and tube dimensions
as per ASME VIII, div.1, Pressure 160 bar.

Material
Outer diameter
BC.01, mm BC.05, mm Safurex® , mm

na 1.71 1.00
31-mm, T 2250C

2.20 1.31. 0.85

25-mm, T 1900C

For plant operations a different wall thickness is conclusive. The advised minimum
allowable wall thickness of the heat exchanger tubes when checked by eddy current,
based on operating conditions can be learned from table 3.

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Table 3. Miminum tube wall thickness in relation to the materials and tube dimensions
under operating conditions, pressure 145 bar.

Material
Outer diameter
BC.01, mm BC.05, mm Safurex® , mm

na 1.45 0.70
31-mm, T 2140C

1.50 1.00 0.50

25-mm, T 1870C

The high mechanical properties of SafurexÒ result in a low minimum wall thickness, this
in combination with the allowance enables the use of HP Stripper tubes, with a wall
thickness of nominal 2.5-mm compared to 3-mm in BC.05 material.

The net effect of the reduction in wall thickness of 0.5-mm compared to the wall
thickness specified in BC.05 material is a longer lifetime as shown in figure 5.
An additional advantage is that the reduction in tube wall thickness results in a larger
inner diameter of the heat exchanger tube improving the heat exchange performance
and in turn having an impact on the dimensions and finally on the weight of the
equipment.

Figure 5. Lifetime HP stripper tubes

2 .5

2 B C.05 B E.06

1 .5
Extra wall thickness, m

0 .5

0
Year

11

23

32

41

44
2

14

17

20

26

29

35

38

47

-0 .5

-1

-1 .5

-2

-2 .5

-3

Years On strea m

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8.2.2 Heat exchanger tubes for Pool condenser / Pool reactor

Significant advantage using SafurexÒ is achieved in the Pool condenser/Pool reactor.
Critical in the fabrication of a Pool condenser/Pool reactor is the tube-to-tubesheet
welding of the U-bundle which is done with internal bore welding (IBW).
It is universally known that this welding technique is a very reliable way of welding tubes
to a tubesheet when executed correctly. Important in this aspect is the ratio between
tube diameter and tube wall thickness. Due to the high mechanical properties of
SafurexÒ the wall thickness of the tubes will remain in the for IBW peRFTt range
dictated by the diameter in relation to the wall thickness range, being between 2 and 3
mm. The difference in wall thickness for different materials can be learned from table 4.
Bear in mind that the tubes need to be bended and that due to this bend a reduction of
wall thickness takes place, the following wall thickness have to be considered. The
smallest radius in the U-bundle will be R= 85-mm, with this radius one remains below
the cold deformation limit of 15%.

Table 4. Wall thickness U-tubes

Material
Wall thickness
BC.05, mm Safurex® , mm

1.45 0.70
31-mm, T 2140C

1.00 0.50
25-mm, T 1870C

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9. Side effects when using SafurexÒ

When using SafurexÒ, additional savings in the design of equipment are possible,

9.1.Tubesheet thickness
The higher mechanical properties of the heat exchanger tube leads also to a reduction
in tubesheet thickness. When calculating these tubesheets in accordance with the
Standards of the Tubular Exchanger Manufacturers Association TEMA, a reduction of
some 25 % in thickness is achieved.

9.2. Bellows design

HP Heat exchangers are provided with "Flanged and Fluid" expansion joints to
compensate for the difference in thermal expansion between the different materials
present in the shell side. The calculation is based on the axial deformation. The bellows
also have to compensate for stresses during operations. Since the thermal expansion
coefficient between C. steel and Safurex® is almost identical, the bellows design can be
simplified.

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10. HP piping

Large savings are achieved in HP piping.

In addition, the diameters of the pipes
available in Safurex® are bigger than
available in the BC.01 or BC.05 quality.
Presently, the maximum diameter available
in the austenite material is up to 14".
In this diameter, the length of the pipes is
limited to some 2 until maximum 3 meters.
In Safurex®, the maximum sizes are far
larger; dia. 18" pipe has been made
commercially.
Photo 4. HP Pipe, size 14"

Due to the high mechanical properties,

different schedule can be used.
This has a large effect on the wall
thickness leading to
· Downsizing of the pipe.
· Longer pipe lengths.
· Fewer welds are needed in the
HP piping.
· Less welding time and welding
consumables.
· Less inspection costs.
· Less expansion loops.
· No tracing or jacketing Photo 5. Bended Safurexâ piping
· Less sensitive for atmospheric corrosion.

The use of a lower schedule has a big impact on the weight of the HP Piping as can be
learned from table 5.

Table 5. Weight comparison of 12" HP piping

Material type Schedule Wall thickness, Weight, Kg/mtr

mm
BC.01 160 33.32-mm 293
BC.05 120 25.40-mm 187
Safurexâ 80 17.48-mm 132

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Not only the schedule will be different, but also the pipe size can be down scaled. This
is possible at sizes of 12” and more. The inner diameter of the tubes changes
dramatically; then, one pipe size less can be used and still having the same internal
pipe surface as can be learned from table 6.

Table 6. Down sizing of HP piping

Size, " OD Sch.160 ID, mm Sch.80 ID, mm Delta, mm Delta - 1 size

6 168.3 18.26 131.8 10.97 146.4 14.6
8 219.1 23.01 173.1 12.7 193.7 20.6
10 273 28.58 215.8 15.09 242.8 27
12 323.8 33.32 257.2 17.48 288.8 31.7 4.6
14 355.6 35.71 284.2 19.05 317.5 33.3 -7.9
16 406.4 40.49 325.4 21.44 363.5 38.1 -3.2
18 457.2 45.24 366.7

These tables are typical pipe sizing for a 3,250 mtpd tons Pool condenser Urea plant.

All these advantages are having a large consequence on the HP Piping. For a typical
3,250 mtpd plant, the consequences have been listed in tables 7 & 8.

Table 7. BC.01 piping Table 8. Safurexâ piping

Size Qty (mtrs) Weight Size Qty (mtrs) Weight

(kgs) (kgs)
3/4"-sch160 5.5 16 3/4"-sch80 5.5 12
1"-sch160 5.5 23 1"-sch80 5.5 18
11/2"-sch160 5.5 40 11/2"-sch80 5.5 30
2"-sch160 5.5 62 2"-sch80 5.5 42
3"-sch160 5.5 119 3"-sch80 5.5 85
4"-sch160 5.5 187 4"-sch80 5.5 125
6"-sch160 5.5 377 6"-sch80 5.5 238
8"-sch160 66 7,461 6"-sch80 66 2,860
10"-sch160 11 1,925 8"-sch80 11 721
12"-sch160 11 2,666 10"-15,1 mm 11 1,073
14"-sch160 55 15,372 12"-17,5 mm 55 7,380
16"-sch160 11 4,080 14"-19,0 mm 11 1,762
Total: 32,328 16"-21,4 mm 0 0
Total: 14,346

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From these tables it is obvious that a weight saving of more than 50% is achieved and
that the costs as a consequence thereof are reduced by a factor 2.5.

Also the other piping components have the same type of savings.

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11. Miscellaneous products

The fact that Stamicarbon designs a full SafurexÒ Synthesis leads to the request to
Sandvik to deliver product shapes that are not in the delivery program of Sandvik.
For that reason other specialized fabricators were approached to deliver product forms
needed. Sandvik has exclusive supply agreements with these companies. In order to
ensure the quality of these products, Sandvik does market these products and tests
these materials as per the Stamicarbon specifications.

These products are:

11.1 Forgings
The availability of forgings required to
manufacture in an economical way
products has been guaranteed in that
several forging mills have an agreement
with Sandvik to forge for them the
requested shapes. All however under
strict control and via Sandvik.

Photo 6. Forging

11.2 Plates
Since 1998 plates in SafurexÒ have been produced. These plates are fabricated by
Industeel. The responsibility and quality assurance and Quality Control is in hands of
Sandvik

11.3 HP Piping bends

HP Piping is made by Sandvik, the pipe
diameter is unlimited, and up to 18” pipes
have been produced. Bending these
pipes is a different story. Also here two
specialized companies deliver induction
bended bends in SafurexÒ. As said before
the quality is Sandvik’s responsibility.

Photo 7. 16" pipe bend

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11.4. HP Pipe flanges

With the use of SafurexÒ the possibility is there to simplify the flange connections in HP
piping. This new design is not only cheaper but makes also the bolting of these flanges
easier and less sensitive for leaks and crevice corrosion.
A joint research programme between Sandvik, LTS and Stamicarbon has led to the
development of a for the urea industry new type flange connection, the TECHLOCK
clamp type connector. This connector is well proven in the oil industry and can be used
in the urea field only if made of SafurexÒ. Photo 9 shows the difference between a
conventional flange connection and a TECHLOCK connector.

Photo 8. Details of Techlock connector Photo 9. Difference in size, typical 4"

The cost for the connectors in a typical 3,250 mtpd tons urea plant is only some 55%
compared with ANSI flanges with Lens ring joints

A 4” pipe connector was installed in the outlet pipe line of the HP carbamate pump of a
Stamicarbon urea plant. After 6 months in service the connector was opened and
inspected. An inspection after dismantling showed the connector as being not used at
all. No corrosion was found at the SafurexÒ mating faces of the flanges and seal ring.
The seal ring has been replaced by a new one and the used seal ring is now with
Stamicarbon.

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The advantage of this joint is cost savings but of more in importance is the savings on
maintenance costs and the reliability of this joint.

Photo 10. In use

11.5 Valves and accessories

For valves and other accessories, special forgings are needed. In dialogue with the
vendors of these products, forge mills were approached and deliver the requested
forgings.

SafurexÒ has achieved a major advantage

in the reliability and maintenance of valves.
In the past sealing problems were common
and accepted. Maintenance was expensive
since refurbishing of the stem seat was
necessary. This refurbishing meant to replace
the seat or to mill the seat SafurexÒ has
made a simpler valve design possible since
the risk for crevice corrosion in not existing.
With the application of SafurexÒ also the
material selection for a valve is now optimal.
So far, the valve body was made from BC.01
or BC.05 material while the stem was made
from duplex material. This in order to obtain
the desired difference in hardness between seat
and stem and the required stiffness of the stem.
This resulted in wear of the valve seat and thus
expensive maintenance. Photo 11. 12" Safurexâ valve

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The design of a SafurexÒ valve is such that the body will be made from SafurexÒ and
the spindle can be made from a normal 22.05 (BE.03) duplex material. The
consequence of this will be that maintenance in the future will be such that only the
stem has to be replaced.

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12. In plant test results of Safurexâ

Inspections have been performed of Safurex® equipment installed in commercial plants.

The inspections performed, confirm the results of the previously performed laboratory
tests; the corrosion rates are low, comparable and or lower than the rates found when
using BC.05 material.

Below a review of the findings so far.

12.1 HP Carbamate Condenser in the El Delta Urea Plant

The HP Carbamate Condenser in the El Delta plant in Egypt was the first ever build
equipment in full Safurex® and was inspected after 932 days on stream; the findings
were as follows,

· The Safurex® overlay and liner reveal a peRFTt corrosion behavior, no sign of
any corrosion was observed.
· The remote field eddy current measurements (RFT) did not show any corrosion
in the tubes; the findings matched those of the base line measurements executed
when building the equipment.

12.2 The HP Carbamate Condenser in the Police Urea Plant, Poland.

An inspection took place after 289 days on stream; the findings were as follows,

· The inspection did reveal a perfect

corrosion behavior of the tube, plate
and overlay components.

· The remote field eddy current measurements

(RFT) did not indicate any decrease of
wall thickness in the heat exchanger tubes
compare with the base line measurements
performed during the manufacturing of the
equipment; the corrosion rate nears zero.
Photo 12. HP carbamate condenser
after 289 days on stream

12.3 Safurex® in HP Strippers.

In the HP Stripper the most critical conditions from corrosion point of view are present.
Before specifying any Safurex® for HP Strippers numerous tests, experiments and
investigations were successfully executed. Also over those last years, a lot of
information about the material under stripping conditions has been obtained and the
results meet the expectations. Below one finds a summary of the findings of Safurex® in
HP Strippers.

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12.3.1. HP Stripper in the UF-2 DSM Urea plant

The DSM stripper was build when Safurex® was still in full development. In spite of the
fact that SafurexÒ was not yet approved, three tubes from the first ever made Safurex®
heat were installed in this Stripper.
In March 1999 after one year of production and in 2001 after some three years of
production, the HP Stripper was inspected. During these inspections each time a
Safurex® heat exchanger tube was removed for further investigations. The tubes were
removed after an Remote Field Eddy Current wall thickness test

The tubes have been extensively examined by both Stamicarbon and Sandvik. The
results of this investigation can be summarized as follows,

Wall thickness measurements by remote field eddy current method.

The remote field eddy current (RFT) measurement executed in 1999 indicated a
corrosion rate of 0.07 mm per year; this was identical with the corrosion measured in
the BC.05 heat exchanger tubes. It can also be stated that the area in which the
corrosion occurs is identical with the area in which the BC.05 tubes show wall thickness
decrease, the top three meters of the heat exchanger tubes. In 2001, the wall thickness
measurements were repeated. Evaluating the records it can be stated that the corrosion
rate measured in the Safurex® tubes was reduced to 0.05 mm per year and that the
corrosion rate in the other BC.05 tubes was measured in average 0.07 mm per year as
expected.

Metallurgical examination.
After the Remote Field Eddy Current measurements, the Safurex® heat exchanger
tubes were metallurgical examined. The protruded tube ends showed a smooth surface.
The area influenced by corrosion is identical with the area as found for the BC.05 tubes.
(Upper 3 meter of the heat exchanger tube). It was also observed that the overall
corrosion proceeds via the austenite phase. The wall thicknesses as measured by RFT
technique were confirmed.

12.3.2. Liquid distributors in Ultrafertil, Brazil Stripper

An inspection of this plant after 853 days
on stream. Did not show any corrosion of
the SafurexÒ liquid distributor system.
The Delta_P test of the liquid distributor
holes gave identical figures as during the
final inspection of the Stripper at the
fabricators shop.

Photo 13. Used liquid distributor

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13. Practical experience with equipment fabricated in Safurexâ

It is commercial proven that HP equipment in Safurex® can be fabricated using

conventional techniques at lower costs than when using other materials. At this moment
several HP components have been made in Safurex® of which many are in operation as
can be learned from the table below.

1997
• HP Scrubber: DSM Holland

1998
• HP Carbamate Condenser: El Delta, Egypt
• HP Carbamate Condenser: Police, Poland

1999
• HP Stripper: Agrium, Canada
• HP Carbamate Condenser: Petfurdo, Hungary

2000
• High efficiency reactor trays: Shiraz, Iran

2001
• HP Stripper: Shiraz, Iran
• HP Carbamate Condenser: Razi, Iran
• Siphon Jet reactor trays: SKW, Piesteritz Germany
• HP Carbamate Condenser: El Delta, Egypt
• HP Carbamate Condenser: Dneproazot, Ukraine

2002
• Siphon Jet reactor trays: SKW, Piesteritz Germany
• HP carbamate Condenser ABF, Malaysia
• HP Stripper ABF, Malaysia
• HE-trays: ABF, Malaysia
• Several (control) valves Agrium, Canada
• HP Control valve ABF, Malaysia
• HP pipe lines Agrium, Canada
• HP Stripper Asaluyeh, Iran
• Poolcondenser Asaluyeh, Iran
• Reactor Asaluyeh, Iran
• HP Scrubber Asaluyeh, Iran

2003
• Siphon Jet reactor trays: SKW, Piesteritz Germany
• HP Stripper SAFCO, Saudi Arabia
• Poolcondenser SAFCO, Saudi Arabia
• Reactor SAFCO, Saudi Arabia
• HP Scrubber SAFCO, Saudi Arabia
• HP Piping SAFCO, Saudi Arabia
• Valves & accessoiries SAFCO, Saudi Arabia
• Siphon Jet Reactor trays: ABF, Malaysia
• HP Piping ABF, Malaysia
• HP Piping Reactor- HP Scrubber Agrium, Canada

2004
• Reactor: QAFCO, Qatar
• Siphon Jet reactor trays QAFCO, Qatar
• HP Stripper SAMAD, Saudi Arabia
• PoolReactor NINGXIA, P.R. China
• HP Stripper NINGXIA, P.R. China

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14. Safurexâ in oxygen free carbamate solution

The most challenging goal is to produce urea in an oxygen free urea plant by using
Safurex®. Numerous tests conducted under laboratory conditions show indeed that
Safurex® remains passive under oxygen free conditions.
The tests have been conducted with carbamate solutions at Urea reactor conditions
temperature 1830C and up. The results of this test are shown in table 9..

Table 9. Results in oxygen free carbamate

Material type Corrosion, mm / year Selective attack, mm

Safurexâ 0.03 5

The behavior of different materials which can be used in the HP Synthesis when using
oxygen to passify and the effect when reducing the oxygen content can be learned from
figure 6. It shows clearly that all known materials so far cannot maintain their passivity
and high (and active or transpassive) corrosion is the result. Only Safurex® shows no
reaction when lowering the oxygen content. The corrosion rate remains constant.

Figure 6. Behavior of typical materials in oxygen free carbamate solutions

100
BC.01
BC.05
SAF 2205
Safurex®
Corrosion mm/year

10

1
0.0 0.1 0.5 1.0 10.0 100.0

0.1

0.01
PPM Oxygen

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15. Safurexâ in oxygen reduced carbamate solutions

15.1 Shiraz Urea Plant, Iran

In the mean time, we will be testing the lower oxygen content down to 0.3% in a
commercial Stamicarbon 1,500 mtpd Stripping Urea plant in Iran.
This test became possible since the HP stripper was in SafurexÒ, while the HP
carbamate Condenser had a BC.05 alloy protection.
If the test is completed a presentation about the test will be given during this
symposium.
Also other experiences with lower oxygen concentrations are available and operating
under more severe conditions than present in Stamicarbon Urea plants.

15.2 Profertil’s urea plant, Argentina

Besides process performance the advantages of Safurex® above other construction
materials can be learned from this HP Stripper, build already in 1999.
The decision to build this HP Stripper in Safurex® was taken, because this heat
exchanger was made considerable larger than required for the plant capacity. The
larger HP Stripper was selected because replacement of the HP Stripper was part of a
plan to increase the plant capacity considerably.

The consequence of this large HP Stripper, operating at current (low) capacity would be
that a uniform liquid distribution could not be achieved (turn down ratio). An irregular
distribution would lead to heavy corrosion of the heat exchanger tubes, resulting in
serious damage to the Stripper if BC.05 heat exchanger tubes would be installed.

This Stripper was never installed in the plant were it was designed for.
Presently this Stripper is operating in the Profertil plant in Argentina. In April 2003, it
replaced the Snamprogetti stripper that failed due to heavy corrosion problems which
caused the plant to shut down very frequently.
With the Stamicarbon Safurex® Stripper the plant is now in operation since beginning
May 2003. The stripper runs at the desired load to full satisfaction. The stripper bottom
temperature is 204.5 0C and the total oxygen fed as air to the synthesis is 0.45 % of the
CO2 feed to the synthesis. This air is partially fed into the bottom of the HP Stripper.

Stamicarbon performed an inspection of this HP Stripper in March 2004. The results are
impressive as can be learned from the inspection results,

On stream 292 days,

Top temperature 188 0C
Bottom temperature 204.5 0C

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Both the channels are lined, no corrosion could be observed.

An impressive behavior of SafurexÒ was found on the liner of the top cover. Although
the lifting trunnion was not removed and thus causing a large cold spot, no
condensation corrosion was found in the liner below, see photo’s 14 & 15.

Photo 14. Top cover with lifting lug Photo 15. Liner surface of top cover

The tubes in the top tube sheet and the tube-to-tubesheet welds are as new, no sign of
any corrosion could be observed in the tube ends in spite of mal distribution and taking
into consideration that a gap was present between the ferrule and the
tube end, see photo’s

'

Photo 16. Top tubesheet Photo 17. Detail of tube to tubesheet

In the bottom part of this HP Stripper the most severe conditions are present due to the
high temperature, but also here SafurexÒ behaved quite well.
It can be concluded that, in spite of the higher temperatures and the fact that the liquid
distribution in this HP Stripper which was modified to suit Snamprogetti's process is
poor, the SafurexÒ still shows good corrosion resistance and the overall corrosion rate
measured is more or less identical with the corrosion rate measured after one year of
operations in the DSM HP Stripper viz. 0.08-mm per year.

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Photo 18. Bottom tubesheet

15.3 HP Stripper in the Shiraz Urea plant

Another positive observation with respect to the behavior of Safurex® was gained
beginning 2003. Some 4 months after initial start up, a leak occurred in a flange face
connection of the top man way closure in a Safurex® Stripper. These kinds of leakages
normally lead to corrosion of the flange faces.

Photo 19. BC.05 flange face after leak Photo 20. Safurexâ flange face after leak

When opening the leaking flange it appeared however that even though the 316
serrated gasket was badly corroded, the Safurex® flange faces did not show any
corrosion; after some slight brushing in order to remove the corrosion product
originating from the gasket, a new gasket could be installed and the plant could be
started, see figures 19 & 20.

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15.4 Exposure test of SafurexÒ in a Snamprogetti designed plant.

SafurexÒ test coupons have been exposed in the bottom of a SNAM Stripper operating
at 204 0C with an oxygen content of 0.2%. The samples were removed and examined.
The weight loss of the material after 532 days exposure was some 0.05 mm/year on-
stream. The samples have been placed back in the HP Stripper for further exposure.

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16. Future developments

It is scheduled that in 2004 a new Stamicarbon Pool condenser plant with a capacity of
3,250 mtpd designed with only HP SafurexÒ equipment will go into production.
The equipment has been fabricated without problems. Here the oxygen content can
also be reduced quite significant.

The ultimate test, to run a commercial urea plant without oxygen is near. At this
moment, the fabrication of the components for a urea plant build all in Safurex® is on
going. This 3,250 mtpd urea plant is build for Safco and is planned to go into production
in the year 2005. This will be the first commercial Urea plant that can operate without
the supply of any oxygen.

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17. Economical consequences

The economical consequences will be impressive.

There will be significant differences in material and in costs. The ease in maintenance
cannot be expressed in a value but the difference is evident.

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18. Conclusions

Reviewing this paper, following conclusions can be drawn,

· SafurexÒ is a proven construction material that has kept all the promises we had on
our list. Many references achieved since 1992 show that the corrosion properties are
supreme.

· All parts that need to be fabricated for a SafurexÒ Urea Plant are proven and also
proven is the fact that the equipment is less expensive. Besides this, maintenance
becomes easier and longer operating period between shut downs are possible. The
operation of the Urea plant is easier and one can operate with less care.

· SafurexÒ contributes to Plant safety and reliability. It will at the end result in lower
production costs.

· The biggest challenge to produce Urea in an oxygen free environment is near.

· Even in existing Urea plants the oxygen content can be lowered. The use of SafurexÒ
in non Stamicarbon urea plants confirm this statement.

· Tests in these plants show also that the limits with respect to maximum operating
temperatures are shifted and are higher than with any other material currently used in
commercial operating Urea plants.

· SafurexÒ will keep the urea world moving and more papers about the success of
SafurexÒ will for sure follow but then about the operational achievements.

· The use of SafurexÒ provides significant process and investment advantages

described in other papers published during this symposium.

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