PPCHEM Ten Years of Experience with Polyamines in the High-Pressure Steam System of a Naphtha Cracker

Ten Years of Experience with Polyamines in the High-Pressure

Steam System of a Naphtha Cracker
Roy van Lier, Fabrice Cuoq, Rick Peters, and Jo Savelkoul

ABSTRACT
A decade ago, the ammonia/morpholine treatment of the 12.5 MPa steam system of one of SABIC Europe's naphtha
crackers was successfully converted to a polyamine program. Although application of film forming chemistry does not
come without challenges, experience in Geleen, Netherlands, generally has been positive.
The changeover to polyamines was instigated by fouling and corrosion problems in the steam system that could not
be solved using classic alkalization programs. The transition was inspired by Einstein's quote "We can't solve prob-
lems by using the same kind of thinking we used when we created them."
This paper provides an update on the cracker's polyamine application, including the results of the most recent turbine
inspections. Ten years of experience is interpreted and discussed in relation to the state-of-the-art of conventional
water/steam cycle treatment programs and in respect to recent film forming amine related publications.

INTRODUCTION unit against treated condensate exiting the CPU. Upon

Author's Copy

investigation it became clear that the corrosion products

In previous publications [1,2] the configuration, character-
originated from a zone of localized attack of the shell of
istics and specific challenges of the 12.5 MPa steam
the heat exchanger in the inlet area of polished conden-
system of one of SABIC's naphtha crackers in Geleen,
sate. As evident from Figures 1 and 2 the failure mode
Netherlands, have been described. The historical ammo-
responsible for the damage was unequivocally (single-
nia/morpholine treatment of the olefins plant's water/
phase) flow-accelerated corrosion (FAC).
steam cycle was successfully replaced by a polyamine
program at the end of 2005. The present article marks the
Despite the – certainly by today's standards – unusual
tenth anniversary of this breakthrough petrochemical
configuration of its impingement plate, the unit had been
application.
in operation for more than 20 years. The shell has been
repaired and the inlet configuration modified.

UPDATE ON NAPHTHA CRACKER POLYAMINE
APPLICATION
There is a lot of good news to report in this section:
• a largely uneventful cracker turnaround when it comes
to the steam system, with the exception of two specific
heat exchanger cases,
• exceptionally clean and mechanically sound turbines,
• no major upsets except for some disturbances in the
condensate polishing unit (CPU).
The abovementioned topics and observations are now
elaborated:
Economizer
Significant iron oxide fouling was found inside and down-
stream of an all-carbon steel shell-and-tube type econo-
mizer for cooling the feed flow to the condensate polishing
For the record, with the peculiar impingement configura-
tion described, FAC was bound to occur in this heat
exchanger at some point in time, independent of the type
of condensate treatment applied.
Air-Cooled Condenser
The goals of the cracker's polyamine program are (i) to
foster the formation of a magnetite layer with minimal sus-
ceptibility to mechanical removal and chemical dissolution
of iron values, and (ii) to remove suspended iron oxides via
the blowdowns of the steam drums and transfer line
exchangers (TLEs), the carbon beds in the CPU and the
cartridges of the boiler feedwater (BFW) filter. BFW and
condensate pump strainers constitute another manage-
able outlet since these may be periodically removed and
cleaned. By contrast, the accumulation of iron oxides in
certain low-flow areas is uncontrolled and unwanted. An
example of this can be seen in Figures 3 and 4.

© 2015 by Waesseri GmbH. All rights reserved.

356 PowerPlant Chemistry 2015, 17(6)

 Ten Years of Experience with Polyamines in the High-Pressure Steam System of a Naphtha Cracker
Figure 1:
View of damaged shell section of heat exchanger showing
impingement plate mounted with intermittent plate/shell welds.
Author's Copy
Figure 2:
Detailed view of encircled area in Figure 1 showing single-phase
FAC damage as a result of this unusual configuration.
It is believed that the observed messy, sticky fouling goes
back to the early days of the polyamine program. Indeed,
this particular condenser had not been opened since
2001. It was cleaned by hydrojetting.
For the record, waterside fouling of the feedwater pre-
heater addressed in [1] was significantly less than before.
Turbines
As described in [1] the Geleen cracker uses steam
turbines to drive cracked gas, ethylene (C2) and propylene
PowerPlant Chemistry 2015, 17(6)
PPCHEM
Figure 3:
View of head of air-cooled condenser as part of condensate
system – encircled drain nozzle particularly susceptible to
fouling.
Figure 4:
View of most fouled section of channel head.
(C3) compressors. Several pumps are steam turbine
powered as well.
The C3 turbine is an ABB unit, 60 % backpressure –
11 MPa, 40 % condensation – 1.8 MPa. It serves as the
internal reference for assessment of the effect of the
polyamine program on the steam system's rotating
machinery since it is the only turbine that has been
opened for planned inspection and maintenance work
pre-2005 and during the last turnaround.
357
 PPCHEM Ten Years of Experience with Polyamines in the High-Pressure Steam System of a Naphtha Cracker
a) b)
Author's Copy
Figure 6:
Integral view of C3 turbine rotor before the polyamine program.
Following 12 years of continuous service including
7½ years of exposure to polyamines, as visible in
Figures 5a and 5b, the C3 turbine was found to be excep-
tionally clean and in excellent mechanical state. No effort
was made to sample and analyze the negligible
"deposits".
In the pre-polyamine era turbines typically showed minor
fouling of iron oxides and silica/(Na,Al-)silicates, with the
former more prevalent in the high-pressure section and
the latter at lower pressures. For the record, the turbine
deposits visible in Figure 6 contained no ammonium or
amines and no corrosive anions (chloride, carbonate,
sulfate).
Unfortunately, instrumentation around the cracker tur-
bines is insufficiently accurate to quantify any potential
efficiency improvement related to the use of film forming
amines, which, according to older Russian studies using
octadecylamine (ODA), can amount to up to 2 % [3].
Condensate Polishing Unit
In 2012, SABIC, together with other industrial parties, initi-
ated a project to investigate the interaction between
358
Figure 5:
Partial views of C3 turbine rotor after
12 years of continuous service,
including 7½ years of exposure to
polyamines, prior to cleaning and
maintenance work:
a) high-pressure/medium-pressure
section
b) low-pressure section.
polyamines and ion exchange resins. Work was carried
out under the umbrella of KWR, the Dutch Watercycle
Research Institute [4].
Contrary to what was expected on the basis of the results
of the above study, problems with diminished cation
exchange resin loading capacity resurfaced in the CPU in
2013 and 2014. These have since been attributed to resin
fouling due to breakthrough of hydrocarbons from the
carbon filters, which has everything to do with the fact that
the activated carbon material has been in operation for
well over a decade. The carbon beds will be integrally
replaced and backwashing procedures revisited and reim-
plemented.
In hindsight, it would have been better to include a carbon
filter baseline study in the 2005 conversion protocol. There
is also still a need for a better understanding of the inter-
action between polyamines and activated carbon in
general.
INTERPRETATION AND DISCUSSION
In this section SABIC Geleen's polyamine experience and
position is discussed in relation to the state-of-the-art of
conventional water/steam cycle alkalization programs as
well as recent – since issuing of [2] – and otherwise rele-
vant publications on film forming amines. For this, the
informative PPChem 101 Fossil Cycle Chemistry series
[5–16] and Boiler and Heat Recovery Steam Generator
(HRSG) Tube Failures Lessons by Bursik and Dooley
[17–25] provide a suitable framework, because they cap-
ture the essence of many dimensions of water/steam
cycle treatment well.
Design Aspects
As explained in a previous paper [26], steam generators in
the (petro)chemical industry in many cases primarily serve
PowerPlant Chemistry 2015, 17(6)
 Ten Years of Experience with Polyamines in the High-Pressure Steam System of a Naphtha Cracker
as process stream coolers. This also holds for the TLEs in
the Geleen cracker, which are referred to as quench cool-
ers by many a process engineer. This reality should be
borne in mind when reading "cycle chemistry is frequently
called upon to find a remedy for incorrect design or mate-
rial selection and in this way to avoid preprogrammed
component failures" in Chemistry Lesson 3 [7].
Makeup Water Treatment
In Chemistry Lesson 2 [6] it is stated that "[i]f an industrial
cycle is to be operated with high reliability, availability, and
efficiency, it needs makeup of the same quality as utility
cycles do." This is correct from a technical point of view,
but for economic reasons often not possible with indus-
trial steam generation as the cost of high-purity makeup
would become prohibitive. Geleen site plants are fortunate
to have access to demineralized water of consistently
good quality at a competitive price – this has certainly
simplified the use of polyamines.
Acid Conductivity
Author's Copy
The skepticism of organizations like VGB and EPRI about
all-volatile treatment (AVT) programs involving organic
chemicals goes back to deep-rooted concerns about
(turbine) damage due to elevated acid conductivity levels.
For reasons explained in Chemistry Lesson 4 [8], achiev-
able acid conductivities in industrial cycles are typically
higher than in utility cycles. The reader is referred to
[1,26,27] for Geleen site experience with and opinions on
acid conductivity. The inspection results shared in this
paper prove once more that acid conductivities consis-
tently above 0.2 µS · cm–1 need not pose a threat to the
integrity of turbines, or of other steam system compo-
nents for that matter.
The authors do however acknowledge that higher
(degassed) acid conductivity values in relation to the
turbine warranty remain a major hurdle to the advance-
ment of polyamines. This, for instance, is implicit again
from a joint 2013 Siemens-BK Giulini (BKG) paper [28].
A 2014 paper by CWB Wasserbehandlung, supplier of
Fineamin® [29], reports on two power plant cases with
successful compliance of degassed acid conductivities
with the VGB limit of 0.2 µS · cm–1 [30]. The authors are not
aware of any recent Helamin® study on this subject.
Compliance with OEM requirements and guidelines in
general does not seem to be an issue with Anodamine™
[31,32]. This "green" film forming product is utilized in
multiple power stations, particularly in the USA. A
31.0 MPa supercritical once-through unit with a superheat
temperature of 590 °C reportedly operates with a steam
acid conductivity below 0.08 µS · cm–1 at an Anodamine™
concentration of 1 mg · kg–1 based on the BFW flow.
PowerPlant Chemistry 2015, 17(6)
PPCHEM
Anodamine™ has raised the interest of EPRI and is being
studied in more detail [33,34].
Unfortunately, no specific information about the composi-
tion of Anodamine™ is shared. The product is said not to
(de)protonate in the normal pH operating window of
water/steam cycles. It does not contain neutralizing
amines but relies on the presence of, for example, ammo-
nia in the cycle instead. The thermoelectric Seebeck effect
purportedly plays a role in the way the surface active com-
ponent(s) interact(s) with metal surfaces. No record seems
to exist of the limitations of Anodamine™, which is crucial
information when assessing the suitability of a film forming
product for (industrial) steam raising applications.
As inferred in a previous article [2], GE holds the trump
card with regard to acid conductivity as this company is
the sole supplier both of turbines and film forming amines
to the industry. Recent relevant GE publications include
[35–37]. Interestingly, the GE turbine described in [37] is
operated with steam treated with a GE blend of film form-
ing and neutralizing amines and an acid conductivity of
0.4–1.0 µS · cm–1, which is well above the company's own
specified limit.
Guidelines
In light of acid conductivity arguments and for many other
reasons there is a clear need for guidelines for AVT(F) pro-
grams, wherein the F refers to film forming – this as an
addition to the established AVT(O) and AVT(R) treatments,
wherein O and R stand for oxidizing and reducing, respec-
tively. Considering that the chemistry 101 lessons were
published in 2008–2009, it is not very surprising that
Lesson 5 [9] does not contain a description of AVT(F).
However, it is a missed opportunity that the revised VGB
guidelines [30] do not, not even in broad terms.
Fortunately, IAPWS has taken on the task of preparing a
first technical guidance document for the application of
film forming amines in fossil and combined cycle plants
for publication in 2016 [38]. The authors hereby offer their
support to this important initiative.
In Tube Failures Lesson 1 [17] the point is made that
"cycle chemistry is responsible for about 50 % of failures
in fossil plants and about 70 % in combined cycle units
with HRSG". In our view, this indicates that conventional
treatment programs fail to protect too many steam sys-
tems. It is believed that having AVT(F) guidelines in place
will help to establish film formers as a real alternative treat-
ment option and reduce reluctance with operators to use
polyamines.
User-supplier relationships are expected to benefit from
independent AVT(F) guidelines as well. As noted in
Chemistry Lesson 7 [11] on feedwater treatment with
organic chemicals, "[t]he users mostly rely on information
359
 PPCHEM Ten Years of Experience with Polyamines in the High-Pressure Steam System of a Naphtha Cracker
supplied by the respective chemical vendor or on their
own operating experience". Similar allusions are made in
Lessons 8 [12] and 10 [14] on boiler water treatment.
Luckily, more and more (general) information on
polyamines is becoming available in the public domain.
BKG, now part of Kurita Water Industries, supplier of
Cetamine®, is leading the way in this regard. Recent
Cetamine® related papers include [39–46]. A second
Cetamine® meeting was held in Graz, Austria [47]. It is
hoped that Kurita will bring new impetus to polyamine
research efforts and product development, and expand
film forming amine use to Japan and beyond.
Boiler Fouling by Corrosion Products
The danger of corrosion products entering a boiler in rela-
tion to under-deposit corrosion (UDC) mechanisms is
brought up in Chemistry Lesson 6 [10] on oxygenated
treatment. The reality of magnetite deposition in high heat
flux zones in vertical steam generators in combination with
the risk of the presence of non-volatile impurities in the
boiler water is the principal reason why a polyamine treat-
Author's Copy
ment has been implemented at the Geleen cracker.
An interesting recent study on magnetite deposition in
boiling heat transfer in the presence of different organic
treatment chemicals including a non-specified film form-
ing amine provided by BKG has been reported by Lister's
group [48].
Boiler Water Treatment
Chemistry Lesson 9 [13] deals with boiler water treatment
using sodium phosphate and caustic soda. It is remark-
able that these solid alkalis are still so much accepted
today given the damage they can cause when wrongly
applied or (accidentally) overdosed. It appears that the
"dark side" of solid alkali based programs is systemati-
cally underestimated.
Tube Failures Lessons 3 to 6 [19–22] are dedicated to the
UDC-type mechanisms hydrogen damage, caustic goug-
ing and acid phosphate corrosion. Not only can caustic
gouging and acid phosphate corrosion not occur in a film
forming amine treated water/steam cycle, but the risk of
hydrogen damage is vastly reduced as well by the contin-
uous removal of deposits. This makes it impossible for
corrodents to concentrate underneath loose magnetite
deposits and does away with costly periodic off-load
chemical cleanings.
Another inherent risk associated with solid alkalis is
turbine fouling through mechanical carry-over. Instead, a
polyamine program offers the advantages of improved
turbine efficiency and good protection against corrosion
during shutdowns.
360
Steam System Hydraulics
The issue of increased pressure drops due to rippled mag-
netite formation associated with AVT(R) programs – and
mitigation by the German 1970s so-called combined
water treatment – is mentioned in Chemistry Lesson 6
[10]. Reduced hydraulic resistance through the use of
polyamines has been reported with an 8.0 MPa Lamont-
type forced circulation boiler at the Geleen site [26] and
more recently in a Russian study [49]. Unfortunately, no
information on the type and concentration of the applied
filming amine(s) is disclosed in the latter. In [50] the
improved flow conditions are attributed to the phenome-
non of fluid slip.
Protection during Layup
The Geleen cracker's experience with polyamines is that
protection of the steam system during maintenance work
and inspections is adequate. During turnarounds, when
the steam system in its entirety is exposed to the atmos-
phere for a period of several weeks, hardly any flash rust
formation is observed.
Since film former technology could bring many benefits
for layups, it is unfortunate that it is not discussed as part
of Chemistry Lesson 11 [15] on this topic. Contrary to the
newly issued guidelines for feedwater, boiler water and
steam/condensate, it is anticipated that future VGB guide-
lines for layup will include a description of conservation
options using film formers.
Recent work on preservation of (the) water/steam cycle
(components) during outages using polyamines has been
published by Eskom [51] and by BKG/ICL/Kurita [52–56].
Anodamine™ has been applied for layup by North
American power plants [57]. Interestingly, ODA, "film
former 1.0", is still advocated and employed for layup
[58–61], [60] and [61] describing Chinese applications.
Protection against Corrosion-Fatigue and Flow-
Accelerated Corrosion
Evidence such as presented in [3,62] suggests that filming
amines have a mitigating effect on the damage mechanisms
described in Tube Failures Lessons 2 [18] and 7 [23]: corro-
sion-fatigue and FAC, respectively. This warrants further
investigation – for corrosion-fatigue also in relation to layup.
Instrumentation and Automation
The requirements for plant cycle instrumentation
described in Chemistry Lesson 12 [16] are unlikely to be
met in a cracker. A lack of instrumentation and automation
is what is holding the authors back from bypassing the
CPU as envisaged in the early days of the cracker's
polyamine program [1].
PowerPlant Chemistry 2015, 17(6)
 Ten Years of Experience with Polyamines in the High-Pressure Steam System of a Naphtha Cracker
The authors are following the development and trialing of
on-line photometric polyamine analyzers [63,64] with
interest.
CONCLUSIONS AND FINAL REMARKS
Conditioning of the 12.5 MPa steam system of one of
SABIC Europe's naphtha crackers in Geleen, Netherlands,
has evolved from AVT(R) in 1979 to AVT(O) from the
mid-1990s onwards to AVT(F) since 2005. The transitions
in the treatment program reflect the changing under-
standing of the physicochemical interactions between
water and steel over time (AVT(R) 씮 AVT(O)) and the avail-
ability of improved film forming amine chemistry
(AVT(O) 씮 AVT(F)).
The use of hydrazine was abandoned in the 1990s in order
to enhance the magnetite layer's resistance to FAC. Ten
years have passed since the remaining ammonia/morpho-
line treatment was successfully replaced by a polyamine
program. This breakthrough film forming amine applica-
tion has not been without difficulties, but the Cetamine®
Author's Copy
chemistry in place meets the cracker's requirements and
expectations.
According to Einstein, "The only source of knowledge is
experience." It is hoped that the future IAPWS AVT(F)
guidelines will help broaden the use of film forming amines
to the extent that they become the recognized addition to
the palette of available treatment methods for water/
steam cycles they deserve to be.
ACKNOWLEDGMENT
The authors wish to thank the management of SABIC for
permission to publish this paper.
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PowerPlant Chemistry 2015, 17(6)
 Ten Years of Experience with Polyamines in the High-Pressure Steam System of a Naphtha Cracker
THE AUTHORS
Roy van Lier (M.Sc., Raw Materials Processing, Delft
University of Technology, Delft, Netherlands, M.A.Sc.,
Hydrometallurgy, The University of British Columbia,
Vancouver, Canada) started his career 20 years ago as a
process metallurgist in the international mining industry. In
2001, he joined the DSM Materials & Corrosion
Department in Geleen, Netherlands, where he worked
closely together with Jo Savelkoul. In 2005, he succeeded
his mentor, working as a corrosion & water treatment
specialist with the SABIC Manufacturing Competence
Center in Geleen. In that role, ultimately, he assisted all
SABIC plants worldwide. In 2013, he joined SABIC
Technology & Innovation (T&I). As a chief scientist he
maintains a keen interest in utility water systems, although
with T&I his focus is on water on the petrochemical
process side, mainly the improvement of phase separa-
tions to reduce fouling in crackers. Roy van Lier is the
(co-)author of 16 technical papers and a book contribu-
tion.
Fabrice Cuoq (M.Sc., Materials Science, National
Author's Copy
Institute of Applied Sciences, Lyon, France, Ph.D.,
Environmental Sciences, Aix-Marseille University, Aix-en-
Provence, France) completed his studies in 2012 and
started working with SABIC Technology & Innovation in
2013. There he is a colloidal chemistry specialist providing
expertise notably in oil-in-water emulsion breaking and
dispersant technology. Like his mentor Roy van Lier,
Fabrice Cuoq is also highly interested in understanding
and furthering polyamine chemistry.
Rick Peters (M.Sc., Mechanical Engineering, Eindhoven
University of Technology, Eindhoven, Netherlands) started
his career with SABIC 3½ years ago. He works as a
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process engineer in the operational departments of the
naphtha crackers in Geleen, Netherlands. In his role, he
focuses on day to day plant operation with respect to util-
ities and energy. He is also involved with troubleshooting
and optimization of the cracking process at large.
Jo Savelkoul (B.Sc., Physical & Inorganic Chemistry and
Environmental Science, University of Applied Sciences,
Heerlen, Netherlands) worked with DSM in Geleen,
Netherlands, from 1961 to 2004. From 1979 to 2004 he
was a senior corrosion & water treatment specialist, and
head of the Water Laboratory of the DSM Materials &
Corrosion Department. Jo Savelkoul spent many years
working on the development of water treatment programs,
monitoring and test methods for cooling water, and the
mitigation of fouling and corrosion in industrial steam
systems. He has (co-)authored multiple papers on these
topics. Jo Savelkoul has been a member of the Dutch
National Standardization Institute, the Netherlands
Corrosion Centre and ISO task forces for various activities
in the field of industrial water treatment. Since his retire-
ment in 2004 he has been working as a private consultant
and course instructor in the fields of corrosion and water
treatment.
CONTACT
Roy van Lier
SABIC Technology & Innovation
L'Ambassadeur
Business Park Stein 108
6181 MA Elsloo
Netherlands
E-mail: roy.van.lier@SABIC.com
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