Corrosion in Urea Synthesis Solutions

Alstom, Växjö

NTT Consultancy
 Table of contents

- Introduction
- Stamicarbon CO2-stripping process
- Mechanism of carbamate corrosion
- Role of process parameters on corrosion
- Materials of construction in urea synthesis
- Morphology of corrosion phenomena in carbamate
solutions

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 Functional block diagram of the Stamicarbon
CO2 - stripping urea process

NH3 CO2

Synthesis

Low-pressure
recirculation

Wastewater Purified process

Evaporation
treatment condensate

Finishing

Urea
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 Urea processes

1. Once through processes

2. Conventional total recycle processes (1950’s)

3. Stamicarbon CO2 – stripping process (1960’s)

4. Further improvements (1990’s)

pool condenser; pool reactor design

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 Stamicarbon CO2 – stripping urea process

l m
Cooling
water
g e
Steam
h
water
f
i
Con-
TCW TCW
c densate j

d
Steam

NH3

Condensate
CO2 k
Steam
b
Condensate
Urea melt to
a granulation

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 Synthesis section of urea 2000 plusTM pool
reactor design

Carbamate recycle
LP absorber

HP
NH3 Pool reactor Scrubber

CO2

HP Stripper
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 Chemical reactions in urea synthesis

Formation of ammonium carbamate

2NH3 + CO2  NH2COONH4 + a cal

Dehydration of ammonium carbamate to urea

NH2COONH4  H2O + NH2CONH2 - b cal

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 Corrosion mechanism

High conductivity of urea synthesis solution due to

dissociation of ammonium carbamate:

NH2COONH4  NH2COO- + NH4+

Ammoniacal form of strong Bronsted acid: carbamic acid

with NH4+ as the solvated proton
(proton donor for cathodic reaction).

NH2COO- … NH4+

NH4+  NH3 + H+ (H3O+  H2O + H+)

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 Corrosion mechanism

Passive corrosion (oxide dissolution):

Cr2O3 + 6 NH4+ → 2 Cr3+ + 6 NH3 + 3 H2O

Cr2O3 + 6 H3O+ → 2 Cr3+ + 9 H2O

Passive/active corrosion (metal dissolution):

Anodic reaction: Me  Men+solv + n e-

Cathodic reaction: 2 NH4+ + 2e-  2 NH3 + H2

O2 + 2 H2O + 4e-  4 OH-
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 Corrosion mechanism

Ammonium carbamate in equilibrium with

ammonium(bi)carbonate

NH2COONH4 + H2O  (NH4)2CO3  HOCOONH4 + NH3

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 Passivation

Passivation reaction:

2 Cr + 3 H2O → Cr2O3 + 6 H+ + 6 e–

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 Active corrosion

Fe + 2 NH4+ → Fe2+ + 2 NH3 + H2

Ni + 2 NH4+ → Ni2+ + 2 NH3 + H2

2 Cr + 6 NH4+ → 2 Cr3+ + 6 NH3 + 3 H2

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 Voltomogram of 316L UG (X2CrNiMo18-14-3) in urea
synthesis solution

5.000

3.000
I /area (mA/cm 2)

<

1.000

-1.000

-3.000

150.0 250.0 350.0 450.0 550.0 650.0 750.0

E vs. 0.0000 (mV)

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 Active behaviour of stainless steel in
ammonium carbamate
log ic 1 2 3

a+c Ea E

C
1 = active region
log ic 2 = passive region
3 = transpassive region
a = anodic reaction
c = cathodic reaction
a + c = sum curve
C = 2NH4+ + 2e  2NH3 + H2

One zero potential Ea = Metal corrodes

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 Active/passive behaviour of stainless steel
in ammonium carbamate

log ia

Ep

Ea e
c k
a+c+k
c+k
k represents the reaction O2 + 2H2O + 4e  4OH-
a + c + k = sum curve
Two zero potentials:
Ea = metal in active state
log iC
Ep = metal in passive state

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 Passive behaviour of stainless steel in
ammonium carbamate

log ia

Ep

a+c+k Ep e
k
c
c+k

One zero potential left (Ep).

log iC Metal is passsive

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 Relevant process parameters on corrosion

- Oxygen content / redox potential

- Temperature

- NH3 : CO2 ratio

- Carbamate, water and urea content

- Chloride contamination

- Sulphide contamination
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 Relation between oxygen concentration in the
liquid phase of a urea synthesis solution and the
active (A) – passive (P) behaviour
Oxygen AISI 316 L X2CrNiMoN X2CrNiMoN2 X1CrNi26-1
concentration (UG) 25-22-2 9-6-2 (super
(duplex steel) ferritic
steel)
< 0.1 ppm A A A/P? A/P?

0.5 ppm A A A/P A/P

1 ppm A A A/P A/P

3 ppm A A/P A/P A/P

5 ppm A/P A/P A/P A/P

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 Temperature and oxygen pressure level in the
synthesis section of urea CO2 stripping process

temperature oxygen
pressure

oxygen pressure

temperature

bottom top bottom top

HP stripper HP condensor reactor

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 Materials of construction in urea synthesis

- Influence of alloying components Cr, Ni, Mo

Cr and mo improve stability of passive layer.
Ni is detrimental; it forms ammonia complexes that lower the
activation energy for the dissolution of the metal

- Influence of microstructure
presence of precipitations is detrimental for corrosion
resistance; susceptible to intergranular corrosion

- Quality testing by Huey-test and Streicher-test

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 Tests to determine susceptibility to intergranular
corrosion of stainless steels

Test Environment Standard Test Criterion Affects

duration
carbide -phase
In hours
Huey test 65% HNO3 ASTM A262 5 x 48h weight loss
boiling practice C microsc. exam.
Stac spec + +
53961
HNO3/HF 10% HNO3 ASTM A262 2 x 2h weight loss
test 3% HF 70°C practice D
+ -
Strauss 6% CuSO4 ASTM A262 24h 1 electric
test 16% H2SO4 practice E resistance
Cu–chips boiling 2 bending + -
3 noise
Streicher 19% g/l Fe2(SO4)3 ASTM A262 120h weight loss
test 50% H2SO4 boiling practice B microsc. exam
+ -
Oxalic 10% oxalic acid ASTM A262 1.50 min anodic
acid test room temp. practice A 1 A/cm3 etching
pattern
+ -
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Comparison of some samples of 316-types stainless
steel of one European steel producer;
Results of Huey-test and plant exposure for about one year

Steel type Corrosion rate

Huey – test µm/48 h Plant exposure µm/year

average surface stern face average surface stern face

316 Ti 6.83 30 160 210 80 125

316 L 1.81 80 60 55 80 160

316 L 2.91 80 270 110 180 550

316 L 8.11 480 200 200 415 320

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 Materials of construction in urea synthesis

- Influence of alloying components Cr, Ni, Mo

- Influence of microstructure

- Materials selection criteria

X2CrNiMo18-14-3 (316L UG)
aust. stainl. steels
X2CrNiMoN25-22-2

X2CrNiMoN22-5-3
X2CrNiMoN25-6-3 duplex stainl. steels
X2CrNiMoN29-6-2

-
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Material of construction selection criteria for liquid
concentrated carbamate (>10% wt)
Temperature [oxygen] in liquid phase Materials of construction
°C ppm (wt)

190 < Tn < 210 [O2] > 4 X2CrNiMoN29-6-2

X2CrNiMon25-22-2
190 < Tn < 210 0.1 < [O2] < 4 X2CrNiMoN29-6-2, Zr, Ta
135 < Tn < 190 [O2} > 4 X2CrNiMoN29-6-2
X2CrNiMo18-14-3 (316L UG)
X2CrNiMoN25-22-2
X2CrNiMoN22-5-3
135 < Tn < 190 2 < [O2] < 4 X2CrNiMoN29-6-2
X2CrNiMoN25-22-2
X2CrNiMoN22-5-3
135 < Tn < 190 [O2] < 2 X2CrNiMoN29-6-2, Zr, Ta
70 < Tn < 135 Oxidizing environment; lower X2CrNiMo17-13-2 (316L)
limit unknown X2CrNiMoN22-5-3

Tn < 70 Oxidizing environment; lower X2CrNi19-11 (304L)

limit unknown X2CrNiMo17-13-2 (316L)
X2CrNiMoN22-5-3

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 Material of construction selection criteria for liquid
diluted carbamate (<10% wt)

210 °C

170 °C

X2CrNiMo17-13-2
O2 free environment
X2CrNiMoN22-5-3
150 °C X2CrNiMoN29-6-2

O2 > 1 ppm
X2CrNiMo18-14-3
X2CrNi19-11
(316LUG)
X2CrNiMo17-13-2
120 °C

Tn °C X2CrNi19-11
X2CrNiMo17-13-2

0.0005 1.0 10.0

(Carbamate)
% (wt)
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 Corrosion rates in (oxygen free) carbamate solutions
100
BC.01
BC.05
SAF 2205
Corrosion mm/year

Safurex
10

1
0.0 0.1 0.5 1.0 10.0 100.0

0.1

0.01
P P M Ox ygen

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 Global composition of urea synthesis
solution (USS)

Mole fraction:
water: 31 %
ammonia: 39 %
urea: 18 %
carbamate: 12 %

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 Morphology of corrosion phenomena in carbamate
solutions

- Passive / active (overall) corrosion

- Stern face attack
- Pitting and stress corrosion cracking (SCC) in liquid
phase
- Crevice corrosion
- Condensation corrosion
- overall corrosion / crater like attack
- strain induced intergranular cracking
- Corrosion in pinholes
- Erosion-corrosion
- Hydrogen embrittlement
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Ruptured (BC.01) stripper tube due to overall
corrosion

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 HP Stripper
N14 N4
Gas outlet N13 N14

N4

see sheet 7
N4 N13

N1

USO inlet N7
N1 N7
Rupture disk
Steam inlet
N5 N11 10 weep holes
N5
dia. 6mm
equally divided
see sheet 8

Alternative B Alternative C
N4

N12
diameter
Vent N1
N6 Condensate N7
N6 outlet

N8
N8
Combinations of
see sheet 9

diameter
N15 the alternitives A
N9 up to C allowed as
CO2 inlet well. N9
N3
N3 Alternative D is
N13 only allowed if
N10 diameter is smaller
GUSO outlet N2 then approximately N2 N10
Alternative A 1000mm Alternative D
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 Top chamber of stripper
Lining or overlay
welding N14

N13
Bufferlayer
Overlay welding

Gas outlet to
HDCC 800  dia  1000

N4

N1

Liquid inlet
Lining or overlay from reactor
welding
10

Overlay welding
R**
N7

**
R must be  0.25
x channel wall
thickness with a
Bufferlayer minimum of 30mm Only alternitive A is drawn. Alternitives B up to
D(see sheet 6) are applicable.

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 Liquid divider of stripper with hold down plate and
holding down bolts

8.5mm
vent/drain hole **
dia 26 At least 3 lifting

–1.0
30
lugs per hold down
dia 12

2 +0.0
2 plate segment

10
* 2
PTFE rings
Hold down plate thickness 2.5mm
sealweld A A
* Weld a 15mm long piece of dia
4mm wire parallel to the gastube,
Reactor wall material to be used: BC.05 acc. to
specification A4-18005. Section A-A
** Number of holes about 1/3 of the
600

number of tubes and equally divided.

*** Minimal three stud bolts per hold
down plate segment. Holding down bolts

A A
PTFE bushing PTFE rings
2 thickness 2.5mm

Tube plate

Gas tube with divider Stud bolt ***

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 Liquid divider of stripper
dia 12 3 holes equally
seal weld seal weld spaced; dia … +0.05
dia. 36

1.6
ID. 20
dia. 28 *
OD. 25

10
15

25
dia 31

50
586
Seal weld
11°

3
ID. 24

OD. 28 *

1.6
1.6
45

dia 25.5 ±010

22

10.5
3 holes

12

1.6
dia 33.4 +0.05 – 0.00

dia 37

OD. 27 Liquid divider

45°
Gas tube
* tight fit
* tight fit dia 33.5 ± 0.05
10
Stripper
pipe
dia 30.5 0.00 – 0.05
3.2 1.6

Gas tube with liquid divider PTFE bushing

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 Bottom chamber of stripper

N8
2d

200
d 8

To be supported Straight
length 1.5d
LP R.A source for level
HP 25 25 Dia 27 -0.0 +0.5
measurement
Hole for HLS
N9**

***
****
N15
Min.
CO2 from
compressor 150
N3
Leak detection hole: *
Cyl. volume
800  dia  1000 dia. 5mm … m3

28
N15
**** 28 * See instrument data sheet, loop number L-200.
** Nozzles N9 and N10 prependicularly above
Dia. 55 N13 each other. Dia N9 to be checked by contractor.
Dia. 55
same level N10** *** Must satisfy the design code and 2mm
N2 corrosion allowance.
as N9 **** N15 and N9 on same elevation and 180° in
Hole for level opposite orientation
Outlet transmitter
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Active corrosion in stripper tube due to flooding

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Active corrosion in stripper tube due to flooding

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Standard inspection program (HP equipment / Stainless
Eddy Current measurement Stripper tubes
Steels)

Steam
Corroded
area
2 - 3 meters

Baffle

Area with α
Fe2O3 scale build
up

Typical behavior ECM measurement

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 Stripper tube wall thickness versus time

X new tubes
%-age of tubes

51 months
average value
74 months on
stream
X
40

X
20

X X tube wall thickness,mm

X X
0

2.50 3.00 3.50

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Condensation corrosion in liner top stripper

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Condensation corrosion in liner top stripper

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Condensation corrosion in strip overlay welding

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Strain induced intergranular cracking

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Microphoto of strain induced intergranular cracking

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Preferential locations of strain induced
intergranular cracking
Strip
Cracks Liner

Vessel wall

Liner
Cracks

Vessel wall

Ground weld area

Cracks Cracks Strip Liner

Vessel wall

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Stern face attack protruding tube ends

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Pitting and SCC in HP stripper gas tube

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Microphoto of pitting and stress corrosion
cracking

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Crevice corrosion of gas tubes due to fouling

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Fouling of gas tubes HP Stripper

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 Oil fouling of HP Strippers

Oily, sticky material (mixed up with fibres):

- PTFE fibres originating from packing of HP pumps

- Oil contamination originating from:

- CO2 compressor
- stuffing boxes of NH3 pumps
- ammonia feed from ammonia plant

PS: Centrifugal CO2 compressor to be preferred above

compressors of reciprocating type.
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Erosion - corrosion in valve

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Erosion corrosion in valve

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Embrittled titanium heat exchanger tube
due to titanium hydride formation

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 Corrosion in piping

• Condensation corrosion in gas lines

• Intergranular corrosion in weld-o-lets

• Stress corrosion cracking and crevice corrosion at

sealing faces of flanges (LP section)

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Condensation corrosion at thermowell

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Case: Intergranular corrosion in weld-o-let in HP
line of Urea plant

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 Weld-o-let failure in process line from reactor to
HP stripper

Weld-o-let ruptured during installing a bracket

Consequences: 4 people killed

5 people injured

Plant shut-down 2 months

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Location of failure in weld-o-let of thermowell

Thermowell
Failed here
RTJ flange
1½”

8” NB E.S. MPE
SS 316 175 mm

1½”, NB SCH 8O Pipe

Flow from reactor to HP Stripper

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Weld-o-let connection to pipeline

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Corroded areas at HAZ’s of weld-o-let

1 ½” NB pipe

Failed here

Corroded areas

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Ruptured weld-o-let

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Ruptured weld-o-let

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Weld-o-let with corroded HAZ’s

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Weld-o-let with corroded HAZ’s

4 mm

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Intergranular corrosion in HAZ of weld-o-let

50 m

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Radiographic examination indicating corrosion in
HAZ’s of weld-o-let and connecting 11/2” pipeline

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 Steam & Condensate System in Fertilizer Plant
Inert vent
steam

150 ºC high
PIC 4.5 bar pressure
high pressure steam condenser
film evaporator drum
condensate
drain
flash tank
PIC
9 bar
LIC LIC

HIC
vent CW
PIC N2 purge
steam saturator
21 bar LIC vent steam
condenser
25 bar steam LIC
steam condensate blow-down
tank
BL
tsp
hydrazine

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 SCC in tubes of HP Carbamate Condenser

Tube
Connection weld

Overlay weld

C-steel
tube sheet corroded
area

Shell side Blockage due to rolling

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External SCC in AISI 316L urea grade HP
Carbamate Condenser tube

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External SCC in AISI 316L urea grade HP
Carbamate Condenser tube

180 m

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 Urea Synthesis solution compared to sulphur
trioxide and sulphuric acid in aqueous solution

CO2 + H2O HOCOOH HOCOOH + NH3 HOCOO- + NH4+

Carbonic acid

CO2 + NH3 NH2COOH NH2COOH + NH3 NH2COO- + NH4+

Carbamic acid

SO3 + H20 HOSO2OH HOSO2OH + H2O HOSO2O-+ H3O-

Sulphuric acid

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 Corrosion mechanism

After dissolution of C2O3 protective layer the first step in

(passive/active) corrosion is formation of an absorbate:

Me + NH4+ Me… H+…NH3 Me-H+…NH3

The next step is the release of a proton to form a metal

hydride:

Me-H+…NH3 + e- Me – Had + NH3

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 Corrosion mechanism

1. Two hydrogen atoms, absorbed at the surface, will meet

and join to form a hydrogen molecule:
2Me – Had 2Me …. H2 2Me + H2

2. A next proton is bonded to the adsorbed hydrogen atom

to form a hydrogen molecule – ion:
2Me – Had + NH4+ Me-H…H+…NH3 Me-H2+…NH3

followed by a second reduction and release of the

hydrogen molecule:
Me – H2+ + e- Me….H2 Me + H2
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 Polarisation curve stainless steel 316L UG in
carbamate solution

Log i

Potential versus active corrosion potential

Sum current density (anodic + cathodic reactions)

2NH4+ + 2e- 2NH3 + H2
Fe Fe + 2e
++ -

O2 + 2H2O + 4e 4OH-

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 Increase of stripper outlet temperature

Increase of temperature will result in increase of

passive corrosion rate and may cause activation of e.g.
stripper tubes.

Increase of stripper outlet temperature can occur as a

result of:

• Increase of N/C mol ratio

• Increase of H/C mol ratio
• Increase of steam pressure
• Unequal liquid distribution

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 Material designation BC.01 (A4-18005)
For acceptable materials, see: MS.26

1. Weld metals

1.1. Weld metal for overlay and connection welds.

All deposited weld metal shall after final heat treatment, if any, have a fully
austenitic structure (max. ferrite content 0.6 %) with the following composition (%
wt):
C max. 0.045, Cr min. 17.0, Ni min. 14.0, Mo 2.20‑3.00, Mn min. 3.00.

1.2. Weld metal for connection welds only.

Deposited weld metal shall after final heat treatment, if any, have a fully austenitic
structure (max. ferrite content 0.6 %) with the following composition (% wt):
C max. 0.030, Cr. min. 17.0, Ni min. 13.0, Mo 2.20‑3.00

Deposits with a composition as mentioned under point 1 of designation BC.05 are

also acceptable.

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 Material designation BC.01 (continued)
2. Huey test

The materials shall be Huey‑tested in accordance with Stamicarbon specification

53961 and shall meet the following requirements:
The average value of the overall attack for 5 boiling periods of 48 hours each shall
not exceed 0.54 gr/m2 hr (3.3 m/48 hr).

3. Selective attack.
The penetration of selective attack as determined by microscopic examination after
the Huey test shall not exceed

-- for wrought materials, including heat affected zones: 70 m perpendicularly to,

and 200 m in to the direction of, rolling or forging.
-- for weld deposits: 200 m

Note
Where material according to BC.01 is required, also material according to BC.05
may be allowed. Stamicarbon to be consulted.

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 Material Specification MS.26 (A4-18005)

All wrought material shall have a fully austenitic structure (max. ferrite content 0.6 %)
after final heat treatment at the mill with the following composition (% wt):

C max. 0.030, Cr 17.0‑18.5, Ni 13.0‑15.0*, Mo 2.20‑3.00, Si max. 1.00,

Mn max. 2.00, P max. 0.045, S max. 0.030, N max. 0.22.

The following standard materials are acceptable provided that their composition
corresponds with the above values.

ASTM : AISI 316 L/UNS S 31603

AISI 316 LN/UNS S 31653 *
DIN : X 2 CrNiMo 17 13 2/W.S.N. 1.4404
X 2 CrNiMo 18 14 3/W.S.N. 1.4435
X 2 CrNiMoN 17 12 2/W.S.N. 1.4406 **
X 2 CrNiMoN 17 13 3/W.S.N. 1.4429 ***

The nickel content of nitrogen‑containing materials may be min. 11.0 % for :

* i.e. N min. 0.10 %
** i.e. N min. 0.12 %
*** i.e. N min. 0.14 %

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 Material designation BC.05
For acceptable materials, see: MS.34
1. Weld metals
Weld metal for overlay and connection welds.
All deposited weld metal shall after final heat treatment, if any, have a fully austenitic
structure (max. ferrite content 0.6 %) with the following composition (% wt):
C max. 0.040, Cr min. 24.0, Ni min. 21.0, Mo 1.90‑2.70, Mn min. 3.00
2. Huey test
The materials shall be Huey‑tested in accordance with Stamicarbon specification 53961
and shall meet the following requirements:
The average value of the overall attack for 5 boiling periods of 48 hours each, shall not
exceed 0.16 gr/m2 hr (1 m/48 hr).
3. Selective attack
The penetration of selective attack as determined by microscopic examination after the
Huey test shall nowhere exceed 70 m, in any direction

Note: Solidification defects in overlay welds are acceptable up to a depth of 100 m.

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 Material Specification MS.34
All wrought material shall have a fully austenitic structure (max. ferrite content 0.6 %)
after final heat treatment at the mill, with the following composition (% wt):

C max. 0.020, Cr 24.5‑25.5, Ni 21.0‑23.0, Mo 1.90‑2.30, Si max. 0.40,

Mn max. 2.00, P max. 0.020, S max. 0.015, N 0.10‑0.16

The following standard materials are acceptable provided that their composition
corresponds with the above values.

ASTM : UNS N08310

UNS S31050 (for forgings: according to Code Case 2038)
DIN : X 2 CrNiMoN 25 22 2/W.S.N. 1.4466
X 2 CrNiMoN 25 25 2/W.S.N. 1.4465
BS :
AFNOR :
JIS :
SIS :

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 Material designation BE.06
For acceptable materials, see: MS.50
1. Weld metals
The chemical composition of the deposited weld metal may differ from the base
material but shall be of a similar material type.
The ferrite content in the deposited weld metal and heat affected zone of the weld
shall be 30‑70 %.
2. Streicher test
The materials shall be Streicher‑tested in accordance with Stamicarbon specification
71112 and shall meet the following requirements:
The value of the overall attack shall not exceed 0.7 gr/m 2 hr. (4.3 m/48 hr)
3. Selective attack
The penetration of selective attack as determined by microscopic examination after
the Streicher test shall nowhere exceed 70 m, in any direction.
Notes:
1. Solidification defects in overlay welds are acceptable up to a depth of 100m.
2. Heat exchanger tubes shall be tested for homogeneity (ferrite‑austenite ratio) by
eddy‑current testing in accordance with Stamicarbon specification 71108.

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 Material Specification MS.50

All wrought material shall have a homogeneous ferritic‑austenitic structure, after

final heat treatment at the mill, with a ferrite content of 40‑60 %.
The material shall have a uniform ferritic structure with austenite islands fully
enclosed by ferrite.
The material shall be Sandvik Safurex

Safurex corresponds with the following standard:

ASTM : UNS S32906 (according to Code Case 2295)

DIN :
BS :
AFNOR :
JIS :
SIS :

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