Corrosion and Material Issues in Boilers: August 2016

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Corrosion and Material Issues in Boilers
Presentation · August 2016

DOI: 10.13140/RG.2.2.35359.15528
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Esa K. Vakkilainen
Lappeenranta University of Technology
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Modern Pulp Mill
Recovery & Energy
Esa Vakkilainen
29th August – 1st September, 2016
esa.vakkilainen@lut.fi
Pulp Mill Energy and Recovery
Processes
Lecture 11: Corrosion and Material
Issues
Pulp Mill Energy and Recovery Processes

Esa Vakkilainen -2-
Recovery Boiler Corrosion
Main items
 Types of corrosion in boilers?
 What is chlorine corrosion?
 When to use Sanicro 38?

Esa Vakkilainen -4-
Introduction
 When recovery boilers are designed one of the
most difficult questions that arise is; what kind of
materials should one use for different parts of
the boiler.
 Corrosion is typically divided into areas based
on location of corrosion;
 water side corrosion, in the steam/water side of the boiler
tubes
 high temperature corrosion, in the superheaters
 low temperature corrosion, economizers and air heaters

Esa Vakkilainen -5-
Corrosion of lower bends is not
uniform!
0.70
0.60
0.50
CORROSION RATE [mm/year]
0.40
0.30
0.20
0.10
0.00
347
347
347
347
347
347
347
347
347
347
HR3C
HR3C
HR2M
HR2M
HR2M
SPRAY
SPRAY
SH PANELS/MATERIAL

Esa Vakkilainen -6-
Normal tube environment

Esa Vakkilainen -7-
Sulfidation
 Sulfidation is the most common form of
corrosion in the lower furnace, in openingas and
in superheater tubes.
 In particular hydrogen sulfide (H2S) contents
close to the wall in the lower furnace can be
around twenty mole percent.
 In modern, high solids boiler the concentration
close to the wall above the tertiary air is only
some tens of ppm.

Esa Vakkilainen -8-
Sulfidation
 In sulfidation the iron reacts with sulfur in the gas

phase forming iron sulfide FeS.
 The protective oxidized surface of metal tube
reduces in presence of sulfur containing
species.

Esa Vakkilainen -9-
Effect of temperature and H2S
concentration on corrosion rate of
carbon steel and alloy AISI 304
(Salmenoja and Tuiremo, 2001)

Esa Vakkilainen -10-
Sulfidation attack to SH tube
(Suik, 2001)

High temperature corrosion
 Superheater tube side surfaces thin.
 Ash is sticking to the windward side of the tube.
 Molten layer exists at tube sides.
 Fuels contain minor amounts of impurities.
 These impurities can cause high temperature
corrosion in the superheaters.
 Especially vanadium, sulfur and alkali metals
cause high temperature corrosion.

Forest residue superheater ash
Biomass boiler
(Kurkela et al., 1998)

Chromium decreases corrosion

Even best materials corrode in
RB SH
(Salmenoja and Tuiremo, 2001)

Alkali corrosion
 Recovery boiler ash is normally solid
 Na and K form ash with low melting points
500…600 oC
 Molten alkali contact -> fast corrosion
 Chemical reactions occur faster with molten phase
 Liquid phase provides an electrolyte for
electrochemical reactions
 Liquid phase dissolves the corrosion products
 Liquid phase can fluidize the ash
First melting temperature
640
0 CO3/(Na2+K2), mol-%
620 5
10
600 15
20
580
oC
30
560
540
520
500
0 2 4 6 8 10 12 14 16
K/(Na+K), mol-%

Effect of T0 on SH corrosion
Black liquor
Ref. Metso
Chloride corrosion
 Chloride forms NaCl, Cl2 and HCl in gaseous from
 In active oxidation gases react with iron to FeCl2
 When in contact with oxygen it reacts back to
Fe2O3 releasing chloride in gas form
 Reformed iron oxide layer is porous and does not
offer protection from corrosion
 Released chloride can react with fresh iron oxide
and the cycle repeats
 Active oxidation mens rapid waste of superheater

Chloride corrosion - two boilers
5
4
High carbonate (Cl=2.0 w-%)
Corrosion rate, mm/a
Low carbonate (Cl=0.8 w-%)

3
0
400 450 500 550 600
Metal temperature, oC

Corrosion of T22
180
160
Corrosion rate [mills/y]
140
120
100
80
60
40
20
0
460 480 500 520 540 560
Temperature [ºC]

Hot chlorine corrosion
Main components of corrosion product layer
FLUE GAS Fe O 3
2
Fe O
3 4
Cl-rich layer
(+ some S)
Base Metal ( Tube Wall )
Loose grains
Corrosion product
Solid steel

Laboratory Test Results
Original
Surface ?
K Fe-
Cl oxide Salt
(Cr) (S) mixture
(NaCl+KCl+
Na2SO4+
Steel K2SO4 )
2¼ Cr - 1 Mo

Reactions
Deposits
O2 2KCl+Fe2O3 K2Fe2O4+C l2
Oxide layer
Steel grains
O2 +FeCl 2 Fe3 O4 +Cl2
2 2 Crack. Oxide scale is
flaking off
Fe
Intergranular corrosion front.

Tube wall
Chlorides.
Chloride corrosion in
superheater bank
Iron Oxide
Cl usually found here
Steel ( T22 )
(Koivisto, 2000)

Visuals on SH Corrosion
Large
pits
Rough surfaces Flaking oxide

Identification / Microscopic
Oxide
EDS analysis
Cl
Oxide

Visuals on Chlorine Corrosion
Hot chlorine corrosion,

inner tubes forming the
hair pin are the most
corroded ones

Molten hydroxide corrosion
 Typically sodium hydroxide vapor reacts with available
sulfur and chloride species
 Close to air and liquor ports the carbon dioxide partial
pressure can be low
 There it is possible that sodium hydroxide condenses to
the tube surface
 This kind of corrosion occurs behind the furnace tubes
close to air ports where gases can leak
 In addition it has been found at liquor gun openings
 SS 304L has ~10 times higher corrosion than CS
 In high pressure boilers the wastage of composite layer
can occur in less than two years
 Alloys with high nickel to chrome ratio seem to be able to
resist this corrosion
Acidic sulfate corrosion
 Boilers running at high sulfur dioxide emission
can experience acidic sulfate corrosion
 Formation of acidic sulfates, sodium bisulfate or
pyrosulfates occurs at flue gas temperatures
below 400 … 450 oC and causes problems
especially in boiler banks
 Formation of acidic sulfates is reduced by
running boiler with low level of excess air and
low sulfur dioxide emissions

Sulfur dew point
 When flue gases cool their capability of holding
species in gaseous form weakens and such
species start condensing
 The temperature where condensed species
appear is called dew point temperature
 Acid dew point means conditions where this
condensate is acidic
 Typically sulfur dew point refers to conditions
where sulfur trioxide starts condensing
 Also HCl condensation is possible
Furnace corrosion
 The first major corrosion problems emerged in 1960s.
 Heavy wall corrosion at Kaukopää was discovered 1961
 Sulfidation of iron oxide layer was found to be the main
cause
 Wasn’t solved until the composite tubing appeared 1972
 The second wave of problems hit when composite floor
tubes started cracking
 Several reasons exist for cracking of stainless steel 304
 Alloy 825 and modified alloy 835 (Sanicro 38) tubes
seem much less prone to cracking than 304L
 The third wave of furnace problems hit in the 1990’s,
when primary airport cracking caused large problems
 Use of highly alloyed steels (e.g. alloy 825 or alloy 625)
has not solved this problem
304L floor with corrosion

Role of temperature spikes is
uncertain
Floor tube temperature T1939
420.0
400.0
380.0
360.0
340.0
320.0
300.0
Time ( 2.10.1995 )

General floor corrosion
 Kraft recovery boiler furnace has very reducing
environment
 Water shift reaction causes high levels of carbon
dioxide and hydrogen
 In addition the burning black liquor droplets can
cause very high levels of reductive gases
 But general corrosion seems not to be the
limiting factor of current recovery boiler furnace
life

Molten smelt corrosion of floors
 Recovery boiler floors have large patches of
metal loss
 These spots are too big for pitting
 One probable cause is molten smelt corrosion
 Layer on the tubes can melt if high heat flux from
startup burners

Other causes of molten smelt
corrosion of floors
 There is smelt flowing along the tubes
 Large flow could eat away protective smelt layer
 Layer close to tubes can contain low melting
compounds
 Smelts with polysulfide in them have very low
melting temperature

Corrosion in flowing smelt,
Samples after 1 hour
304L
High Cr

Corrosion, materials in flowing
smelt
Corrosion in Flowing Smelt
0.5
Corrosion Rate
0.4
[mm/h]
0.3 304L
0.2 50 % Cr
0.1
0
0 5 10 15 20 30 40 50 70 90
Distance from Specimen End

Galvanic corrosion
 It’s well known that carbon steel floor tubes
corrode fastest close to the weld to composite
tubing
 This is one disadvantage of carbon steel floors
 Compared to 304L, Sanicro 38 is slightly better
but Sanicro 65 increases the corrosion of carbon
steel significantly
 Coatings effect on corrosion was similar to that
of Sanicro 65 (i.e. strong galvanic effect)

Galvanic corrosion of carbon
steel

Floor tubes, Galvanic corrosion
in polysulphide smelt
4
corrosion rate
3
Relative
2
1
0
Alloy 825 304L Alloy 625 45Cr/50Ni
coating
Carbon Steel coupled to:

Thermal fatigue of floors
 Thermal cycles take place in recovery boiler floors
 A cycle is initiated each time boiler is shut down and
started up
 Such spikes have also been observed during normal
operation
 Cracks can be created when a certain amount of cycles
has occurred

Thermal fatigue of floors
 The higher the stresses or strains associated with a
thermal cycle the fewer cycles are needed for a crack to
initiate.
 Normally these failures can be traced to occurrence of
very large temperature peaks
 The main risk with thermal fatigue is the fracture doesn’t
stop at the interface between carbon steel and cladding
but continues to grow into the carbon steel

Example of thermal fatigue

Char bed resistance
 Floor tube cracking is in most cases found to be
environmentally assisted
 So that there must be some chemicals, which at certain
temperature assists crack initiation and propagation
 In addition to this chemical and temperature an electrically
conductive electrolyte is needed
 Savcor has measured the bed electrical resistance. The bed
resistance varies a lot from “normal” between 2 and 5 kcm
to as low as 0.1 kcm and sometimes even lower
 So there is molten phases in the bed during normal
operation

Water washing
 Doug Singbeil, Paprican has made SCC tests in
simulated water wash conditions
 Tests show (salt + water) can cause cracking at
temperatures  170 oC.
 They have found a threshold stress about 170
MPa and a threshold temperature about 160 oC
for 304L
 It seems that the presence of sodium sulfide will
prevent complete dryout until about 180 oC

Airport corrosion
 Some of the recorded corrosion phenomena
include
 cold side corrosion,
 membrane cracking
 tube cracking

Airport corrosion - Cold side
corrosion
 Cold side corrosion is caused by molten
hydroxide corrosion
 Vaporized sodium hydroxide deposits on cold
back side of air port tubes
 Especially boilers with cast air tubes have
suffered from this corrosion mechanism
 As rate with compound is much higher than with
carbon steel, this doesn’t normally present great
concern

Airport corrosion – Membrane
wastage
 At upper and lower end of air ports there is
larger width of membrane, because of tube
bends
 This membrane is then at higher temperature
and exhibits higher corrosion rates
 Corrosion can be augmented by periodic
temperature excursions

Airport corrosion – Tube
cracking
 There are differences with external conditions
between air ports even close to each other
 The following affect the corrosive environment:
 presence of molten smelt on the char bed surface
 flow of molten smelt towards the air port tubes
 presence of large pieces of char near primary air ports
 It has been suggested that a combination of
several events may lead to tube temperature
excursions at primary air ports

Furnace design and materials
finned membrane wall

made from composite tubes
protective welded cladding
refractory with studs

Furnace corner design
Blocked tube needs to be

removed
‘rounded’ corners

Properties of typical floor tube
materials
Carbon 304L Sanicro 38 Sanicro 65

steel (Alloy 825) (Alloy 625)
Main elements Fe 20Cr–10Ni 20Cr–40Ni 20Cr–60Ni
Thermal expansion, 10–6 /C 13.5 17.5 14.9 13.9
Thermal cond., W/mC 41 19 16 14
SCC resistance Excellent Low High Excellent
Corrosion resistance Low Moderate Excellent High

Modern CS floor

Furnace floor
Smelt out Frosen smelt layer

Floor angles and smelt level
FRONT WALL REAR WALL

SMELT OVERFLOW LEVEL PROTECTIVE
FROZEN LAYER
b a
A. IN THE OLDEST DESIGN: FLAT FLOOR

MINIMUM SMELT OVERFLOW LEVEL
B. IN THE NEXT GENERATION DESIGN : b < 5 , a = 0

INCREASED SMELT OVERFLOW LEVEL
C. IN THE MODERN DESIGN: a = b > 2,5o
SUBSTANTIAL SMELT OVERFLOW LEVEL
IN ALL DESIGNS STABLE WATER CIRCULATION

Choice of furnace material –
Sanicro 38
 Sanicro 38-type composite material has the best
corrosion resistance in molten polysulfides
 Test panels of Sanicro 38 installed in 1991 and
1994 have not shown any alarming corrosion
 Nor have there been any reported cracking
found in recovery boiler bottoms made from
Sanicro 38 since 1995
 This highly alloyed material seems to have good
corrosion resistance, but it is fairly expensive.

304L as furnace material
 Stainless steel 304L seems to last well in the
furnace walls above the char bed
 It is very resistant to sulfidation
 SCC in the tubes at the furnace bottom tubes
has made manufactures and recovery boiler
owners search for replacement materials in that
area
 304L is not popular in modern high dry solids
boiler bottoms
 304L is used extensively above primary air ports
Furnace material Bends
 Suppliers’ current recommendations are to use
modified alloys in the front and rear bends and
close to the side walls.
 To facilitate weld inspection the whole lower
furnace is often made of modified alloys up to
and over the primary air ports.
 The present favorite is Sanicro 38
 In addition of high content of chrome and nickel
the tube has about the same thermal expansion
coefficient than the carbon steel
Sanicro 65 as furnace material
 Sanicro 65 (Alloy 625) composite tubing is
another possibility
 It has very favorable properties considering
thermal fatigue and stress corrosion cracking
 There are some reports of failure.
 Another area under study is the air port cracking.
Primary air ports and smelt openings seem to
exhibit cracking
 Thermal cycling and smelt contact are
suspected causes
Membrane materials
 Membrane materials should be similar to the
tube material used
 Composite membrane or totally stainless steel
membrane is used with composite tubing
 Fins receive thermal radiation and need to
conduct heat to the tube proper
 Fin surface is at higher temperature than tube
 In high heat flux areas and with wide fins this
can lead to tube cracking
 A composite membrane has better thermal
conductivity as compared to solid material
Burned membrane

Japanese and Swedes use
refractory and studs

Superheater design and materials
Operation problems that cause superheater
failure can be
1. Condensate blocked tubes during start up
2. Water from hydrotest not being evacuated during
start up
3. Water carryover from the drum
4. Desuperheater spray water quality control issues
5. Sootblower action
6. High temperature cycling caused by poor
superheating control

Superheater corrosion
 Even the most modern recovery boilers suffer
from superheater corrosion
 Corrosion is the main problem that limits the
ability of kraft recovery boiler to produce
electricity
 In comparison to coal fired boilers kraft recovery
boilers have higher rates of alkali metals,
chloride in gaseous form and often highly
reducing conditions caused by carryover
particles

Superheater corrosion
 On the other hand levels of some high

temperature corrosion causing substances like
antimony, vanadium and zinc are typically low

Increasing temperature ->
corrosion
(Fujisaki et al., 1994)

Superheater corrosion – steam
temperature
 Main steam temperature is the main parameter
that affects the choice of superheater materials.
 The rule of thumb is to keep the superheater
surface temperature below the first melting
temperature of deposits
 Corrosion rates in final superheaters are
increased because superheater material
temperatures are highest

velocity
 Steam side heat transfer coefficients in typical
recovery boiler superheaters are low
 Superheater surface temperature can be tens of
degrees higher than the bulk steam temperature
 Surface temperatures and thus corrosion rates
are greatly affected by superheater positioning
 Furnace radiation can effectively be reduced by
placing a screen to block radiation heat flux
 Therefore placing the hottest superheaters
behind the nose or screen will significantly
decrease corrosion
velocity
200
180
Furnace radiation
160 Behind nose
Tsurface - Tsteam, oC
140
120
100
80
60
40
20
0
0 5 10 15 20 25 30 35
Steam velocity m/s

Typical SH materials
 Typical primary superheater materials are
carbon steel
 Secondary and tertiary superheater materials
contain often 1 to 3 % Cr
 These kinds of materials are easy to weld and
have good corrosion protection.
 T22/10CrMo910 material can usually be used up
to 495 oC steam outlet temperatures
 With higher temperatures and higher chloride
and potassium contents it is advisable to use
higher chromium containing tubes
Example superheater materials
Cr Ni Mo Si Cu Al Mn C Fe Other
15Mo3 0.3 0.3 0.3 0.26 0.3 0.65 0.16 97.6
SA213 - T12 1.0 0.5 0.45 0.45 0.1 97.5 P,S
13CrMo44 1.0 0.3 0.3 0.26 0.3 0.55 0.14 97.1
SA213 - T11 1.25 0.50 0.75 0.45 0.15 96.9 P
10CrMo910 2.3 1.00 0.50 96.1
SA213 - T22 2.25 1.00 0.75 0.45 0.15 95.4 P
X10CrMoVNb91 9,0 0,3 1,00 0,40 0,50 88,7 V, Nb
SA213 - T91 9,0 0,33 0,99 0,24 0,03 0,45 0,11 88,7 Cb, N
HCM 12 12.0 1.00 86.9 V, Nb
X20CrMoV121 12.0 0.5 1.00 0.50 0.50 0.23 85.2 V
AISI 304 19.0 9.5 71.4
SS3338 18.0 12.0 0.72 0.15 69.2 Nb, Ta
AISI 316 17.0 11.0 2.70 69.2
AISI 321 18.5 10.2 0.75 2.00 0.06 68.5
AISI 347 17.5 10.3 1.30 0.70 1.60 0.08 68.4 Nb, Ta
253 MA 21.0 11.0 1.70 66.2 N, Ce
2205 22,0 5,5 3,20 1,00 2,0 66.2
Esshete 1250 16.0 11.0 1.25 1.00 7.0 62.5 V, Nb
AISI 309 23.0 14.5 0.70 1.50 0.10 60.2 P
HR2M 22.2 14.4 1.49 0.55 3.14 0.03 58.1 N
YUS170 24,4 13,2 1,50 0,78 0,58 0.02 59.5 N, P
AISI 310 25.0 20.5 0.50 0.08 53.8
Alloy 800 HT 21.0 32.5 0.50 0.40 0.40 0.75 0.05 44.3 Ti
HR3C 25.0 29.5 0.42 1.28 1.10 0.06 42.6 N
AC66 27.0 32.0 0.25 0.02 0.8 0.06 39.2 Ce, Nb

Superheater corrosion –
chromium
(Fujisaki et al., 1994)

Superheater corrosion – tube
arrangement
Flue gas
Secondary Tertiary
‘Cooler edge tubeb'

Material selection for black
liquor lines and evaporators
Esa Vakkilainen
Main items
 Stress corrosion cracking (SCC) in black liquor
 Use of 316 in evaporator?

Composition of steels
Cr Ni Mo N
304 18 9 0 00.6
316 17 11 2 0.06
254SMO 20 18 6 0.01
DUPLEX
2205 22 5.5 3 0.17

Typical composition of black liquor
% in dry solids % in dry solids
Na 20 NaOH 1-3
S 3-5 Na2S 3-9
K 1-2 Effective alkali 3-7
Cl < 1 Na2CO3 <10
SO4 <10 Na2SO4 <10
CO3 <10
Organic 60

Alkali in liquors
COOKING WASH STRONG

LIQUOR LIQUOR LIQUOR
Temperature (oC) 160-170 90 160-180
Dry solids (%) 30 15 85
Alkali (NaOH + Na2S) g/l 50 7 55
% in D.S. 20 5 5
g/kg H2O 80 9 283

NaOH in black liquor
(Actual mill data)
600
500
Mill 1
Mill 2
400 Mill 3
Alkali (g /kg H2O)
Mill 11
Mill 4
300 Mill 5
Mill 6
Mill 7
200 Mill 12
Mill 8
Mill 13
100
0
70 72 74 76 78 80 82 84 86 88 90
Dry solids (%)

General corrosion at 160 °C
0.140
0.120
0.100
Corrosion rate (mm/year)
304L
0.080 316L
SS2353
254SMO
0.060 2205
0.040
0.020
0.000
1
Steel

Relative corrosion of steels
500
Relative Corrosion
400
316
300 254SMO
200 304L
2205
100
0
140 150 160 170 180
Temperature (C)
Andritz data
The effect of alkali on SCC
110 250 430 670 g Na2S+

NaOH
/kg H2O

This is what can happen

SCC of material 316L
-Batch test
-Mill black liquor
-Dry Solids 80%
-NaOH 6 % in D.S.
-Temperature 182-185 oC
-Duration 7 days
-Material 316L

SCC at 165 °C in HD concentrator
Duration 8 months
Place near distribution box
Materials u-shapes
Tensile stress 1.0*Rp0.2
Steel Stress corrosion

cracking (SCC)
304L NO
316L YES
317L YES
SS2353 YES
774=No8904 YES
254SMO YES
Duplex 2205 NO
Duplex 2304 NO
Recommended piping material
 Black liquor (before final concentrator) 304
 Black liquor (after final concentrator) Duplex
 Weak and strong NCG 316
 Methanol 316
 Ash, biosludge 304

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Corrosion and Material Issues in Boilers

Presentation · August 2016

Electicity generating costs View project

Pyrolysis of some biomasses widely available in Brazil View project

The user has requested enhancement of the downloaded ﬁle.

Pulp Mill Energy and Recovery Processes

 What is chlorine corrosion?

 When to use Sanicro 38?

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

 In sulfidation the iron reacts with sulfur in the gas

Pulp Mill Energy and Recovery Processes

(Salmenoja and Tuiremo, 2001)

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

(Kurkela et al., 1998)

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

(Salmenoja and Tuiremo, 2001)

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Low carbonate (Cl=0.8 w-%)

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Intergranular corrosion front.

Cl usually found here

Pulp Mill Energy and Recovery Processes

Rough surfaces Flaking oxide

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Hot chlorine corrosion,

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes

Pulp Mill Energy and Recovery Processes