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SHORT COURSE
RECAUSTICIZING
CHAPTER 2.1 - PRINCIPLES AND PRACTICE
BY
DALE SANCHEZ
VECTOR PROCESS EQUIPMENT INC.
TOPICS
• BASIC CHEMISTRY
• FLOWSHEET OPTIONS
• GREEN LIQUOR PREPARATION
• WHITE LIQUOR PREPARATION
• LIME MUD WASHING
• CONTROLS
1
RECAUSTICIZING CYCLE
WEAK WASH
SMELT LIME MUD
DISSOLVING WASHING
LIME KILN
SMELT
WATER
FROM LIME
RECOVERY MUD
BOILER LIME MUD
SLAKER GRIT
DREGS
/CAUSTICIZERS
WHITE LIQUOR
BASIC CHEMISTRY
2
CHEMICAL REACTIONS
• SLAKING
CaO + H2O Ca(OH)2 + Heat
• CAUSTICIZING
Ca(OH)2 + Na2CO3 2NaOH + CaCO3
OVERALL REACTION
• EQUILIBRIUM REACTION
• REVERSIBLE
• INCOMPLETE
3
REACTION AT SOLID/
LIQUID INTERFACE
Na+
CaCO3
CO3=
UNREACTED
CORE
OH-
CaO
DEFINITIONS
TTA = TOTAL TITRATABLE ALKALI
NaOH + Na2S + Na2CO3
AA = ACTIVE ALKALI
NaOH + Na2S
EA = EFFECTIVE ALKALI
NaOH + ½ Na2S
SULFIDITY %
Na2S / AA or Na2S / TTA
4
DEFINITIONS
CE = CAUSTICITY %
NaOH x 100
NaOH + Na2CO3
Lime Availability %
CaO / Kiln Product
OPERATING CAUSTICIZING
105
EFFICIENCY
100
95
SULFIDITY=0%
% CE 90
SULFIDITY=15%
85
5% SULFIDITY=30%
80
OPERATING CE
75
0 50 100 150 200
TTA g/l
5
FREE CaO vs CAUSTICITY
7
6
% FREE LIME
5
4
3
2
1
0
70 75 80 85
% CAUSTICITY
6
FLOWSHEET WITH PRESSURE FILTERS
Weak Wash
Smelt Tank
Lime Kiln
Green Liquor Lime Mud Filter
Stabilization Lime
7
GREEN LIQUOR PREPARATION
Smelt
Weak Wash Clarified
Stabilization Green Liquor
Tank
Dregs Filter
Dregs Holding Tank
Outlet
Time
8
RAW GREEN LIQUOR
STABILIZATION TANK
RAW GREEN LIQUOR TOP MOUNTED AGITATOR
INLET PIPE
DOWN COMER
OPTIONAL SIDE
MOUNT AGITATOR
GREEN LIQUOR
CLARIFICATION OPTIONS
• SEDIMENTATION CLARIFIERS
• PRESSURE FILTERS
– CROSS FLOW FILTERS
– SOCK TYPE FILTERS
9
GREEN LIQUOR CLARIFIER
RAKE DRIVE
CLARIFIER
FEED
MAX LL
STORAGE ZONE
MIN LL
FEEDWELL CLARIFIED
LIQUOR OUT
CLARIFICATION ZONE
UNDERFLOW OUT
CLARIFIER INTERNALS
10
Clean Green Liquor!
Clarifier Feed Clarified Green Liquor
GREEN LIQUOR
CLARIFIER PROBLEMS
DIRTY GREEN LIQUOR
• Clarifier too small (rise rate too high)
• Properly designed internal components
• Use of Contaminated condensate
• Lack of Stabilization tank
• Settling aid addition problem (Polymer)
11
DREGS PRECOAT
FILTER
DREGS FILTER
OPERATIONAL PROBLEMS
12
WHITE LIQUOR PREPARATION
Green Liquor
Lime
White Liquor
Grit
Lime Slaker
Causticizers Clarifier
Lime Mud
LIME SLAKER
OVERFLOW TROUGH
LIME TO VENT SCRUBBER
SCREW
AGITATOR CLASSIFIER DRIVE
GREEN
SECONDARY GREEN
LIQUOR
LIQUOR FEED
GRIT
TO CAUSTICIZERS
CLASSIFIER
COMPARTMENT
SLAKING COMPARTMENT
13
LIME SLAKER
LIME SLAKER
• Sized based on retention time in
slaking compartment.
– For Clarifiers – 15 to 20 mins
– For Pressure filters – 20 to 25 mins
• Correct operation determines white
liquor strength
14
LIME SLAKER PROBLEMS
• OVERLIMING
– Lime feed rate and or GL flow and strength
• BOILING
– GL Temperature control and or lime feed rate
• GREEN LIQUOR TEMPERATURE
– Heating – Direct and indirect type heaters
– Cooling – Indirect heat exchangers
• FRESH LIME MAKE-UP - the way it is added
• GRIT – too much or too little grit can be an indicator
of a problem
FRESH
LIME
Kiln
15
SLAKER GRIT
HANDLING
• WASH GRIT TO pH LESS THAN 12.5
WITH GRIT WASHER
SLAKER GRIT
HANDLING
• GRIND OR
PULVERIZE GRIT
AND FILTER ON
DREGS FILTER OR
RECYCLE TO
LIME SLAKER
16
CAUSTICIZERS
INLET
OUTLET
INLET
RISER
OUTLET PIPE
WHITE LIQUOR
CLARIFICATION
OPTIONS
• SEDIMENTATION CLARIFIERS
• VERTICAL TUBE TYPE
PRESSURE FILTERS
• PRESSURE DISC FILTERS
17
WHITE LIQUOR CLARIFIER
RAKE DRIVE
CLARIFIER
FEED
MAX LL
STORAGE ZONE
MIN LL
FEEDWELL CLARIFIED
LIQUOR OUT
CLARIFICATION ZONE
UNDERFLOW OUT
18
WHITE LIQUOR
CLARIFIER PROBLEMS
• CLOUDY OVERFLOW
– Over Liming
– Fresh Lime
• LOW UNDERFLOW SOLIDS
– Over Liming
– Fresh Lime
– Rat Holing
– Pumping Rate
WHITE LIQUOR
CLARIFIER PROBLEMS
• Rat Holing
DE FE
19
WHITE LIQUOR
CLARIFIER PROBLEMS
• Pumping Rate
QS+ QL
UNDERFLOW
PUMP
QUF
DE FE
QD
FE
HOT WATER
QUF=QS+QL+QD
WHITE LIQUOR
CLARIFIER PROBLEMS
• Pumping Rate
– Mass flow of solids = Slaker solids output.
– Slaker solids output calculated from Green
Liquor flow and Lime rate.
20
VERTICAL
PRESSURE
FILTER
VERTICAL
TUBE TYPE
PRESSURE
FILTER
21
PRESSURE TUBE TYPE FILTERS
FILTRATION CYCLE
Filter 3-5 mins WHITE LIQUOR TO
Backwash 3-5 secs STORAGE TANK
Rest 25-35 secs
A B
Dp
WATER
FROM
CAUSTICIZERS
D F TO LIME MUD
WASHER (WEAK
WASH FILTER)
FEED
TANK
MUD
TANK
Acid washing
– Interval between washes 4 – 8 weeks
– Acid types
• Sulphamic, Hydrochloric, Formic
– Alternative strategy
• Change filter socks every 6 months or when needed.
22
PRESSURE TUBE TYPE FILTERS
PRESSURE FILTER
INTERNALS
23
PRESSURE FILTER
PROBLEMS
• FREQUENT ACID WASHING
– Green Liquor Dregs – contaminates filter socks
– Overliming – temporary blinding of filter socks
• HIGH PRESSURE DROP
– Overliming
– Dregs
– High Mud Level
• SHORT FILTER SOCK LIFE
– Dregs contamination
WL PRESSURE DISC
FILTER
24
WHITE LIQUOR PRESSURE DISC FILTER
CAKE
COMPRESSOR WASH WATER
WHITE
LIQUOR
FROM
CAUSTICIZERS
SEPARATOR
WATER WHITE
LIQUOR
LIME MUD
FEED SLURRY TANK
TANK
TO LIME MUD STORAGE
LIQUOR YIELD
100 100 96.8
82.1
80
60
White Liquor with Mud
White Liquor to Digester
40
17.9
20
0 3.2
0
Causticized Gravity Disc Filter
Slurry System (35% System(75%
Solids) Solids)
25
LIME MUD WASHING
Water
Lime Mud Filtrate
Weak Wash
Lime
Mud Water
Mixer
Lime Mud
Lime Mud Washer Filter
Lime Mud
Storage
• SEDIMENTATION CLARIFIERS
• VERTICAL PRESSURE FILTERS
• NOT REQUIRED WITH
PRESSURE DISC FILTERS
26
LIME MUD WASHER
PROBLEMS
• CLOUDY OVERFLOW
– Over Liming, Fresh Lime, Scrubber Dust,
Contaminated Condensate.
• LOW UNDERFLOW SOLIDS
– Over Liming, Fresh Lime, U/Flow Pumping
• HIGH SODA IN WEAK WASH AND LIME
MUD
– Water Balance, U/Flow Pumping
• TOO MUCH WEAK WASH
– Water Balance
27
LIME MUD PRECOAT DISC FILTER
28
TRS Control via
Mud Dewatering & Oxidation
AIR
Washing
Zone
TO KILN
0.2% Water
Soluble Soda
WITHOUT WITH
OXIDATION OXIDATION
Na2S = 0.04% Na2S = 0.005%
CONTROLS
• CAUSTICIZING CONTROL
Conductivity
On-Line Titration
Near Infrared Spectrometry
• GREEN LIQUOR TEMPERATURE
AND DENSITY
• LIME MUD DENSITY CONTROL
29
SLAKER CONTROL
CONTROL
D C SYSTEM
LIME
GREEN LIQUOR F
SCREW
T C
C
LIME SLAKER
CAUSTICIZERS
CONDUCTIVITY BASED CONTROL SYSTEM
SLAKER CONTROL
CONTROL AUTOMATIC
TITRATOR
D SYSTEM
LIME
GREEN LIQUOR F
SCREW
LIME SLAKER
WL
SAMPLE LINE
CAUSTICIZERS FILTER
TITRATION BASED CONTROL SYSTEM
30
SLAKER CONTROL
CONTROL NIR
SENSOR(S)
D SYSTEM
LIME
GREEN LIQUOR F
SCREW
LIME SLAKER
WL
SAMPLE LINE
CAUSTICIZERS FILTER
NEAR-INFRARED BASED CONTROL SYSTEM
WEAK
SLAKER CONTROL
WASH
CONTROL
SYSTEM
T
D LIME
HEATER
GREEN LIQUOR F
SCREW
T
31
DENSITY CONTROL LOCATIONS
Weak Wash
Smelt Tank
Lime Kiln
Green Liquor Lime Mud Filter
Stabilization
Lime
Lime Mud
Green Washer
Liquor White Liquor
Clarifier
White
Liquor
Dregs Filter Clarifier
Slaker /
Causticizers Water
1000
White Liquor with
800
Mud
600 White Liquor to
400 Digester
400
217
200 135
ALL SOLIDS EXPRESSED
AS SUSPENDED SOLIDS
0 NOT TOTAL SOLIDS
32
OTHER TECHNOLOGIES
• PRESSURE GREEN LIQUOR FILTERS
• FILTER PRESS FOR DREGS
DEWATERING
SUMMARY
WHAT IS IMPORTANT?
• GOOD GREEN LIQUOR
– Raw Green Liquor Stabilization Tank
– Conservatively Sized Clarifier
– Density and temperature control
• DO NOT OVERLIME
– Causticizing Control
– Fresh Lime Make-up.
33
CONCLUSION
FOR TROUBLE FREE OPERATION
• ADEQUATELY SIZED EQUIPMENT
• GOOD GREEN LIQUOR QUALITY
• GOOD LIME QUALITY
• EFFECTIVE CAUSTICIZING CONTROL
– Slaker and Density controls
• LIME MUD WASHING
34