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TAPPI KRAFT RECOVERY 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
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RECAUSTICIZING CYCLE WEAK WASH
SMELT DISSOLVING
LIME KILN
SMELT FROM RECOVERY BOILER
WATER
LIME MUD
GREEN LIQUOR CLARIFICATION
DREGS
LIME MUD WASHING
LIME MUD
WHITE LIQUOR CLARIFICATION
LIME GREEN LIQUOR
SLAKER GRIT /CAUSTICIZERS
WHITE LIQUOR
BASIC CHEMISTRY GREEN LIQUOR
+ LIME
= WHITE LIQUOR
+
LIME MUD
Na2CO3 + H2O + CaO = 2NaOH + CaCO3
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CHEMICAL REACTIONS • SLAKING CaO + H2O
Ca(OH)2 + Heat
• CAUSTICIZING Ca(OH)2 + Na2CO3
2NaOH + CaCO3
OVERALL REACTION Na2CO3 + H2O + CaO
2NaOH + CaCO3
• EQUILIBRIUM REACTION • REVERSIBLE • INCOMPLETE
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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
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DEFINITIONS CE = CAUSTICITY % NaOH x 100 NaOH + Na2CO3 Lime Availability % CaO / Kiln Product
Note: All chemical concentrations are expressed on a Na2O basis e.g. TTA = 120 g/l as Na2O Other units of measure are lb/ft3 & lb/gal
OPERATING CAUSTICIZING EFFICIENCY 105 100 95
SULFIDITY=0%
% CE 90
SULFIDITY=15%
85
SULFIDITY=30%
5%
80
OPERATING CE
75 0
50
100
150
200
TTA g/l
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FREE CaO vs CAUSTICITY 7 % FREE LIME
6 5 4 3 2 1 0 70
75
80
85
% CAUSTICITY
FLOWSHEET WITH CLARIFIERS Smelt Tank
Weak Wash Lime Kiln
Green Liquor Stabilization Green Liquor Clarifier
Dregs Filter
Lime Mud Filter Lime Lime Mud Washer White Liquor
Slaker / Causticizers
White Liquor Clarifier Water
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FLOWSHEET WITH PRESSURE FILTERS Weak Wash Smelt Tank Lime Kiln Green Liquor Stabilization Green Liquor Clarifier
Lime Mud Filter Lime Pressure Filters
White Liquor
Water
Dregs Filter
Slaker / Causticizers
Water
FLOWSHEET WITH PRESSURE DISC FILTER Weak Wash Smelt Tank Green Liquor Stabilization Green Liquor Clarifier
Water
Lime Kiln Lime Mud Filter Lime Pressure Disc Filter White Liquor Water
Dregs Filter
Slaker / Causticizers
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GREEN LIQUOR PREPARATION Smelt
Weak Wash Stabilization Tank
Smelt Dissolving Tank
Clarified Green Liquor
Clarifier
Dregs Filter
Dregs Holding Tank
Variation in Green Liquor Density or Temperature in Stabilization Tank
Density or Temperature
Inlet
Outlet
Time
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RAW GREEN LIQUOR STABILIZATION TANK RAW GREEN LIQUOR
TOP MOUNTED AGITATOR
INLET PIPE DOWN COMER
OPTIONAL SIDE MOUNT AGITATOR
PUMP TO GREEN LIQUOR CLARIFIER
GREEN LIQUOR CLARIFICATION OPTIONS • SEDIMENTATION CLARIFIERS • PRESSURE FILTERS – CROSS FLOW FILTERS – SOCK TYPE FILTERS
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GREEN LIQUOR CLARIFIER RAKE DRIVE
CLARIFIER FEED MAX LL STORAGE ZONE
MIN LL FEEDWELL CLARIFICATION
CLARIFIED LIQUOR OUT ZONE
UNDERFLOW OUT
CLARIFIER INTERNALS
Photo courtesy of Dorr-Oliver Eimco
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Clean Green Liquor! Clarifier Feed
Clarified Green Liquor
Photo courtesy of Dorr-Oliver Eimco
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)
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DREGS PRECOAT FILTER
Photo courtesy of Dorr-Oliver Eimco
DREGS FILTER OPERATIONAL PROBLEMS • Wet cake discharge • High soda loss • Difficulty forming a precoat
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WHITE LIQUOR PREPARATION Green Liquor Lime White Liquor Grit Lime Slaker Causticizers
Clarifier Lime Mud
LIME SLAKER OVERFLOW TROUGH LIME
TO VENT SCRUBBER
SCREW CLASSIFIER DRIVE
AGITATOR GREEN LIQUOR
SECONDARY GREEN LIQUOR FEED
GRIT
TO CAUSTICIZERS
CLASSIFIER COMPARTMENT SLAKING COMPARTMENT
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LIME SLAKER
Photo courtesy of Kadant Black Clawson Inc. – Goslin™ Products Group
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
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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 MAKE-UP Single Silo
Two Silos Reburned
Fresh
FRESH LIME
SLAKER
SLAKER
From Kiln
SLAKER
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SLAKER GRIT HANDLING • WASH GRIT TO pH LESS THAN 12.5 WITH GRIT WASHER
Photo courtesy of Kadant Black Clawson – Goslin™ Products Group
SLAKER GRIT HANDLING • GRIND OR PULVERIZE GRIT AND FILTER ON DREGS FILTER OR RECYCLE TO LIME SLAKER
Photo courtesy of Kadant Black Clawson – Goslin™ Products Group
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CAUSTICIZERS INLET
OUTLET
INLET OUTLET
RISER PIPE
WHITE LIQUOR CLARIFICATION OPTIONS • SEDIMENTATION CLARIFIERS • VERTICAL TUBE TYPE PRESSURE FILTERS • PRESSURE DISC FILTERS
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WHITE LIQUOR CLARIFIER RAKE DRIVE
CLARIFIER FEED MAX LL STORAGE ZONE
MIN LL FEEDWELL CLARIFICATION
CLARIFIED LIQUOR OUT ZONE
UNDERFLOW OUT
WHITE LIQUOR CLARIFIER For successful clarifier operation • Causticizer retention of 90 minutes • Good accurate torque indication on rakes • Properly sized variable speed underflow pumps with density and flow measurement
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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
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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.
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VERTICAL PRESSURE FILTER
Photo courtesy of Kadant Black Clawson – Goslin™ Products Group
VERTICAL TUBE TYPE PRESSURE FILTER
Photo courtesy of Kadant Black Clawson – Goslin™ Products Group
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PRESSURE TUBE TYPE FILTERS FILTRATION CYCLE Filter 3-5 mins Backwash 3-5 secs Rest 25-35 secs
WHITE LIQUOR TO STORAGE TANK
A
B
Dp
WATER FROM CAUSTICIZERS
D
F
TO LIME MUD WASHER (WEAK WASH FILTER)
FEED TANK MUD TANK
PRESSURE TUBE TYPE FILTERS Acid washing – Interval between washes 4 – 8 weeks – Acid types • Sulphamic, Hydrochloric, Formic
– Alternative strategy • Change filter socks every 6 months or when needed.
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PRESSURE TUBE TYPE FILTERS For successful operation of pressure filters. • Clean green liquor < 100 mg/l • Causticizer retention time 150 -180 minutes. • Causticizing control system.
PRESSURE FILTER INTERNALS
Photo courtesy of Kadant Black Clawson – Goslin™ Products Group
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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
Photo courtesy of Dorr-Oliver Eimco
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WHITE LIQUOR PRESSURE DISC FILTER COMPRESSOR
CAKE WASH WATER
WHITE LIQUOR SEPARATOR
FROM CAUSTICIZERS
WHITE LIQUOR
WATER
LIME MUD SLURRY TANK
FEED TANK
TO LIME MUD STORAGE
LIQUOR YIELD 100
96.8
100 82.1
80 60
White Liquor with Mud White Liquor to Digester
40 17.9
20 0
3.2
0 Causticized Slurry
Disc Filter Gravity System (35% System(75% Solids) Solids)
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LIME MUD WASHING Water Lime Mud
Filtrate Weak Wash
Lime Mud Mixer
Water
Lime Mud Washer
Lime Mud Storage
Lime Mud Filter
LIME MUD WASHING • SEDIMENTATION CLARIFIERS • VERTICAL PRESSURE FILTERS • NOT REQUIRED WITH PRESSURE DISC FILTERS
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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
LIME MUD PRECOAT DRUM FILTER
Photo courtesy of Dorr-Oliver Eimco
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LIME MUD PRECOAT DISC FILTER
Photo courtesy of Dorr-Oliver Eimco
LIME MUD FILTER PROBLEMS • HIGH MOISTURE IN KILN FEED – Over Liming, Fresh Lime, Dregs, Overloaded
• FREQUENT PRECOAT CHANGES – Blinding of Precoat • Over Liming, Fresh Lime, Dregs, Wash Water
• HIGH SODA IN KILN FEED – Cake Wash, High Moisture
• TRS EMISSIONS FROM KILN – Cake Wash, Overloaded
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TRS Control via Mud Dewatering & Oxidation AIR Washing Zone
TO KILN 0.2% Water Soluble Soda WITHOUT OXIDATION Na2S = 0.04%
WITH OXIDATION Na2S = 0.005%
CONTROLS • CAUSTICIZING CONTROL Conductivity On-Line Titration Near Infrared Spectrometry
• GREEN LIQUOR TEMPERATURE AND DENSITY • LIME MUD DENSITY CONTROL
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SLAKER CONTROL CONTROL SYSTEM
D C
LIME GREEN LIQUOR
F
SCREW T
C C
LIME SLAKER CAUSTICIZERS CONDUCTIVITY BASED CONTROL SYSTEM
SLAKER CONTROL CONTROL SYSTEM
D
AUTOMATIC TITRATOR
LIME GREEN LIQUOR
F
SCREW T
LIME SLAKER SAMPLE LINE
CAUSTICIZERS
WL FILTER
TITRATION BASED CONTROL SYSTEM
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SLAKER CONTROL NIR SENSOR(S)
CONTROL SYSTEM
D
LIME GREEN LIQUOR
F
SCREW T
LIME SLAKER SAMPLE LINE
WL FILTER
CAUSTICIZERS
NEAR-INFRARED BASED CONTROL SYSTEM
WEAK WASH
SLAKER CONTROL CONTROL SYSTEM T D
LIME
HEATER
GREEN LIQUOR
F T
SCREW
STEAM CONTROL VALVE
ΔT SLAKER CONTROL AND GREEN LIQUOR DENSITY
LIME SLAKER
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DENSITY CONTROL LOCATIONS Weak Wash
Smelt Tank
Lime Kiln Green Liquor Stabilization
Lime Mud Filter Lime Lime Mud Washer White Liquor
Green Liquor Clarifier
Dregs Filter
White Liquor Clarifier
Slaker / Causticizers
Water
EFFECT OF DENSITY CONTROL ON WHITE LIQUOR CLARIFIER UNDERFLOW BASED ON 1000 GPM OR LPM TO DIGESTER 1600 1400 gpm or lpm
1200 1000
1400 1217 1000
1135 1000
1000
White Liquor with Mud White Liquor to Digester
800 600 400
400 217
200
135
0 25% solids
Green Liquor
35% solids
ALL SOLIDS EXPRESSED AS SUSPENDED SOLIDS NOT TOTAL SOLIDS
45% solids
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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.
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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
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