You are on page 1of 34

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

1
RECAUSTICIZING CYCLE
WEAK WASH
SMELT LIME MUD
DISSOLVING WASHING
LIME KILN
SMELT
WATER
FROM LIME
RECOVERY MUD
BOILER LIME MUD

GREEN LIME WHITE


LIQUOR GREEN LIQUOR
CLARIFICATION LIQUOR CLARIFICATION

SLAKER GRIT
DREGS
/CAUSTICIZERS
WHITE LIQUOR

BASIC CHEMISTRY

GREEN + LIME = WHITE + LIME


LIQUOR LIQUOR MUD
Na2CO3 + H2O + CaO = 2NaOH + CaCO3

2
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

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

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
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

FLOWSHEET WITH CLARIFIERS


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

6
FLOWSHEET WITH PRESSURE FILTERS
Weak Wash
Smelt Tank
Lime Kiln
Green Liquor Lime Mud Filter
Stabilization Lime

Green White Pressure Filters


Liquor Liquor
Clarifier
Water

Dregs Filter Slaker /


Causticizers Water

FLOWSHEET WITH PRESSURE DISC FILTER


Weak Wash Water
Smelt Tank
Lime Kiln
Green Liquor Lime Mud Filter
Stabilization
Lime
Green Pressure Disc Filter
Liquor White
Clarifier Liquor
Water

Dregs Filter Slaker /


Causticizers

7
GREEN LIQUOR PREPARATION
Smelt
Weak Wash Clarified
Stabilization Green Liquor
Tank

Smelt Dissolving Clarifier


Tank

Dregs Filter
Dregs Holding Tank

Variation in Green Liquor Density or


Temperature in Stabilization Tank
Inlet
Temperature
Density or

Outlet

Time

8
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

9
GREEN LIQUOR CLARIFIER
RAKE DRIVE

CLARIFIER
FEED
MAX LL

STORAGE ZONE

MIN LL

FEEDWELL CLARIFIED
LIQUOR OUT
CLARIFICATION ZONE

UNDERFLOW OUT

CLARIFIER INTERNALS

Photo courtesy of Dorr-Oliver Eimco

10
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)

11
DREGS PRECOAT
FILTER

Photo courtesy of Dorr-Oliver Eimco

DREGS FILTER
OPERATIONAL PROBLEMS

• Wet cake discharge


• High soda loss
• Difficulty forming a precoat

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

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

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 MAKE-UP


Single Silo Two Silos
Reburned Fresh

FRESH
LIME

SLAKER SLAKER From SLAKER

Kiln

15
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

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

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

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

Photo courtesy of Kadant Black Clawson – Goslin™ Products Group

VERTICAL
TUBE TYPE
PRESSURE
FILTER

Photo courtesy of Kadant Black Clawson – Goslin™ Products Group

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

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.

22
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

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

Photo courtesy of Dorr-Oliver Eimco

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

LIME MUD WASHING

• 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

LIME MUD PRECOAT DRUM


FILTER

Photo courtesy of Dorr-Oliver Eimco

27
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

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

STEAM CONTROL VALVE

ΔT SLAKER CONTROL AND LIME SLAKER


GREEN LIQUOR DENSITY

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

EFFECT OF DENSITY CONTROL


ON WHITE LIQUOR CLARIFIER
UNDERFLOW BASED ON 1000 GPM OR
LPM TO DIGESTER
1600
1400
1400
1217
1200 1135
1000 1000 1000 Green Liquor
gpm or lpm

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

25% solids 35% solids 45% 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

You might also like