Recausticizing

&
Lime Kiln Area

By: Andre Syahputra

 Contents
1. Safety Issues
2. Core Values TOPICC
3. Purpose & Targets of Recausticizing
4. Recausticizing & Lime Kiln Quality Control
Safety Issues Potential Hazards
Parameter Test Plan
Total suspended solid in WL, GL, X-
Filter CD Filter and WWL
Total Active Alkali & Total Titrable
Alkali (TAA & TTA) in GL and WL
Analysis of Lime Mud
Water Soluble Sodium of Lime Mud
with Flame Photometer
Available CaO
Potential Incident
• Exposed hot liquor into skin and
eyes.
• Inhaled vapors chemicals from
hot sample.
• Contact or exposed chemicals
HCL into eyes.
• Exposed hot liquor into skin and
eyes.
• Inhaled vapors of H2S
• Inhaled vapors of Formaldehyde.
• Contact finger with hot container.
• Contact sample that contains
alkali with skin and eyes.
• Gasometer is Blow
• Contact finger with hot container.
• Contact chemicals HCl 0.5N into
eyes.
Severity
• Can be irritating to the eyes
• Can be irritating to the skin
• Can be irritating bronchial tube
• Can be irritating to the eyes
• Can be irritating to the skin
• Irritating respiratory tract
• Can make blood and organs
poisoning (with repeated
exposure)
• Can be irritating to the eyes
• Can be irritating to the skin
• Fatality
• Can be irritating to the eyes
• Can be irritating to the skin
Safety Issues Preventive Actions

• Follow standard procedures of test

plan and safety & 5S in laboratory

• To active BAGUSi and NCR Program

• Always using PPE (Personal

Protective Equipment)
TOPICC
Purpose & Targets of Recausticizing
• Part of the overall chemical recovery
in pulp mill.
• The main purpose of recausticizing process is converts sodium carbonate
(Na2CO3) into sodium hydroxide (NaOH) for use in the cooking process,
utilizing calcium oxide (CaO).
Purpose & Targets of Recausticizing

Two consecutive reaction occur during recausticizing:

• Slaking
CaO(s) + H2O(aq) → Ca(OH)2 (s)

• Causticizing
Ca(OH)2(s) + Na2CO3(aq) → 2NaOH(aq) + CaCO3 (s)
Purpose & Targets of Lime Kiln

Convert calcines lime mud (CaCO3) to reactive lime CaO by drying and
subsequent heating for reuse in the recaustizing process.

Chemical reaction in lime reburning:

CaCO3(s) → CaO(s) + CO2(g)
Recausticizing & Lime Kiln
Quality Control

• Soda Content of Green Liquor and White Liquor

• Total Suspended Solid
• Lime Mud Analysis
• Available CaO & Residual CaCO3
• Specific Gravity of Green Liquor Recovery Boiler
• Conductivity of Condensate
Soda Content of White Liquor
TEC/PLB-0069-PR

• Define the method for analysis of Strong White Liquor as a means of controlling
the strength (level) of kraft cooking liquor

• By checking the contents of TAA, TTA, Na2S, %S in White Liquor

Soda Content Procedure Analysis

Mix the sample, pipette 2 mL sample into 250 mL

1 erlenmeyer and add 50 mL demin water

Add 25 mL BaCl2 solution and 3 drops PP indicator and mix.

2 Titrate with HCl 0,5 N until colorless. *DO NOT REFILL
THE BURRETE. Record the volume of HCl 0.5 N
consumed as “A”

Add 5 mL formaldehyde (the pink color will return) and

3 continue titrate until colorless. Record the volume of
HCl 0.5 N consumed as “B”

Add one drop of MO indicator and continue titrate to an

4 orange and point. Stop the titration. Record the volume
of HCl 0.5 N consumed as “C”
Soda Content Formula of Calculation

2𝐴 − 𝐵 𝑥 𝑁 𝑥 31
✓ Sodium Hydroxide (g/L) = 𝑉
2 𝐵 − 𝐴 𝑥 𝑁 𝑥 31
✓ Sodium Sulphide (g/L) = 𝑉
𝐶 − 𝐵 𝑥 𝑁 𝑥 31
✓ Sodium Carbonate (g/L) = 𝑉
𝐵 𝑥 𝑁 𝑥 31
✓ Total Active Alkali (g/L) = 𝑉
𝐶 𝑥 𝑁 𝑥 31
✓ Total Titrable Alkali (g/L) =
𝑉
𝑁𝑎2𝑆
✓ %Sulphidity =
𝑁𝑎𝑂𝐻 + 𝑁𝑎2𝑆
𝑁𝑎𝑂𝐻
✓ %CE =
𝑁𝑎𝑂𝐻 + 𝑁𝑎2𝐶𝑂3
Total Suspended Solid of Liquor

• Number of impurities in green liquor, such as : carbon, lime mud and

inorganic material

• To determine the suspended solid in the white and green liquor as indication
of the efficiency of green liquor and white liquor clarifiers
Total Suspended Solid of Liquor
Procedure Analysis
• Dry a glass micro fibre filter paper at 105°C ± 3° for approximately 1 hours,
cool in a desiccator for 5 minutes and weigh record in grams as “A’’

• Insert the glass micro fibre filter into a filter holder and clamp
securely and connect it into a 1000 mL filtering flask
• Stir the sample and transfer 300 mL of the sample (80±5°C) Record
the sample volume as”V”

• Moisten the filter with small amount of water, apply a vacuum and pour
the hot sample into the filter in funnel
• Rinse the filter with hot (60°C - 70°C)

• Oven dry the filter at 105°C±3°C for approximately 2 hours

• Cool in a desiccator for 10 minutes
• Weigh and record in grams as”B”
Total Suspended Solid of Liquor
Formula Calculation

𝐁 − 𝐀 𝐱 𝟏𝟎𝟎𝟎𝟎𝟎𝟎
TSS (mg/L) =
𝐕

B = dried sample weight (gr)

A = fiber filter paper weight (gr)
V = volume sample taken (mL)
Lime Mud Analysis
Dry Solid & Water Soluble Sodium
TEC/PLB-0071-PR

• To define the method of incoming inspection for purchased raw materials that
require laboratory analysis to verify the purchased product meets specification

• By the ratio of the mass sample of lime sludge after drying at a T= 150°C ± 3°C
to it is mass at the time sampling

• Water soluble sodium (in lime sludge) is sodium that is dissolved and washed
out from lime sludge when this is treated with by a specific procedure

• To define the method to determine of the water soluble sodium in the lime mud
filter
Lime Mud Dry Solid Analysis
Procedure
• Oven dry in an oven at 105°C ± 3°C for approximatel 30 minutes
CONTAINER • Cool in a desiccator for 5 minutes
• Weigh and record in grams as “C”

• Add approximately 10 grams of samples to the container

LIME MUD
• Weigh and record the sample in grams as “A”

• Dry in oven at 150°C ± 3°C for 60 minutes or constant

SAMPLE • Cool in a desiccator for 10 minutes
• Weigh and record the sample in grams as “B”
.
Lime Mud Dry Solid Analysis
Formula Calculation

𝑩−𝑪 𝒙 𝟏𝟎𝟎
% Dry Solid content =
𝑨

A = lime mud sample weight in gram

B = dried lime mud cake weight in gram
C = empty weight of the weighing container in gram
Lime Mud Water Soluble Sodium (WSS)
Analysis Procedure
TEC/PLB-0293-PR

Weigh a sample of about 15 grams of the lime mud. Add 500 mL of distilled
water. Stir vigorously with a magnetic stirer for 60 minutes.

Filter and collect the filtrate in another flask. Dilute a mL sample solution to
100 mL in volumetric flask. Add 10 mL caesium aluminium solution

Determine the sodium content of the sample solution from a calibration graph
obtained by plotting the emissions against the sodium content.
Lime Mud Water Soluble Sodium (WSS)
Analysis Procedure
TEC/PLB-0293-PR

Before filling up
Prepare a series of
to the mark add 10
5 calibration
mL cesium Use the distilled
solutions by
aluminium water as blank
diluting V mL of
Calibration Graph the standard
solution. Select solution with
the volume V so adding of cesium
sodium solution to
that the working aluminium
100 mL with
range of the flame solution
distilled water in
photometer is
volumetric flask
covered
Lime Mud Water Soluble Sodium (WSS)
Formula Calculation

5000. 𝑐. 10
WSS(%) =
𝐴. 𝑤. 𝑑

c = the concentration of sodium (mg/L)

A = volume of sample solution taken (mL)
W = mass of sample taken (gr)
D = (dry matter content of the sample (%)
Available CaO and Residual CaCO3

• Residual CaCO3 is how Many lime not change be CaO.

• To define the method of measuring the residual carbonate (CaCO3) content of

reburned lime.
Available CaO Analysis Procedure
RAP-TEC-C11-T

While continuing to stir,

Weigh a sample Remove the flask from add a few drops of
0,50 grams ± 0,01 the hot plate then add phenolphthalein (PP)
150 mL of carbon indicator and titrate with
gram of quick Transfer the sample to 0,5N HCL until
dioxide free distilled Place the flask on
lime. Record the a 250 mL Erlenmeyer colorless. Record
water. Add 15 grams of magnetic stirrer.
sample weight flask. Add 20 mL carbon volume(mL) of 0,5N
granulated sugar Replace the stopper HCL consumed as “V”
(grams) as “W” dioxide free distilled
water. Place the and stir for 50 and the normality as “N
Erlenmeyer flask on a minutes ± 10
hot plate and boil for ± 2 minutes
minutes.

𝑉. 𝑁. 2,8
% Available CaO =
𝑊
Residual CaCO3 Analysis Procedure
RAP/TEC/PLB-0074-PR

Tilt the mixing flask After ± 2 minutes the

so that the HCL liquid level should
Pipette 5 mL of 20% mixes with the lime stop moving, record
HCl into the other sample, then shake the reading on the
compartment of the the flask until the graduate burette of
mixing bottle. lime is decomposed the calcinometer
.

1 2 3 4 5 6
Weigh a sample 0,4 Open tap, the water Let stand for 1
grams ± 0,001 grams level in the graduate minute, then insert
of lime sample. burette should be at the mixing flask into
Transfer into one zero. Place the a cooling bath until
compartment of the rubber stopper firmly the bottle reaches
mixing flask into the top of the room temperature
mixing flask then
close the tap.
Specific Gravity of Green Liquor from
Recovery Boiler
1 Mix the sample thoroughly

Rinse a graduated cylinder

2 with the sample liquid and fill
the cylinder until overflowing

Record the hydrometer Immerse a thermometer into

reading as “S” and the sample and insert a
5 temperature as “T” 3 hydrometer slowly in to the
sample, then release and let it
stabilize

Read the hydrometer’s scale

4 and the temperature solution
Conductivity of Condensate

• Conductivity is a measure of the ability of a solution to carry

an electrical current

• To estimating the amount of residual chemical in pulp after

various bleaching sequence
Conductivity of Condensate
Analysis Procedure
RAP-TEC-A11-T (TAPPI T 252)

Turn on the conductivity meter and rinse with

de-mineralized water

Immerse the probe into the filtrate

Turn on the conductivity meter shake the probe

Rinse the electrode with de-mineralized water, then turn it

off
Quality Control Parameter Target of
White Liquor

Testing
No Parameter Test Method Unit Target Analysis Location
Frequency
1 TAA TEC/PLB-0069-PR Every 4 hour g/L 100-105 Central lab

2 TTA TEC/PLB-0069-PR Every 4 hour g/L 120-125 Central lab

3 %S TEC/PLB-0069-PR Every 4 hour % 29-32 Central lab

4 CE TEC/PLB-0069-PR Every 4 hour % 80±1 Central lab

Quality Control Parameter Target of
TSS of Recausticizing Area
No Sample Test Method Testing Frequency Unit Target Analysis Location

1 WL TEC/PLB-0068-PR Every 4 hour mg/L ≤20 Central lab

2 GLST 1, 2, 3 TEC/PLB-0068-PR Every 8 hour mg/L ≤1200 Central lab

3 GLC 1, 2, 3 TEC/PLB-0068-PR Every 8 hour mg/L ≤80 Central lab

4 X-FILTER 1, 2, 3 TEC/PLB-0068-PR Every 4 hour mg/L ≤30 Central lab

5 CD 1, 2, 3, 4, 5, 8, 9 TEC/PLB-0068-PR Every 4 hour mg/L ≤ 20 Central lab

6 WWL Line 1, 2 TEC/PLB-0068-PR Every 8 hour mg/L ≤ 100 Central lab

Quality Control Parameter Target of
Lime Mud Filter and Lime Kiln

Lime MUD Filter Quality Unit LMF 1, 2, 4, 5, 6, 7, 8, 9

Solid % 70±5
WSS % ≤0,5

Lume MUD Filter Quality Unit LMF 1, 2, 4, 5, 6, 7, 8, 9

CaO in Reburn Lime % ≥85,0
Res CaCO3 % 2±0,5
Conclusion

• Recausticizing and Lime Kiln Area testing parameter

✓ Soda Content of WL and GL
✓ TSS
✓ WSS
✓ Solid
✓ Available CaO and Residual CaCO3
• To controlling process in Recausticizing and Lime Kiln, which impacted a cooking
process at Digester.
Thank you for your attention!