Hot Lime Clarification in Cane Juice

Treatment and Its Relative Advantages

for the Production of Raw Sugar

G. Eggleston1, A. Monge2 and B. Ogier1

1 SRRC-USDA-ARS 2 Cora Texas Factory

New Orleans, Louisiana White Castle, Louisiana
U.S.A. U.S.A.
 Presentation Outline
¾ U.S. sugar industry – background information

¾ Large Factory Study:

* Description of different clarification

systems

* Results highlights

¾ Overall advantages and disadvantages of

cold, intermediate and hot lime clarification
processes
Louisiana Sugarcane Industry

¾ At the start of this research

in 1995 only 1 out of 19
factories operating hot
lime clarification with
the majority operating cold
lime clarification. After this
research, in 2004 over 85%
operate hot or intermediate
lime clarification
 Large Factory Study
of
Cold, Intermediate and Hot Lime
Clarification
 Factory and Study Information
¾ Study occurred in 2000 grinding season
¾ Season grinding rate was 521 short tons/h and ~1900 gallons/mi

¾ Milk of Lime (MOL) added (~12 baume)

¾ 4 ppm flocculant added
¾ Dorr Oliver 444 clarifiers 75% green

¾ 99% of the cane was billeted

25% burnt
Cold Liming
cold MJ ~38 oC

Filtrate
MOL ~65.5 oC

#1 MJ
#3 LJ
~38 oC Lime
Tank
Lime Incubator
Tank
Tank
~40.5 oC 8
min
Flash Tank Rt=4 min #2 Incub HJ
101 oC
amylase
#4 FHLJ Clarifier #5 CJ
Rt=1 min Rt=91 min 96 oC
#6 FES
Rt=30 min
Incubator tank
(8 min)
Lime tank
(2 min)

Lime tank
(2 min)
 Incubator tank

Lime
tank overflow

Lime
overflow tank
cold mixed juice
Intermediate Liming
cold MJ ~38 oC
82-93 oC Rt= 1 min
50%
Heater
50%
MOL Filtrate
~65.5 oC
#2 HJ
#1 MJ
#4 HLJ
~38 oC Lime
Tank
Lime Incubator
Tank
Tank
~65.5 oC 8 min

Flash Tank Rt=4 min #3 Incub HJ

101 oC
#5 FHLJ Clarifier #6 CJ
Rt=1 min Rt=91 min 96 oC
#7 FES
Rt=30 min
 Intermediate Liming Process

The Incubator Tank filtrate juice

cold mixed juice

50% heated mixed juice

pH Control for Cold and Intermediate Liming
Incubator
Tank

Lime tank

Lime tank
Hot Liming
cold MJ ~38 oC
82 oC Rt = 1 min
50%
Heater
50%
Filtrate
~65.5 oC
#1 MJ #2 HJ
~38 oC
#3 Incub HJ Incubator
Tank
Rt=30 sec ~65.5 oC Rt=12 min
Flash Tank Heaters
101 oC

#5 FHLJ
MOL Clarifier #6 CJ
#7 FES
Rt=91 min 96 oC Rt=30 min
 Flash Tank

9 cm

Lime
line
Hot water line
(for flushing)

Air control
To Splitter Box
pH Measurement System Sampling in Hot Liming

Flash heated limed juice

(Sample)

Cooler

pH
electrode
Instrumentation for Control of Hot Lime Clarification
 Summary of Operational Differences
Processing Cold Intermediate Hot
Parameter
Cold mixed juice 100% 50% 50%
(38 oC)
Heated mixed juice -- 50% 50%
(82-93 oC)
Temperature of 40.5 oC 65.5 oC 65.5 oC
incubated juice
Rt in incubation tank 8 min 8 min 12 min

Rt in lime tanks 4 min 4 min --

Where lime is added 1st lime 1st lime After flash

tank tank tank
 Result
Highlights
Turbidity Removal
 % Turbidity Removal (Season Average)
100
% Turbidity removal (MJ to CJ)

Intermed
Hot

Cold

90
Season Differences in Turbidity (ICU420nm)Values

COLD INTERM HOT

Mixed 57153 ± 60283 ± 59437 ±
Juice 10959a 8014a 5504a
Clarified
3165 ± 454a 1966 ± 354b 2100 ± 333b
Juice
Final Evap
6079 ± 911a 5022 ± 762b 4868 ± 358b
Syrup

Raw Sugar 755 ± 252 693 ± 311 445 ± 24

¾ Better factory control in both Intermediate & Hot liming

 In another 1999 factory study:
Cold
% Turbidity (420nm) Removal
98 Av ± SD
Cold Intermediate (30% heated juice) MJ 43417 ± 7032a
96
% turbidity removal

CJ 3952 ± 1450a
94
FES 6808 ± 1081a
92
90 Intermediate
88 Av ± SD

86 MJ 45165 ± 5095a
CJ 2028 ± 675b
84
Early Mid Late Average FES 4887 ± 659b

¾ Therefore, turbidity improvements gained by only pre-heating 30%

of the juice before lime addition!!!
Settling Behavior
Volume of floc (ml))
Settling Behavior

300

200
Initial Settling Rate (ISR)
100
in ml/min
0
11
0 0.5 1 1.5 2

% mud volume
Time (min) 10.8
10.6
10.4
10.2
Mud volume at infinity 10

(MVinf) 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7

1/time (min)

Break Point is the time in seconds it took for the flocculated, flash
heated limed juice to settle to half its original volume
 Settling Behavior
Season Average Data
ISR Breakpoint MVinf Visual
Process (ml/min) (sec) (ml) Floc
Shape

Small, fine
Cold 99 42 13.5
flocs

Intermediate 145 34 10.1 Large flocs

Medium to
Hot 98 48 12.1
large flocs
 Settling Behavior
Cold versus Intermediate Lime Clarification Study

Process Time in ISR MVInf

Season ml / min

Cold
Early 165 ± 60 17.2 ± 2.5
Mid 325 ± 96 10.2 ± 2.4
Late 277 ± 73 11.9 ± 1.1
Intermediate
Early 198 ± 105 14.6 ± 5.4
Mid 262 ± 62 13.0 ± 1.2
Late 333 ± 94 10.9 ± 0.5
 - - adsorbed colloidal
cane juice -
particle - -- - - - - - particles, i.e.,

- - - - - -- -
proteins, polysaccharides

- -
Lime + phosphate in juice

calcium
phosphate forms PO43-
- -- Calcium
Ca - -
2+
Phosphate
3-
-
PO4 Bridging
- - Ca
2+ Ca2+ -
- - --
- - - -
small floc

Precipitates impurities in the

clarification tank

Small floc formation in cold lime clarification

 - -
cane juice -
- -- - - - -- adsorbed colloidal
particles, i.e.,
particle
- --- -- - proteins, polysaccharides
--
Heat (only 30% of juice)
coagulated - - -
colloids - -
- - - -- - Heated Floc
- - -
-
Lime + phosphate in juice
calcium
phosphate forms PO43- - -
- -
Ca2+- - - -- - Calcium
3- - -
PO4 Phosphate
- - Ca2+ Ca2+ - - - -
- - Bridging
- -
- -
- -- -- - - - -
- - larger flocs
-

Larger floc formation in intermediate and hot liming

 Effect of Mud Volume on Initial Settling Rate

30
Mud Volume after 18 min

25

20

15

10

0
0 100 200 300 400 500
Initial Settling Rate (ml/min)

¾ Setting Rates: Initial mud to the factory overrides any

clarification process being used
Dextran
 Season Average Dextran (ppm/Brix) Data

Sample Cold Intermediate Hot

MJ 790 ± 480 804 ± 513 551 ± 136
HJ N/A 459 ± 277 400 ± 185
Incub J 529 ± 317 717 ± 539 582 ± 187
LH/HLJ 1001 ± 550 680 ± 451 N/A
FHLJ 362 ± 112 697 ± 716 361 ± 118
CJ 357 ± 183 492 ± 483 295 ± 140
FES 467 ± 172 582 ± 428 274 ± 65
Raw Sugar 432 ± 315 356 ± 88 158 ± 74
Dextran Summary

¾ Pre-heating of MJ before incubation

removes some dextran in Intermediate
and Hot liming

¾ Dextran is formed in the cold lime tanks

¾ Overall, dextran in hot liming raw sugar

is better
Lime Addition
 Differences in Lime Addition
Lime Added (rel. season av.)
Clarificatio (Ca as CaO; ppm/Brix)
n Change MJ
Process MJ LJ/HLJ/FHLJ to
LJ/HLJ/FHLJ

Cold 22.1 ± 0.7 39.9 ± 1.2 17.8

Intermediat
20.8 ± 2.0 39.7 ± 0.1 18.8
e

Hot 21.3 ± 2.2 28.8 ± 5.2 7.5

Factory Season Average Data

HOT LIMING

Only 0.46 kgs lime / ton cane in

2000 (Hot liming) compared to
0.58 in 1999 (Intermediate liming)
Color Formation and
Removal
 Color Removal and Formation
14

12

10
Icumsa color (ICU)
Thousands

8 cold
Intermediate
6 Hot

0
MJ Inc J FHLJ FES
HJ LJ CJ Raw Sugar
Sam ple
pH
 pH
8

Week 1
7
C o ld
pH

I n te r m
6

5
M J in c u b J FHLJ FES
HJ LJ CJ Raw Sugar

Week 2
7
C o ld
pH

In te r m
H o t
6

5
M J in c u b J F H L J F E S
H J L J C J R a w S u g a r

Week 3 Target FES pH

8

7
C o ld
in Week 3
pH

In te r m

6
H o t
Interm and
5
Hot increased
M J in c u b J F H L J F E S
H J L J C J R a w S u g a r
Sugar Losses
 Sucrose Losses

% Sucrose lost = ( (% Glu)out - (%Glu)in ) . MWSUC X 100

Brix Brix
---------------------------------------
(% Suc) in X MWGlu
Brix

Shaffler et al, 1986

Sucrose Across Across Across Across Total
Incubat Flash Clarifier Evaps
Losses Tank Heater s

Cold 0.0 0.64 0.55 1.03 2.22

Early Interm 0.0 0.33 0.19 0.90 1.41
Hot -- -- -- -- --
Cold 0.0 0.25 0.71 0.23 1.19
Mid Interm 0.0 0.0 0.88 0.32 1.20
Hot 0.25 N/a 0.41 0.64 1.30
Cold 0.0 0.40 0.42 0.25 1.07
Late Interm 0.0 0.0 0.46 0.09 0.55*
Hot 0.0 N/a 0.11 0.0 0.11*
 U.S. $$$ Sucrose Losses – Season Averages
ONLY APPROXIMATIONS
Across Across Across Across TOTAL
Incubator Flash Clarifiers Evaps
Heater

$176,920 $222,178 $209,834 $608,932

Cold

Inter $94,640 $213,949 $176,920 $485,509

m

Hot $18,515 N/a $181,034 $126,724 $326,273

Typical Glucose and Fructose Profiles Across the
Grinding Season
% Glucose + Fructose (Brix basis) 5.5

4.5
Cold
Hot
4

3.5

3
MJ LJ/HJ HLJ CJ FES
Sample Type
Silicate Removal
Silicate Concentrations

¾ No real differences amongst the

3 Clarification Systems
Starch
 Season Average Starch Concentrations
500

Amylase
400 addition
an last
300
evaporator
Cold
ppm/Brix

Inte rm
200 Hot

100

0
MJ HJ incub J CJ FES
Sam p le

¾ Starch is removed in incubation tank (HJ) because added

filtrate contains diastase enzyme from cane
Summary
 COLD LIMING
Advantages Disadvantages
¾ Color formation (~!0%) on
¾ Simple
liming
¾ Traditional
¾ High sugar losses
¾ Cheapest operation
¾ Excessive lime use
(no heating)
¾ Most erratic pH, color and
turbidity control
¾ Small flocs
¾ Least turbidity removal
¾ Clarified juice: high color
and turbidity
¾ Dextran formation in cold
lime tanks
 INTERMEDIATE LIMING
Advantages Disadvantages
¾ Fast settling (largest flocs) ¾ Extra juice heating
¾ High turbidity removal (only ¾ Excessive lime usage
30% of juice needs to be
pre-heated)
¾ Color removal good
¾ Clarified juice: low color
and turbidity, good control
¾ Starch and dextran removal
on pre-heating and incubating
juices
 HOT LIMING
Advantages Disadvantages
¾ Least sugar losses ¾ Requires high temperature
¾ Fast settling pH electrodes
¾ High turbidity removal ¾ Extra juice heating
¾ Less lime (~27%)
¾ No extra dextran formation
and some removal
¾ Very little or no measurable
color formation
¾ Clarified juice: low color
and turbidity, and good control
¾ Less heater incrustation problems
and better heat transfer
 OVERALL SUMMARY

Cold Intermediate

WORST BEST

Hot