Clarification I - Liming + Juice Heating PDF

12/3/2019
Outline
 Introduction to clarification
 Juice heating
 basic concept for juice heating (type of heat transfer / steam table)
 heat transfer (heat transfer rate / overall heat transfer coefficient)
 juice heater (shell & tube heater, plate heater, direct contact heater)
 Liming (Primary flocculation)

 type of lime
 coagulation vs flocculation
 Zeta potential
 reaction in defecation process
 pH control and problems in measurement
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White/raw sugar production (SUTECH)
White/raw sugar production (SUTECH)
Clarification I
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Introduction to clarification
Clarification process is the process used to remove impurities from
the juice to obtain clarified juice of high quality, with a minimum
turbidity, color and a low residual calcium (Ca2+) content. A number of
objectives need to be met including:
 To form flocs to trap all suspended matter, which can be settled at a
satisfactory rate
 To provide conditions of temperature, pH and ion concentration
which will maximize the precipitation of soluble impurities from the
juice
 To produce a settled mud which is amenable to further processing
 To maintain a clarified juice pH that will minimize inversion in the
subsequent evaporation operation.
 To kill or inactivate micro-organisms in the juice by heating
5
F. Beyen. Clarification. Handout of 35th International Raw Cane Sugar Manufactures’ Institute. May 29 – June 8, 2019. Nicholls State University. Thibodaux. Louisiana. USA
Major components of raw cane juice
 Sucrose, reducing sugars (glucose and fructose), monosaccharide
 Polysacharides (dextran, gums, starch) and trisaccharide
 Proteins, amino-nitrogen compounds
 Organic acids (aconitic, malic, citric), salts of organic acids (e.g. calcium
aconitate)
 Salts of inorganic acids (e.g. KCl, CaSO4, phosphates)
 Insoluble matter such as waxes, fats, bagacillo, soil, sand, and clay particles
Steps in juice clarification
 Juice screening to remove bagasse, sand, etc.
 Coagulation of proteins in the juice by heat
 Neutralization of the juice and precipitation of certain soluble impurities
 Separation of the precipitate by decantation and filtration to obtain a clear
juice
6
P. Rein. Cane Sugar Engineering. 2nd edition. Verlag Dr. Albert Bartens KG-Berlin. 2017
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Clarification has a direct effect on:
 Loss of sucrose in final molasses : when impurities are eliminated through
clarification, they go out as filter cake which has low sucrose content (0.3% of
sucrose in cane). On the other hand, if these impurities are not eliminated, they will
find their way in final molasses where they will entrain with them twice their weight
of sucrose (ratio of sucrose to ash being about 2:1).
 Viscosity of massecuites, running’s and molasses : viscosity increase due to
impurities has a great impact on process station capacity and on molasses exhaustion.
 Sugar quality : occlusion of impurities in the sugar crystal deteriorates sugar color
and filterability.
Essential conditions to obtain good clarification
 Constant juice flow
 Constant quality and concentration of additives (lime, flocculant)
 Constant temperature
 Constant pH 7
Types of clarification process
Process Reagents used Precipitate formed Type of sugar Purity rise
made (unit)
Defecation Lime + Calcium phosphate Raw sugar 0.75 – 1.0
(phosphate) (Ca3(PO4)2)
+ flocculant
Sulphitation Lime + SO₂ gas Calcium sulphite White sugar 1.07 – 2.0
+ flocculant (CaSO3)
Carbonation Lime + CO₂ gas Calcium carbonate Refined sugar 3.0 – 4.0
+ flocculant (CaCO3) by filtration
process
Phospho- Lime + Calcium phosphate Refined sugar
defecation phosphoric acid (Ca3(PO4)2) by
flotation process
Flocculant is a substance added to a suspension to enhance aggregation of the suspended particles

8
P. Rein. Cane Sugar Engineering. 2 nd edition. Verlag Dr. Albert Bartens KG-Berlin. 2017 / R.B.L. Mathur. Handbook of Cane Sugar Technology. 2nd Edition. Oxford & Ibh Publishing Company. 1981.
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Procedure for defecation process
 Addition of lime (CaO), to raise the pH value from 5.3 – 5.5 to
7.2-8.0 to get the clarified juice of pH 7.0 -7.3. This can be in
the form of milk of lime (MOL), lime-juice mixture, or lime-
syrup saccharate
 Heating to the boiling point, with flashing to remove entrained or
dissolved air
 The main precipitant is calcium phosphate (Ca3(PO4)2), which
forms the basis of flocs that adsorb much of the other precipitating
materials.
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Functions of clarifying agents
 P2O5 phosphate : minimum levels at 300 mg/kg juice
 Liming (primary flocculation)
 forms the primary calcium phosphate floc
 neutralizes acids
 reduces sugar inversion
 prevents destruction of reducing sugars
 prevents color generation
 Heat
 helps to deaerate juice
 reduces viscosity
 dehydrates protective colloid
 reduces the frictional drag on the settling particles
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Functions of clarifying agents
 Polymeric flocculants (secondary flocculation)
 increase the size of the calcium floc
 improve the floc characteristics for better filter cake handling
 produce good clarity (low turbidity) clarified juice
 produce good filterability of mud, with good clarity of filtrate
Note:
 Primary flocculation involves the linkage of colloidal particles by
precipitated calcium phosphate (Ca3(PO4)2)
 Secondary flocculation is the aggregation of the precipitate into a form
which settles out to leave clear juice
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Importance of phosphate content and other substances
 An amount of 300 mg phosphate/kg juice was considered the minimum
required to obtain a clear juice
 Phosphate content alone is not the critical factor in obtaining good
clarification, a good clarification depends on the ratio of phosphate to
certain other non-sugar in the juice
Phosphate content
R 
Content of SiO 2  Sesquioxides (Fe2 O3 and Al2 O3 )  HCl solubles
R < 0.15  poor clarification; high mud volume; no separate
between clear juice and mud
0.15 < R < 0.25  fair clarification; not brilliantly clear of clarified
juce but improve mud settling
R > 0.25  good clarification; brilliantly clear of clarified juice
and well mud settling
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Huletts Sugar Limited. Sugar Technology
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 Amino acids are not changed much by clarification, though at high pH
values they can react with reducing sugars to give increased color.
 Reducing sugars are also usually stable, though they can be destroyed at
high pH and temperatures in excess of 100 oC. The rate is just significant
at a pH of 6 but increases by a factor of 5 for each pH unit increase but
sucrose is inverted at low pH, high temperature.
 Waxes, gums and pectins are denatured but otherwise unchanged.
 Some inorganic acids, e.g. PO43- , silicates (SO42-) are partly precipitated
by the addition of Ca2+ ions.
 Contents of inorganic ions as K+, Na+ and Cl- are largely unchanged by
clarification. Ca2+ content increases temporarily but often ends up just
slightly above its initial value in raw juice. Mg2+ content drops by up to 20
%, depending on the final pH.
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System of liming
 Cold liming : raw juice at < 45 oC, lime saccharate (or MOL) to pH = 7.8,
heat to 102 oC, flash to 100 oC, add flocculant, clarify
 Warm liming : raw juice at < 45 oC, lime saccharate (or MOL) to
pH = 6.0, heat to 76 oC, lime saccharate (or MOL) to
pH = 7.8, heat to 102 oC, flash to 100 oC, add flocculant,
clarify
 Intermediate liming : raw juice at < 45 oC, heat to primary juice
(at 76 oC), lime saccharate (or MOL) to pH = 7.8, heat to
102 oC, flash to 100 oC, add flocculant, clarify
 Hot liming : raw juice at < 45 oC, heat to primary juice (at 76 oC),
heat to 102 oC, lime saccharate (or MOL) to pH = 7.8,
flash to 100 oC, add flocculant, clarify
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15
G. Eggleston, B. Legendre, M.A. Godshall. Sugar and Other Sweeteners. Springer International Publishing AG 2017.
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Basic concept for juice heating

 The objective of juice heating is to heat the juice up to a temperature a
few degrees above boiling point to allow the flash, which enables any
air in juice to be remove before the clarifier.
 The juice is usually heated in two or more stages, using low pressure
vapor in the first stage to improve steam economy.
 Juice heating is still mostly carried out using shell & tube exchangers or
tubular heaters, plate & frame heaters or plate heaters, and direct contact
heaters.
https://www.tantec- http://www.wermac.org/equipment/plateheatexchanger.html
group.com/en/tantalum/tanta https://www.haarslev.com/product
s/shell-tube-heat-exchanger/ https://www.s-k.com/steam-jet-
lum-heat-exchanger/
heaters/direct-contact-steam-jet- 17
P. Rein. Cane Sugar Engineering. 2 nd edition. Verlag Dr. Albert Bartens KG-Berlin. 2017 heaters.cfm

Types of heat transferred between a body and surroundings
 Latent heat is heat transferred in a
process without change of the body’s
temperature, but in a phase change
Q  m
https://www.quora.com/What-is-sensible-heat
 Sensible heat is the heat exchanged

by a thermodynamic system that
changes the temperature of the system
without changing some variables such
https://www.quora.com/What-is-sensible-heat
as volume or pressure
Q  mC pm t2  t1  m mass flow rate of boiling or condensing fluid (kg/s)
 latent heat of respective fluid (J/kg)
Cpm mean heat capacity at constant pressure (J/kgK)
t1, t2 temperature at position 1 and 2 18
https://www.daikin.co.uk/en_gb/faq/what-is-the-difference-between-sensible-and-latent-heat-1.html
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https://www.misumi-techcentral.com/tt/en/surface/2017/01/273-heat-saving-measures---steam-properties--1.html

Steam in industry
 Saturated steam : a steam that occurs when the liquid and gaseous phases
of water exist simultaneously at a given temperature and pressure.
Saturated steam is commonly used as a heating source for several
applications including reboilers, reactors, heat exchanges and other heat
transfer equipment.
 Superheated steam : a steam at a temperature that is higher than its

vaporization (boiling) point at the absolute pressure. It is steam which is
formed at the temperature which exceeds that of saturated steam at the
same pressure. It is used in turbines to improve thermal efficiency and
other uses (surface technologies, cleaning technologies, etc.)
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https://www.corrosionpedia.com/definition/1005/saturated-steam / https://www.corrosionpedia.com/definition/1050/superheated-steam
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Steam table is the table that summarizes water properties like boiling point,
specific volume, density, specific enthalpy, specific heat and latent heat of
vaporization.
specific volume enthalpy Internal energy Entropy
21

Superheated steam
22
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Heat always find a way to transfer from the higher to lower system until
the equilibrium is reached
T1
T2
 Conduction
 Convection
 Radiation
Object # 1 Object # 2
http://thegophysics.com/thermodynamics-basic-topics/ 23
https://www.machinedesign.com/whats-difference-between/what-s-difference-between-conduction-convection-and-radiation
Juice heating : Heat balance

Heat balance in each fluid stream
Condensing Ts
Ts
t2
Temperature
Cold fluid
t1
0 L
Distance along heater
Heat flow in juice Q  mC pm t2  t1  Q

m
heat flow rate or heat duty (J/s, W)
mass flow rate of juice (kg/s)
Cpm mean heat capacity of juice (J/kgK)
Heat flow in condensing stream Q  mS  t1 temperature of inlet juice
t2 temperature of outlet juice
Q  mC pm t2  t1   m
mS steam flow rate (kg/s)
In absence of heat loss  latent heat of respective fluid (J/kg)
Note : Please see the Cpm of juice and other properties in attached document. 24
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Juice heating : Heat balance

Heat transfer rate between condensing steam and juice
t2
Q  UAFT Tlm  UAFT
Ts  t1   Ts  t2 
T  t 
ln s 1
T 
Steam Ts
s  t2
Q Q t 2  t1
Q  UAFT
ln
Ts  t1 
Ts  t2 
Condensate Ts Q heat flow rate or heat duty (J/s, W)
U overall heat transfer coefficient based on area A (W/m2K)
t1
A outer surface area of tubes
If U is not constant, but varies significantly through the heater
Q  UAFT Tlm  AFT


k 2 Ts  t1   k1 Ts  t 2  k1, k2 local heat transfer coefficient
k 2 Ts  t1  at the end of heat exchanger
ln
 
(W/m2K)
k1 Ts  t 2
FT = 1 for single pass heater 25
Juice heating : correction factor F chart

T
T
26
https://sistemas.eel.usp.br/docentes/arquivos/5817712/LOQ4086/lmtd.correction.factor.pdf
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Juice heating : correction factor F chart

T
T
27
https://sistemas.eel.usp.br/docentes/arquivos/5817712/LOQ4086/lmtd.correction.factor.pdf
Juice heating : Shell & tube heater

Overall heat transfer coefficient
Saturated Conden- Tube Turbulent
steam sate wall Scale Film core juice Overall heat transfer coefficient
1 1 rf ,o ln(ro / ri ) rf ,i 1
Ts     
ho UA ho Ao Ao 2kA Ai hi Ai
k rf,i
For steam condensing, rf,0  0
Temperature
rf,o

hi
t
1 1 rf ,o ln(ro / ri ) rf ,i 1
    
 UA ho Ao Ao 2kA Ai hi Ai
Distance
Overall heat transfer coefficient in tubular heater

hi, ho heat transfer coefficient at inside and outside tube (W/m2K)
1 1 lnr0 / ri  rf ,i 1 rf,i , rf,o fouling factors on the inside and outside tube (m2K)
   
UA ho Ao 2kL Ai hi Ai k thermal conductivity of tube metal (W/mK)
ri, ro inner and outer radius of tube (m)
28
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1 1 lnr0 / ri  rf ,i 1
   
UA ho Ao 2kL Ai hi Ai
 Condensing steam resistance : for vertical tube

y  k 3f  2f gHˆ vap 
1/ 4
ho  0.943  Re < 350

  f LTd  T0  
 
z
 
1/ 2
 k 3f  2f g Td  T0 L 
Coolant
ho  0.003  Re > 350

  3f Hˆ vap 
Temperature  
distribution 1/ 3
T(y, z) Td  k 3f  2f g 
ho  1.76 Re 1/ 3   Re < 1,800
 2 
T0  f 
Steam 1/ 3
 k 3f  2f g 
movement ho  0.0077 Re 0.4   Re > 1,800
Conden-  2 
 f 
(z sate film
4w
Film)thickness Re 
D f 29

1 1 lnr0 / ri  rf ,i 1
   
 Condensing steam resistance : for horizontal tube

1/ 3
 k 3f  2f gL 
hO  0.954  Re  1,000
  w 
 f 
if Td - T0 is small
1/ 4
 k 3f  2f gHˆ vap  4w
hO  0.725  Re 
  f DTd  T0   2 L f
 
Highly flow rate (Rev > 20,000 and Ref > 5,000)
0.8
k f Pr1f / 3  
1/ 2
 
ho  0.026 Re f  Re v  l  
D   v  
4w f 4 wv
where Re f  and Re v 
D f Dv 30
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1 1 lnr0 / ri  rf ,i 1
   
Scale in juice heater

 Resistance of scale
 10.763   time (h)
rf ,i  0.0035 0.8 1   u juice velocity
 u3 
 Juice film resistance

0.14
 k    Lime scale
hi  0.0234  Re b0.8 Prb1/ 3  b 
 Di   0 
when Reb > 2104; L/Di > 10
 b Di v C p ,b  b
Re b  Prb 
b kb
31
https://en.wikipedia.org/wiki/Limescale#/media/File:Kesselstein_k.jpg
For design purposes, heat

transfer coefficient in a fouled
condition prior to cleaning
needs to be considered.
 For secondary heating using

vapor 1, a conservative
design value of 1.0 kW/m2K
is often chosen.
 For primary heating using
vapor 2, a value of 0.9
kW/m2K is used
32
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Effect of juice velocity
Juice velocity affects in the
performance of heater
performance in two aspects
 Velocity in the tube affects the

thickness of the boundary
layer, thus affecting heat
transfer.
 The velocity in the tube affects
the rate of scaling inside the
tube, which has the major
effect on the overall heat
transfer
33

Pressure drop in tubular heater (p)
fNLu 2 u 2 Nu 2  fL 
p   2.5 N    2.5 
2 Di 2 2  Di 
pressure drop pressure drop due to
due to flow in the return headers
tube associated with
contraction expansion
and flow reversals
 primary heating,  = 1.07

0.14
  
   
 0  secondary heating,  = 1.03
Nu 2  fL 
In terms of head drop (m) H    2.5 
2g  i
D  
p pressure drop (Pa) f Moody friction factor

N number of passes L tube length (m)
Di inside diameter of tube (m)  juice density (kg/m3)
34
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(f)
(limit curve)
35
https://en.wikipedia.org/wiki/Moody_chart

Vertical shell & tube heater
36
https://www.tantec-group.com/en/tantalum/tantalum-heat-exchanger/
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Horizontal shell & tube heater
37
https://www.indiamart.com/proddetail/industrial-heat-exchangers-13947906188.html

Juice passes / back side of heaters Juice in and out
16 Pass for Shell & Tubes (Horizontal) 16 Pass for Shell & Tubes (Horizontal)
The back or bottom side of the

tube sheet
two passes per each compartments Only one pass inlet & outlet side
38
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Sutech design
To in-line mixer
39

Juice heater
40
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Juice heating : Plate heater

The plate heater is a pack of thin plates arranged in a frame. The space
between each alternate plate is open to the same fluid. The plates are
corrugated, which gives them strength and helps promote turbulent flow.
41
https://www.alfalaval.com/microsites/gphe/tools/gphe-features-to-look-for/
42
http://www.sugarprocesstech.com/plate-heat-exchanger/
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Fluid circulation
Series flow
Looped (parallel) flow)
43
A. Ibarz, G.V. Barbosa-Cánovas. Unit Operations in Food Engineering. CRC Press. 2013

Basic unit of a plate type heater
Ts Global heat balance
t1 t2
Q  ms   mC pm t2  t1 
Heat transfer equation

Q  UAFT Tlm  UNAp FT Tlm
Ts FT = 1 for single pass heater
Total heat flow transferred Q  ms   U NAp FT Tlm
mS mass flow rate of steam

Cpm mean heat capacity of juice
A total heat transfer area
Ap area of one plate
N number of plate in which there is heat transfer
44
A. Ibarz, G.V. Barbosa-Cánovas. Unit Operations in Food Engineering. CRC Press. 2013 (thermal plate)
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Overall heat transfer coefficient in plate heater (U)
e
Ts Overall heat transfer coefficient

hh
k rf,c 1 1 e 1
  r f , h   r f ,c 
Temperature
rf,h U hh k hc
hc
t
Saturated Conden- Plate Scale Film Turbulent
steam sate wall core juice
1/ 4
 k 3f  2f gHˆ vap 
For condensate film hh  0.943  Re < 350
  f LTd  T0  
 
 
1/ 2
 k 3f  2f g Td  T0 L 
hh  0.003  Re > 350
  3f Hˆ vap 
w mass flow rate of falling film  
(condensate) on the tube (kg/s)
4w
W plate width Re 
 fW 45

Overall heat transfer coefficient in plate heater (U)
For juice side, with turbulent flow (Re > 400)
0.14 Gp mass flow rate per unit cross-sectional
hc De  
 0.26 Re 0.65 Pr 0.4   area (Gp = W/Af)
kf  0  W mass flow rate
Af cross-sectional area for flow
G p De Cp De equivalent (hydraulic) diameter (taken
Where Re  and Pr 
 k as twice the gap between the plate)
Pressure drop in plate heater (p)

 Lp  v 2p
p  8 j f   Lp the path length
 De  2 vp velocity (Gp/)
jf  1.25 Re 0.3
46
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Options for plate design for juice heating
Conventional plate arrangement
This plate has high heat transfer

coefficients above 3,000 W/m2 K
Free flow system plate incorporating a maximum gap of 5.4 mm
A “wide gap” heater with a gap of

6 to 16 mm is normally used because of the
propensity for small pieces of bagasse fiber
to block the inlet, resulting in the heat
reduction of heat transfer coefficients to
below 2,000 W/m2K 47

Advantages:
• high heat transfer coefficients
• high area density, giving a smaller heater for the
same duty
• low liquid holdup
• lighter for the same duty, leading to lower installation costs

• quick response and facilitate close temperature control
• possible to increase capacity by adding additional plates depending on
the size of the frame
• economically feasible due to a close approach temperature than that used
in shell and tube heaters
48
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Disadvantages:
• not practical to clean these heaters mechanically,
because the gaskets are easily damaged
• require chemical cleaning
• need to replace gaskets occasionally
• prone to blocking with fibrous bagasse particles, thus require periodic

reversing of flow
• high shear stress at the same pressure drop compared with shell and tube
heater
49
Juice heating
Comparison of plate heater and shell & tube heat exchanger
Cleaning time
Fouling coefficients
Manufacturing costs
S&T
Installation space GPHE
Operating weight
Heat transfer area
Fluid content
0.0% 10.0% 20.0% 30.0% 40.0% 50.0% 60.0% 70.0% 80.0% 90.0% 100.0%
50
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Juice heating : Direct contact heaters

For direct contact heater, the hot and cold streams are brought into contact
in counter current way without any separating wall.
Assumption: the quantity of incondensable

Juice in gas out is so small
m1 (kg/h)
t1 (oC) Mass balance : m1 + ms = m2
Enthalpy balance :
enthalpy in = enthalpy out
ms (kg/h) ms hs  m1C p t1  m2C p t 2  ms  m1 C pt2
Ts (oC)
Steam m1C p t 2  t1 
Rearrangement ms 
hs  C p t 2
m2 (kg/h) Heater juice out
t2 (oC)
hs enthalpy of steam
51
Juice heating : Direct contact heaters

Advantages:
 much closer temperature (1 to 3oC) than that with tubular heater
 lower pressure vapor can be used for heating
 much cheaper, with no tubes, tube plates
 able to handle solids in the juice with out blocking
 require less floor space
 not required a condensate removal system
 no fouling or necessity to clean the heater
 no need a stand-by heater
 short retention time leading to low sugar losses
 zero head loss, thus reducing the power requirement of the pump
Disadvantages:
 The condensate of the heating media (vapor) added along with heated media
(juice) is an extra load on evaporation system.
 Operation should take care while using low pressure vapors (vapor 3 or 4) as
a heating media to avoid entertainment.
52
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(Primary flocculation)
53
Liming (Primary flocculation)

The purpose of liming is to prevent inversion, maximize the removal of
impurities and increase sedimentation, which will affect positively to the
filtration performance.
 Composition of a good quality quicklime (CaO) in South Africa
CaO 85 – 90% Silica (SiO₂) < 2%
Iron oxide (Fe₂O₃) < 2% Aluminum oxide (Al₂O₃) < 2%
Magnesium oxide (MgO) < 2% Quicklime in
 Poor quality of lime causes: Thailand
 high percentage of Si in lime, retarding the settling of juice in juice

clarifier, thus poor clarification effect is achieved
 high percentage of MgO, retarding filtration and rate of settling
again poor clarification effect
 darkening in juice due to an increase of gummy substances, ash,
which affects adversely the exhaustibility of final molasses
54
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Quicklime in Thailand
Golden Lime Public Thai Poly Chemicals
Co., Ltd Co., Ltd.
Average size 1.4 – 4 inch, 0.2 – 2 mm, Powder 150 m
CaO (%) 82 – 90 > 90
CaCO3 (%) 0–6
MgO (%) 1–3
Fe2O3 (%) 0–1
SiO2 (%) 0–1
Al2O3 (%) 0–2
Bulk density (kg/m3) 750 – 1,000
Color White-grey White fine powder
1.4 – 4 inch 0.2 – 2 mm
55
https://www.irplus.in.th/Listed/SUTHA/lump_lime.asp

Type of lime : milk of lime (MOL) and lime saccharate

 MOL CaCO3 
 CaO H

2O
 Ca(OH)2
quick lime hydrated lime (MOL)
(suspension)
Concentration of MOL
Degree Density g CaO/L g CaO/ g water /
For raw sugar factory,
Baumé (kg/m3) 100 g water g CaO MOL is prepared at a
(°Bé) concentration of
1 1,007 7.5 0.74 133 6-10 °Bé
2 1,014 16.5 1.64 60
3 1,021 26 2.54 38
5 1,036 46 4.43 21.6
7 1,051 65 6.18 15.6
10 1,075 94 8.74 10.4
15 1,116 148 13.26 6.5
20 1,162 206 17.72 4.6
56
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Milk of lime preparation system
http://healthandbeautylifestyle.com/wp-
content/uploads/2016/04/lime-water-cure-for-cancer-and-
treatment-for-other-serious-diseases.jpg
57

MOL or saccharate (with clear juice) : preparation with hydrated lime
58
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Type of lime
 Lime saccharate CaO + C12H22O11  C12H22O11CaO

sucrose mono-calcium saccharate
(solution)
 To obtain mono-calcium saccharate, the ratio of sucrose to CaO is 6:1.

 In practical, a ratio of 7:1 is adopted to ensure an excess sucrose and
thus avoid the tricalcium saccharate (C12H22O113CaO), which are
insoluble
 Advantages : better clarification, higher clarity and purity obtained (less
turbidity), less lime usage, less scale in evaporators
 Disadvantages : increase mud, mud filter losses
59

Lime saccharate preparation system
Valve Valve
Clear juice or syrup Milk of lime
Mixing
tank
pH meter Variable speed

pump
Milk juice at 70 oC
pH electrode Pump
60
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Comparison liming method
MOL Lime saccharate
Forms Suspension Solution
Complete reaction >4h <1h
Reaction and scale Incomplete reaction Complete reaction
results in scaling in heat with less scale
exchangers tubes
Maintenance Require frequent cleaning Less
and constant maintenance
Turbidity of clarified More Less
juice
Sucrose loss More Less
Upstream effect Low Baumé MOL affect Less
evaporator capacity
Mud volume Less mud volume More
61

Comparison of lime saccharate
clarification with MOL, showed
(Doherty et al. 2002):
 lower turbidity, phosphate, and
protein in clarified juice with lime
saccharate
 slightly lower initial settling
velocity of the flocs
 a 10% increase in mud levels
 similar calcium, magnesium,
silica, polysaccharide contents in
clarified juice.
62
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A study of juice clarification by
Sahadeo et al. (2002) reported that
 the initial turbidity of clarified

juice produced by saccharate
liming is lower than that from
MOL.
 The turbidity of both increase
on concentration by
evaporation, but the use of
saccharate still results in lower
turbidity values
63

Sutech design (PT Prima Alam Gemilang)
To in-line mixer
Amount of CaO 0.7038 kg/ton cane

Amount of H2O 10.007 L/kg lime
Amount of raw syrup 250 wt.% MOL 64
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Lime slaker
65

Lime tank
66
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Lime saccharate preparation tank
67

Liming tank
68
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Coagulation vs flocculation
Coagulation is destabilization of colloids by addition of chemical or
coagulant (usually higher cationic salts) that neutralize the negative charges
by rapid mixing.
Flocculation is the agglomeration
of destabilized particles into a large
size particles known as flocs,
which can be effectively removed
by sedimentation. The de-
stabilization is brought about by
physical techniques such as mixing
of the solution, and also sometimes
by the addition of polymers.
69
https://www.slideshare.net/LokeshSaini3/ppt-coagulation-and-flocculation

Coagulation mechanism Flocculation mechanism
70
https://sswm.info/sswm-university-course/module-6-disaster-situations-planning-and-preparedness/further-resources-0/coagulation-flocculation
35
12/3/2019

Zeta potential : the potential difference between the dispersion medium
and the stationary layer of fluid attached to the dispersed particle.
Significance of zeta potential
 indicates the degree of repulsion
-
between adjacent, similarly charge
- particles in a dispersion
-  a high Zeta potential (+ or -) : stability
- -  a low Zeta potential : flocculation
(because attraction exceeds repulsion,
-
and the dispersion breaks)
71
https://www.slideshare.net/deepakrajput/zeta-potential

Zeta potential
The most important factor that affects zeta potential is the pH of the medium.
Other factors include ionic strength, the concentration of any additives, and
temperature.
 The point where the plot
passes through zero zeta
potential is called the
“isoelectric point”.
 The isoelectric point is
the point where
aggregation is most
likely and hence the
colloidal system is least
stable. 72
Zeta potential - An introduction in 30 minutes.Technical note of Malvern Instruments Limited. 2015
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Reaction in defecation process
 Two following reactions take place simultaneously
Ca2+ + K2HPO4 → CaHPO4 + 2K+
CaHPO4 + Ca2+ → Ca3(PO4)2 + H+
 In raw juice, protein is denatured by heating and then coats the solid
particles and the phosphate flocs, and imparts an apparent negative
charge.
73
Huletts Sugar Limited. Sugar Technology / R. Simpson. The chemistry of clarification. Proc S Afr Sug Technol Ass. 1996; 70: 267

 If calcium ions (Ca2+) is introduced in the form of lime when adjusting
the pH. The reaction of organic acids with lime reduces the effect on the
lowering of the Zeta potential. The Ca2+ ions adsorbed at the juice particle
surfaces act as nuclei for this precipitation and the impurities become
incorporated into the coagulum with the Ca3(PO4)2 acting as bridges
between the impurity particles.
74
R. Simpson. The chemistry of clarification. Proc S Afr Sug Technol Ass. 1996; 70: 267
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12/3/2019

Mechanism for hot lime clarification of sugarcane juice
75

Setting of particle (Stokes’ law)
Drag force (Fd) Fd  6ru
R g  p   J 
4 3
Gravity force (Fg) Fg 
3
At terminal velocity Fg = Fd
g  p   J d p2
ut 
18
ut settling velocity or terminal settling velocity (m/s)
dp diameter of the particle (m)
p density of the solid particles (kg/m3)
J density of the liquid juice (kg/m3)
 viscosity of the liquid juice (Pa.s)
g acceleration due to gravity (m/s)
76
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 The success of the primary flocculation is dependent upon the extent of
the calcium phosphate precipitation and the concentration of the calcium
and phosphate ions.
 It is generally accepted that phosphate levels (P2O5) of approximately
300 ppm are required for good clarification, and dosing with 80%
commercial H3PO4 is done when levels are low and processing and
clarification problems are experienced
 Much attention is given to pH control since pH < 7 results in losses due
to sucrose inversion while pH > 8 leads to degradation of reducing
sugars which increase color formation
 Although heating has a significant part to play in clarification, the
superheating is not advantageous. The temperatures just above the
boiling point (104 oC) are the maximum for good practice
77

 The CaO content of clarified juice is a function of the CaO content of raw
juice, organic acids present in the original juice and acid formed in the
clarification process
78
G.H. Jenkins. Introduction to Cane Sugar Technology. Elsevier. 1966. pp.172-188
39
12/3/2019
Effect of lime on the removal of different non-sugars in clarification

79
G.H. Jenkins. Introduction to Cane Sugar Technology. Elsevier. 1966. pp.172-188

What is the pH and pH meter?
 pH (potential of hydrogen ion) is a unit of measure which describes the
degree of acidity or alkalinity (basic) of a solution. The pH value is in the
range of 0 to 14.
 A pH meter is a scientific instrument that measures the H+ concentration in
water-based solutions, expressed as pH.
pH   log H   
A solution containing
more H+ ions remains
acidic, while the solution
containing more OH-
water @ 25 oC
ions remains alkaline
https://www.slideshare.net/ShreyaAhuja2/ph-meter-54084084
80
https://www.pharmaguideline.com/2015/08/principle-and-working-of-pH-probes.html / https://in.omega.com/prodinfo/ph-meter.html https://www.slideshare.net/ShreyaAhuja2/ph-meter-54084084
40
12/3/2019

pH measurement
 A pH meter will be made up of a glass probe, containing two electrodes; glass
sensor electrode and reference electrode
 glass sensor electrode (ex. AgCl cover Ag wire) has a bulb made up of
porous glass or permeable gas membrane coated with silica and metal
salts (alkaline), filled with a pH 7 buffer solution.
 reference electrode (Ag/AgCl) has a bulk made of a non-conductive glass
or plastic, filled with saturated KCl solution
 When the probe is placed in a solution, H+ ions accumulate around the bulb
and exchange with the solid membrane, thus generating the potential at glass
membrane/solution interface that is captured by Ag wire.
 This generated potential is converted into the pH value by comparing with
the potential of reference electrode.
E glass electrode  E   RT / 2.303F log a H 
81
https://www.pharmaguideline.com/2015/08/principle-and-working-of-pH-probes.html / https://in.omega.com/prodinfo/ph-meter.html https://www.slideshare.net/ShreyaAhuja2/ph-meter-54084084

Combination pH electrode
 Solution acidity 
 H+ concentration 
ex. Ag/AgCl
 voltage 
 pH 
Saturated KCl solution
Glass or plastic
 Solution alkalinity 
pH 7 buffer
 H+ concentration 
 (OH- conc. )
Ag/AgCl
 voltage 
Porous ceramic
 pH 
H+ sensitive coating
82
https://www.ysi.com/ysi-blog/water-blogged-blog/2019/02/anatomy-of-ph-electrodes
41
12/3/2019

pH control in juice liming
Liming is controlled to obtain a limed juice pH, which can vary between
7.2 to about 8.0 to give a clarified juice pH between 7.0 and 7.3 or, as
dictated by local conditions.
In order to achieve a stable control of pH the following points should be
aimed at
 low variation of the juice flow
 stable concentration of the MOL or lime saccharate
 complete mixing of lime and juice
 if dosing is done by means of a regulating valve, the size of the latter
should be such that it is 60 to 80% open during normal operation
 MOL or lime saccharate should be sieved to get rid of sand or foreign
matter, which can be damage the pH electrode
83

pH control in juice liming
 use of a pH electrode that can resist high juice temperature. If such
an electrode is not available, the juice going to the electrode must be
diluted with water at pH 7.0 to cool it down to a temperature lower
than 70°C.
 pH electrode must be calibrated
regularly
 check the cleanliness of the pH
electrode
 when comparing juice pH of different
factories, be sure that these values are
obtained at the same temperature
84
42
12/3/2019

Problems in pH measurement : effect of temperature
For water : H2O (l)  H+ (aq) + OH- (aq)
Ionization constant (Kw) of water
 25 oC: Kw = [H+][OH-] = 1.00810-14  neutral point = pH 7.0
 100 oC; Kw =[H+][OH-] =51.310-14  neutral point = pH 6.1
T (oC) Kw (mol2/dm6) Neutral pH
0 0.11410-14 7.47
10 0.29310-14 7.27
20 0.68110-14 7.08
25 1.00810-14 7.00
30 1.47110-14 6.92
40 2.91610-14 6.77
50 5.47610-14 6.63
100 51.3010-14 6.14
85

For cane sugar mill applications (Schaffler 1987)
dpH
 0.0339  0.015pH 25  0.0017pH 225
dt
At elevated temperatures, the pH is lower than the room temperature
measurements suggest. The pH at operating temperature is
pH  pH 25  t  25
dpH 7.5
pH = 5 @ 25 oC
dt 7.0 pH = 6 @ 25 oC
pH = 7 @ 25 oC
6.5
t temperature (oC)
6.0
pH value
pH25 value of solution pH at 25 oC

5.5
In practice 5.0
40 oC < T < 120 oC 4.5
5.5 < pH < 7.5 4.0
0 < Bx < 65 25 35 45 55 65 75 85 95
Temperature (oC) 86
43
12/3/2019
Control items and daily report

Sutech design
Limed juice pH : 7.50 - 8.20
Daily report (KI2)
87
Thank you for your attention

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please follow the next episode
let’s discuss about this topic
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12/3/2019

 Liming (Primary flocculation)

White/raw sugar production (SUTECH)

White/raw sugar production (SUTECH)

Flocculant is a substance added to a suspension to enhance aggregation of the suspended particles

Basic concept for juice heating

Basic concept for juice heating

 Sensible heat is the heat exchanged

Basic concept for juice heating

Basic concept for juice heating

 Superheated steam : a steam at a temperature that is higher than its

Basic concept for juice heating

Basic concept for juice heating

Basic concept for juice heating

Juice heating : Heat balance

Heat flow in juice Q  mC pm t2  t1  Q

Juice heating : Heat balance

If U is not constant, but varies significantly through the heater

Q  UAFT Tlm  AFT

Juice heating : correction factor F chart

Juice heating : correction factor F chart

Juice heating : Shell & tube heater

Overall heat transfer coefficient in tubular heater

Juice heating : Shell & tube heater

 Condensing steam resistance : for vertical tube

ho  0.943  Re < 350

ho  0.003  Re > 350

Juice heating : Shell & tube heater

 Condensing steam resistance : for horizontal tube

Juice heating : Shell & tube heater

Scale in juice heater

 Juice film resistance

when Reb > 2104; L/Di > 10

Juice heating : Shell & tube heater

For design purposes, heat

 For secondary heating using

Juice heating : Shell & tube heater

 Velocity in the tube affects the

Juice heating : Shell & tube heater

 primary heating,  = 1.07

p pressure drop (Pa) f Moody friction factor

Juice heating : Shell & tube heater

Juice heating : Shell & tube heater

Juice heating : Shell & tube heater

The back or bottom side of the

Juice heating : Shell & tube heater

Juice heating : Shell & tube heater

Juice heating : Plate heater

Juice heating : Plate heater

Juice heating : Plate heater

Looped (parallel) flow)

Juice heating : Plate heater

Heat transfer equation

Ts FT = 1 for single pass heater

Total heat flow transferred Q  ms   U NAp FT Tlm

mS mass flow rate of steam

Juice heating : Plate heater

Ts Overall heat transfer coefficient

Juice heating : Plate heater

Pressure drop in plate heater (p)

Juice heating : Plate heater

This plate has high heat transfer

A “wide gap” heater with a gap of