ChElec 501

Sugar Engineering 2
Clarification-Phosphatation
PHOSPHATATION
 Separation mechanism is fundamentally different
from carbonatation.
 In phosphatation,the principal mechanism is
flocculation, while in carbonatation – mainly
inclusion of impurities within the calcium carbonate
crystals
 Phosphatation relies on the formation of flocs
formed by the addition of flocculants, captures
the fine colloidal matter and is separated by
flotation with dissolved air.
 The basic reaction in phosphatation process:
8Ca(OH)2 + 6H3PO4  Ca8H2(PO4)6 +16H2O
SUGAR REFINERY PROCESS
CLARIFICATION BY PHOSPHATATION
RAW SUGAR

AFFINATION

MELTER

TALOFLOC / 3 STAGE SCUM

PHOSPHATATION DESWEETENING

DEEP BED
FILTRATION
FILTER
RECOVERY
BOILING CAKE
ION EXCHANGE
DECOLORIZATION

CRYSTALLIZATION /
PURGING

REFINED SUGAR
The “Talo-Phosphatation” Process
 The “Talofloc” Phosphatation was
developed by Tate and Lyle of England in
the late 70”s.
 It is a combination of traditional
Phosphatation process, modified
equipment and newly developed synthetic
processing chemicals.
Phosphatation Process
Chemical Reaction:
 8Ca(OH)2 + 6H3PO4 = Ca8H2(PO4)6 + 16H2O
 The octacalcium phosphate forms flocs which entraps
most of the impurities and color bodies.
 The primary calcium phosphate flocs formed are very
fine and takes time to form.
 Retention times in the Clarifiers takes as long as 45
minutes.
 The flocculants act as “bridges” to link the phosphate
flocs and form bigger secondary flocs.
The Use Of Flocculants
 The flocculants act as “bridges” to link the phosphate
flocs and form bigger secondary flocs.
 The flocculants are synthetic polyacrylamide of high
molecular weight (up to 26 million).
 Their negative charge binds with the positive sites of
the phosphate flocs.
 The secondary flocs formed are 1,000 x bigger than
the primary flocs.
 The flocculant is added after the acid and lime are
mixed.
The use of flocculants resulted to:
 Reduced operating temp. to 82 oC.
 Increased brix to > 65 oBx.
 Reduced retention time from 45 to 25 minutes
 Reduced sugar losses
 More brilliant and clear liquor.
The Use Of Surfactants
 The positively charged calcium phosphate removes
the negatively charged color and impurities by
attracting them.
 Surfactants or color precipitants are synthetic
chemicals which are a lot stronger
 than calcium phosphate, thus it
 attracts more impurities and color.
Chemical Reaction Model:

Color molecule Surfactant Surfactant-Color

Highly soluble Slightly soluble Complex
Insoluble
 The formed flocs although numerous are very, very fine
and takes time to settle.
 The addition of flocculant greatly increases the size of
the flocs and reduces the flocculation time.
 When used as an adjunct to Phosphatation, the
surfactants increases the % color removal up to 60 %.
The “Talo-Phosphatation” Process
The “Talofloc” Phosphatation is composed of the following
operations.
 Primary flocculation with lime and phosphoric acid.
 Aeration of the primary floc
 Secondary flocculation with the flocculant “Talofloc”.
 Precipitation of the color bodies and impurities with
the surfactant “Taloflote”.
 Filtration of the clear liquor through a Deep Bed Filter
(DBF).
The “Talofloc” Phosphatation consists of three
main processes:
1) Clarification of the melt liquor
2) Filtration of the clarified liquor
3) Recovery of sugar from the scum through de-
sweetening
8Ca(OH)2 + 6H3PO4 
Ca8H2(PO4)6 +16H2O
 TALOFLOC / PHOSPHATATION
PROCESS FLOW DIAGRAM

LIME TALOFLOC
FLOCCULANT SUCRATE
PREP. TANK DRUM
PREP. TANK HEATER

TALOFLOC
DOSING
PUMP CAVITATION
AERATOR

LIME
FLOCCULANT SUCRATE PHOSPHORIC
HOLDING HOLDING ACID

REACTION
TANK TANK

AERATION
CLARIFIER

TANK
FLOCCULANT LIME ACID

TANK
DOSING SUCRATE DOSING PUMP
PUMP DOSING
PUMP

HEAT
EXCHANGER
UNTREATED SCUM
LIQUOR

FLOW
CONTROL
MELT
LIQUOR CLARIFIED
TANK LIQUOR
TANK
CLARIFIED
LIQUOR

FEED PUMP

Figure 9
PHOSPHATATION
 Melt liquor heated in shell & tube HE to 87oC is
feed to the stirred reaction tank , where
phosphoric acid are automatically mixed in
proportion to the liquor flow rate, and lime sucrate
is also added to adjust the pH to 7.
 (Lime sucrate is prepared by adding melt liquor to
7oBe milk of lime in a ratio of 7:1).
 At this pH, the resultant calcium phosphate is in
its most insoluble form and flocculates the anionic
impurities (color, turbidity, suspended solids). This
complex is known as the primary floc.
 From the reaction tank, the liquor is gravity feed
into the aeration tank where the microscopic
particles of air dissolve into the liquor, and
physico-chemically attach themselves to the
primary floc.
 At this point a trace amount of flocculant
TALOFLOTE is dosed, and this coagulates the
primary flocs to form large, gelatinous, aerated
secondary flocs.
 This secondary flocculation takes place in the
circular TALO clarifier where the flocs rapidly rise
to the surface to leave a sparkling, brilliant
clarified liquor underneath.
 CLARIFICATION

INLET

SCUMS
OUTLET

Figure 8
 The clear liquor is drawn –off over a weir with
adjustable plate which control the clarifier liquid
level and sent to the Deep Bed Filter for filtration,
 The scum is constantly removed by a rotating
scraper blade and sent to the Scum Desweetening
Process.
TALO FLOTATION CLARIFIER

SCUM RAKE
SCUM TROUGH

WEIR BOX
SLEEVE

FLOCCULATION SYRUP OUTLET

CHAMBER

FLOTATION CHAMBER

MIXING
BAFFLES SYRUP INLET

Figure 11
The “Talo” Clarifier

Rake
Scums
The “Talo” Clarifier
Scum Discharge
Trough

Scum Rake

Scum Layer
Talo-Phosphatation” Process
 Controlled parameters:
 Melt liquor flow rate – x m3/hr. *Melt liquor brix – 65
max.
 Phosphoric acid dosage – 300 ppm P2O5 on liquors
solids *Phosphoric acid assay – 85%
 Lime sucrate dosage – pH 6.8-7.2
(Prepared by mixing 100 kg CaO with 1 m3 cold
water and 1 m3 raw melt liquor).
 Talofloc dosage – 300 ppm on solids
( Prepared by mixing 200 kgs of “Talofloc” with 6
m3 of raw melt liquor)
 Taloflote dosage – 10 ppm on solids
(Prepared by mixing 1 kg of “Taloflote” with 1 m3
of hot water).
 Weir box setting – controls the retention time in the
Clarifier (25 min. max) and the scum layer thickness
(6”-8” deep).
 Speed of the scum rake – 1-2 rpm.
DEEP BED FILTER
 It is a column packed with layers of different sized
particles decreasing in size from top to bottom of
the filter.
 The layers of filter medium are carefully chosen
both in terms of particle size and density.
 The clarified liquor is pumped via an orifice plate and
percolates down thru the filter media from the top
to bottom.
 The suspended solids are trapped in the interstitial
spacing of the media particles.
 When the concentration of the suspended particles
reach a critical value (DP = 15 psi, detected by the
pressure sensor), back-flush sequence is
automatically initiated.
 The filter is back-flushed in an upflow direction,
with the largest particles having the lowest density,
so that after backwashing the gradation of the
filter medium size is preserved.
 During backwash air sparging is initiated to agitate
the filter media and release the entrapped
suspended solids.
 Backwashing is done with the filtered liquor, so that
no additional sweet water is generated.
 The Deep Bed Filter is fully automated. Operation is
controlled by series of automatic valves, pumps, &
blowers regulated by a central programmable
controller, hence requires minimal supervision.
 The back-washings are returned to the process
buffer tank where they are eventually removed by
flotation in the main clarifier.
Deep Bed Filtration (DBF)
 Talo-Phosphatation comes with a
specially designed filter called DBF.
bone char
 It replaced the pressure filters sand
which use filter aid. sand
gravel
 It is constructed like a sand filter gravel
but uses carefully sized filter media. gravel

 There are usually 5-6 layers of gravel,

sand and bone char.
 The arrangement of the filter media ensures
complete removal of suspended particulates from
the liquor.
 Uses no filter cloths but the media is replaced
periodically (every 2 years)
 Can be operated singly or in a battery of several
units.
 Service cycle of up to 24 hours.
Deep Bed Filter
PROCESS FLOW DIAGRAM

DEEP
BED
FILTE
R

CLARIFIED
LIQUOR

HIGH FILTER FEED

LEVEL TANK OVERFLOW
BACKWASH
RECEIVING TANK HIGH
LEVEL FILTERED BACKWASH
LOW LIQUOR TANK COMPARTMENT
LEVEL
BACKWASH AIR
PUMP BLOWER
FILTERED
LIQUOR

FEED
PUMP
Figure 12
Deep Bed Filter
 PHOSPHATATION / DEEP BED FILTER
PROCESS FLOW DIAGRAM

LIME TALOFLOC
FLOCCULANT SUCRATE
PREP. TANK DRUM
PREP. TANK HEATER

TALOFLOC
DOSING
PUMP CAVITATION
AERATOR

LIME
FLOCCULANT SUCRATE PHOSPHORIC
HOLDING ACID
HOLDING

REACTION
TANK TANK

AERATION
CLARIFIER

TANK
FLOCCULANT LIME ACID

TANK
DOSING SUCRATE DOSING PUMP
PUMP DOSING
PUMP

FLOWMETER SCUM TO BE
DESWEETENED

HEAT UNTREATED
EXCHANGER LIQUOR FILTERED
LIQUOR
85°C

DEEP
UNTREATED TREATED FILTERED BED
LIQUOR LIQUOR LIQUOR FILTE
FLOW TANK TANK TANK R
CONTROL
B/W
AIR
FEED PUMP BLOWER

FEED PUMP

Figure 10
Scum De-sweetening
 The Scums are skimmed off the surface of the
liquor and are sent to the Scum De-sweetening
section.
 About 3-6% of incoming feed liquor is removed with
the scum.
 After treatment, the scum going to waste should
contain <1% of sugar.
The efficiency of the process rests on the following:
 Constant scum feed rate
 Constant dilution feed rate (usually 5:1 or as
sweetwater is needed).
 Uniform flocculant dosage (1.5 ppm on liquor solids).
 Efficient aeration
 Correct scum withdrawal (scum thickness and rake
speed)
3-STAGE SCUM DESWEETENING PROCESS
 It is a counter-current sucrose recovery process.
 Hot condensate or hot pure water is metered via a
positive displacement pump to the scum trough of
the 2nd clarifier. The quantity of water is
proportional to the ratio of water to scum (dilution
ratio).
 This water transfer the scum from the 2nd
clarifier to the mixing tank where it is thoroughly
mixed by a mechanical stirrer and gravity-feed to
the 3rd clarifier where a trace of flocculant
TALOFLOTE is added. A stream of aerated water
is added to this which results in a flotation of scum
and sweetwater.
 This scum is discharged to drain while the low-brix
sweetwater to the trough of the 1st clarifier into
the mixing tank of the 2nd clarifier.
 A mechanical stirrer thoroughly mixes the scum
and the sweetwater and a trace of flocculant
TALOFLOTE is added, simultaneously an aerated
sweetwater stream is added & the mixture flows
by gravity into the 2nd stage clarifier where
separation takes place by flotation to produce
scum on the surface and sweetwater underneath.
 The sweetwater is pumped to the mixing tank of
the 1’st where it is mixed with the scum from the
TALOFLOC phosphatation process.
 Separation takes place in the 1st stage clarifier,
and the sweetwater if transferred to the melter
of the affination station.
 3 STAGE SCUM DESWEETENING
PROCESS FLOW DIAGRAM

SCUM
FLOCCULANT MIXING
PREP. TANK TANK 1
SCUM
MIXING
TANK 2
SCUM
MIXING
CLARIFIER TANK 3
FLOCCULANT 1
HOLDING
TANK
CLARIFIER
2

FLOCCULANT AIR CLARIFIER DISCARDED

DOSING 3
PUMPS SCUM
AERATION AIR
PUMP 1

AERATION AIR
PUMP 2

AERATION
PUMP 3

SWEETWATER
SCUM FROM
TO REFINERY
MAIN
MELTER
CLARIFIER
SWEET SWEET DILUTION
WATER WATER WATER
HOLDING TANK TANK TANK
TANK 2 3

Figure 13
 Table 2: Comparison of Carbonatation and
Phosphatation
Carbonatation Phosphatation
Capital intensive;
Capital Cost Larger filter area Cheaper Equipment
required
Operating Cost Low High, due to cost of chemicals
20-30 %;more dependent on
Color removal 40-50 %; consistent
sugar quality
Requires deep bed pressure
Liquor quality Excellent; includes filtration
filtration before decolorization

Higher lime usage precipitates more

Ash removal Little ash removal
calcium salts

Higher removal than

Starch removal Significant removal
carbonatation

Waste produced Large quantity of cake produced Solid waste quantity small

Maintenance Gas pumps to maintain Low maintenance

Acid beverage floc formation
Acid floc Removes floc-forming impurities
possible
Comparison of Carbonatation and Phosphatation
Carbonatation Phosphatation
Capital intensive, Larger filter
Capital cost area required Cheaper equipment
Operating cost Low High due to chemicals cost
20-30%; dependent on sugar
Color removal 40-50% ; consistent quality
Liquor quality Excellent; includes filtration Requires deep bed pressure
filtration
Higher lime usage precipitaes
Ash removal more calcium salts Little ash removal
Higher removal than
Starch removal Significant removal carbonatation
Waste produced Large quantity of cake Solid waste quantity small
Maintenance Gas pumps to maintain Low maintenance
Acid floc Removes floc-forming Acid beverage formation
impurities possible
Carbonatation is technically the best choice
for decolorization
 Destruction of Invert
 High pH in the first Carbonator ,eliminates
most invert
 Phosphatation due low pH creates more invert
 Buffer Capacity/Sucrose Loss
 Carbonated Liquor pH of 7.8 – 8.2
 Phosphate Liquor pH of 6.8 – 7.1
 Stability of Process
 Carbonatation - excellent process stability
 Phosphatation – temperamental or unforgiving

Carbonatation is technically the best choice
for decolorization
 Quality of Sugar Product
 Carbonatation
 Sparkling
 Much less sediment in final product
 Phosphatation – lesser quality
 Secondary floc
 Some particulates are not removed by Deep
Bed Filter
Carbonatation is technically the best choice for
decolorization
 Additional Benefit of the Carbonatation
 Products contamination by pan scale due to
sulfates will be practically eliminated.
 Acid washing of vacuum pan scale will be
avoided.
 The operation of a Carbonation process
generally is more consistent than other
decolorization process.
Phosphatation
 Higher sucrose loss due to low pH
 Higher energy consumption due to process
instability.
 Lower initial capital cost.
 Flexibility if capacity expansion
 Low degree of color removal