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ChElec 502

Sugar Engineering 2
(Sugar Refinery)

Clarification
CLARIFICATION
General Principles
The washed raw sugar from the melter is acidic,
and contains some insoluble material, such as
bagacillo, and soil, suspended solids, and
colloids.
The colloids are indigenous polysaccharides that
escape the rawhouse clarification.
Clarification of the raw liquor or affination
syrup is a treatment to remove insoluble and
colloidal matter, including the substances
rendered insoluble by the treatment itself. of
precipitate.
Two methods of clarification.

CARBONATATION

PHOSPHATATION

A pressure filtration is also carried out


without using inert filter aid or a chemical
treatment maybe employed using lime or
phosphoric acid or carbon dioxide.
It is a common practice to pre-screen melt
liquor to remove coarse materials
SUGAR REFINERY PROCESS
CCarbonatation Process
LARIFICATION BY CARBONATATION
RAW SUGAR

AFFINATION

MELTER

SLUDGE
CARBONATATION
FILTRATION

1ST AND 2ND


FILTRATION
FILTER
RECOVERY
BOILING
ION EXCHANGE
CAKE
DECOLORIZATION

CRYSTALLIZATION /
PURGING

REFINED SUGAR
Carbonatation Process
The Carbonatation process consists of three (3) main
operations.
A.) Liming and gassing or saturation of the melt liquor.
B.) Filtration of the carbonated liquor and sweet sludge.
C.) Flue gas scrubbing.
CARBONATATION
PROCESS FLOW DIAGRAM
LIMING, THEN GASSING
IN CARBONATATION
TANKS (SATURATORS)
LIME
LIQOUR
MIXER

CARBONATOR A CARBONATOR C

EXHAUST
STEAM

CONDENSATE
TO BOILER

CO2 GAS

RAW
LIQUOR
FROM
MELTER CARBONATED
LIQUOR
RAW MELT LIME TANK
TANK TANK TO FIRST
FILTER

Figure 2
A.) LIMING & GASSING
The precipitation of calcium carbonate through the
addition of milk of lime {Ca(OH)2} and contacting with
gas containing carbon dioxide CO2.
The process is called Saturation because the limed
liquor should be saturated with CO2.
The following chemical reaction occurs:
quick lime + water = hydrated lime
CaO + H2O Ca(OH)2
carbon dioxide + water = carbonic acid
CO2 + H2O H2CO3
hydrated lime + carbonic acid = calcium carbonate
Ca(OH)2 + H2CO3 CaCO3 + H2O
The calcium carbonate chalk formed serves two
purposes:
It traps the color bodies and impurities from the
liquor by inclusion within the carbonate crystals.
The granular chalk is an excellent filtration aid.
The milk of lime is prepared by mixing quick lime in
cold water, to 10-15 o Baume.
It is added directly to liquor at a rate of 0.4-1.2 %
CaO on liquor solids. Liming is done to pH 12.
For each liquor, there is particular lime addition rate
in which filterability will be greatest. This optimum
lime dosage varies from 4 kg CaO/ton in some liquor
to over 12 kg CaO/ton DS.
Poorer quality melts will require more lime.
The 2 or 3 carbonators (or saturators) arranged in
series are usually employed, with progressive lower pH
in each stage
The gassing or saturation is done until all added lime is
thrown down, which is at around pH 7.7 to 8.5.
The 1st stage pH kept at 9.5. About 75-90% of the
carbonatation is achieved at this higher pH.
To immediately reduce the pH at the 1st Saturator,
80-90% of the gas is sent into it. The final gassing is
done at the succeeding up to last Saturator.
The temperature at which the gassing is done has a
great effect on the efficiency of carbonatation.
Lower temperature will result to lesser invert
destruction, thus more % color removal.
But, re-dissolves at lower temp. to calcium
bicarbonate, which is difficult to filter.
The viscosity of the liquor increases at lower
temperatures which slows down filtration.
Bigger calcium carbonate agglomerates form at higher
temperatures.
The optimum gassing temperature is between 80-85 oC.
For gassing the saturators, a small portion of the
boiler flue gas (12% CO2) is scrubbed, compressed and
used.
The gassing or saturation is done until all added lime is
thrown down, which is at around pH 8.5.
The retention time in the saturators could vary
between 40-80 minutes depending depending on the %
CO2 in the scrubbed flue gas.
To maximize the use of CO2, the lime dosage is kept as
high as possible.
Entrainment separators are provided in each saturator
to ensure that droplets are not carried out with the
exit gas.
Values of color removal over the range of 20-60%, but
are generally in the range of 40-50%.
B. Liquor Filtration
First Filtration, Second Filtration, Filter Press
Good liquor filterability is very important and is
affected by:
The quantity of chalk formed which is
determined by rate of lime addition and the
completion of the reaction.
The condition at which the calcium chalks
were grown (pH 9.5 and pH 8.3).
The temperature of liquor which affects
viscosity and formation of chalk agglomerates
(optimum is 85 oC).
The brix of liquor which affects its viscosity.
The optimum brix at filtration is between 60-
63.
The nature of impurities present, e.g. starch
impedes the conglomeration of carbonate
crystals (can be removed by amylase enzyme).
The carbonated liquor is filtered through
pressure leaf filters.
In some cases, filter aids such as diatomaceous
earth, perlite are added to achieve the required
filtration rates.
The liquor is filtered in 2 stages, (1st filtration,
then 2nd filtration) to ensure complete removal
of turbidity. The filtrate is called brown liquors.
(brown liquor1 & brown liquor2, after each
filtration, respectively.
The sweet sludge produced when washing the
liquor filters is filtered through plate & frame
filters for de-sweetening.
A more recent development is the use of a single
membrane plate filter for both pressure and
cake desweetening.
FIRST FILTRATION
PROCESS FLOW DIAGRAM
OVERHEAD OVERHEAD
FILTER AID SMEARING
TANK TANK

FILTER SLUICING WATER

CLARIFIED
WATER

FILTER AID
PREPARATION
TANK

TO SECOND TO OVER HEAD


FILTRATION TO SWEET WATER
SLUDGE TANK
FILTER

CARBONATED BROWN 1 SLUDGE SWEET


LIQUOR TANK LIQUOR TANK WATER
TANK TANK

Figure 3
SECOND FILTRATION PROCESS FLOW DIAGRAM

OVERHEAD OVERHEAD
FILTER AID SMEARING
TANK TANK

FILTER SLUICING WATER

CLARIFIED
WATER

FILTER AID
PREPARATION
TANK

TO
FIRST
TO TO OVER HEAD
FILTER
SLUDGE SWEET WATER
TO IER TANK
FILTER
COLUMN

CARBONATED BROWN 1 BROWN 2 SLUDGE SWEET


LIQUOR TANK LIQUOR LIQUOR TANK WATER
TANK TANK TANK

Figure 4
Pressure Leaf-Filters

Sweetland Filter
Pressure Leaf-Filters

Suchar Filter

Gaudfrin Filter
Sweet Sludge Filtration
The Sludge Filters are usually of the plate &
frame type. Later versions are recessed plate
type with no frames.
The plates are made of high density
polypropylene plastic.
Each plate is covered with polypropylene filter
filtering fabric.
High pressure hydraulic pumps are used to
closely pack the plates before each filtration
cycle.
If properly done, the de-sweetened mud should
contain <2% pol.
SLUDGE FILTRATION
PROCESS FLOW DIAGRAM

HOT WATER

MUD BELT CONVEYOR

DIVERTER
BOX
MUD
HOLDING
BIN

TO
MELTER

MUD TRUCK
SWEET SWEET
SLUDGE WATER
TANK TANK

Figure 6
Mud Bin
Periodic washing of is required to restore permeability.
Approximately filter cloths are wash in situ with
sulfamic acid or inhibited HCl.
At least frequent intervals, they are removed from the
steel support frames and laundered in heavy duty
washing machines.
Filter area required for carbonatation
The installed filter capacity needs to be sized for the
worst sugar quality anticipated without leading to a
reduction in the melting rate. An installed filter area
requirement of 15 m2/ton melt-hr.
Or in volumetric rate: 0.10 m3/m2-hr without filter aid,
and 0.30 m3/m2-hr with filter aid.
Filter cloth
The filtering elements are made of cloth, initially
cotton was used, but were replaced latter with nylon,
then polypropelene which give a much better service.
A monofilament polypropelene woven fabric now
appears to be universally used.
Table 1: Comparison of some types of liquor pressure filters
Automatic
Suchar Auto Gaudfrin
Sweetland Plate and
Filter Diastar
Frame
Fixed vertical Rotating Plates and
Type Drained cloth
circular discs vertical discs membrane filters
Generally
Filter body Horizontal Horizontal Vertical
Horizontal
Vertically
Cloth covered Cloth on steel suspended, Cloth and
Filter Elements
screens frame seamed cloth membranes
elements
Max. operating
520kPa 520kPa 500kPa 600kPa
pressure
Countercurrent
Oscillating jets Moving water Discharges low
Mud sluicing steam/water
between plates jets moisture cake
flow
Filtrate sight One per 2 One per filter
One per disc None
glasses discs element
Access to Bottom half Upper half
Hinged top cover Plates separate
elements drops down shells open
Maximum
100 200 400 300
area/filter in m2
C. Flue Gas Handling Washing and Compressing
To carry out the Carbonatation process at maximum
efficiency, a constant and controlled supply of CO2
should be maintained.
Flue gas containing (10-12% CO2 for coal fired,
slightly lower for oil-fired, & 7-9% for gas-fired),
from the boilers is used for sparging/ gassing in the
saturators.
Flue gas from bagsse-fired boiler would have
different % of CO2 depending on Boiler efficiency
and fuel being burned. Typical gas composition when
burning bagasse:
CO2 = 15 % N2 = 75%
O2 = 3% H2O = 7%
Typical gas composition when burning bagasse:
CO2 = 15 % N2 = 75%
O2 = 3% H2O = 7%
When burning bunker oil, the CO2 % can go as
low as 4%.
Unburnt solids are also part of the flue gas and
should be removed prior to scrubbing.
In the normal range of lime addition, the
quantity of gas required is 60-120 m3 flue
gas/ton of melt.
In practice, the design figure is 150 m3flue
gas/ton of melt which should cope-up with the
lime dosage of 10 kg CaO/ton of melt.
Flue gas are scrubbed to removed particulate
matter and traces of SO2.
Scrubbers can be dispensed with for gas-fired
boilers.
Typical gas composition when burning bagasse:
CO2 = 15 % N2 = 75%
O2 = 3% H2O = 7%
When burning bunker oil, the CO2 % can go as
low as 4%.
Unburnt solids are also part of the flue gas and
should be removed prior to scrubbing.
In the normal range of lime addition, the
quantity of gas required is 60-120 m3 flue
gas/ton of melt.
In practice, the design figure is 150 m3flue
gas/ton of melt which should cope-up with the
lime dosage of 10 kg CaO/ton of melt.
.
Flue gas are scrubbed to removed particulate
matter and traces of SO2.
Scrubbers can be dispensed with for gas-fired
boilers
In other boilers, 2 stage scrubbing maybe
require; the 1st stage for particulate matter
removal,
and the 2nd stage where soda ash solution is
sprayed/recirculated to remove SO2.
Scrubber columns can be filled with ceramic
packings, or could simply be fitted with baffles
and liquid sprays
FLUE GAS SCRUBBING

SCRUBBING WATER

PROCESS TO
WATER CARBONATORS

MOISTURE
COLLECTOR

GAS
BOILER SCRUBBER
FLUE GAS
SODA ASH MIXING AND COMPRESSOR
RECOVERY TANK

FLUE GAS
DUST
COLLECTOR

TO WASTE

Figure 7
Flue Gas
Gas Scrubber
Scrubbed Gas

Soda Ash Inlet

Raschig Rings
Soda Ash Outlet

Cold Water Inlet


Perforated Tray

Used Water Outlet


Gas Distributor
Controlled Parameters
To have an efficient Carbonatation process, the following
should be controlled:
Raw melt liquor flow rate x m3/hr
Melt Liquor Brix 60-65
Milk of lime dosage (as CaO) 0.4-1.0% on liquor s
(the commercial hydrated lime is >75% CaO)
Liquor pHs :
10.0 - 11.5 at liming
9.0 9.5 after the 1st Saturator
8.0 8.5 after the 2nd Saturator

With a fixed CO2% in gas, the pHs of the liquor can


be controlled by controlling lime dosage and
retention time in Saturators.

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