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Module 7. Final

This unit discusses massecuite crystallization after vacuum pans. Crystallizers are used to further cool massecuites and promote crystal growth as cooling increases supersaturation. There are different types of crystallizers that use various cooling methods. Massecuites are pumped to crystallizers where they are agitated to renew the mother liquor around crystals and ensure uniform supersaturation. Agitation also brings fresh massecuite into contact with cooling surfaces. Crystallizers cool massecuites to increase crystal growth but not too low to avoid increasing viscosity which reduces growth rates and requires more power for agitation.

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0% found this document useful (0 votes)
169 views

Module 7. Final

This unit discusses massecuite crystallization after vacuum pans. Crystallizers are used to further cool massecuites and promote crystal growth as cooling increases supersaturation. There are different types of crystallizers that use various cooling methods. Massecuites are pumped to crystallizers where they are agitated to renew the mother liquor around crystals and ensure uniform supersaturation. Agitation also brings fresh massecuite into contact with cooling surfaces. Crystallizers cool massecuites to increase crystal growth but not too low to avoid increasing viscosity which reduces growth rates and requires more power for agitation.

Uploaded by

sena
Copyright
© © All Rights Reserved
Available Formats
Download as PDF, TXT or read online on Scribd
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Module 7

Massecuite-Crystallization

And

Molasses Exhaustibility
Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Table of Content
Unit One: General ........................................................................................................................ 4
1.1 Introduction ..................................................................................................................... 4
1.2 The Use of Crystallizers.................................................................................................. 6
1.3 The Operation of Crystallizers ........................................................................................ 6
1.3.1 Lubrication and Reheating of Massecuites ............................................................. 7
1.3.2 Power Requirement to Derive Crystallizers ........................................................... 7
1.4 Pumping of Massecuites ................................................................................................. 8
1.4.1 Calculation of the Output of a Rota Pump .................................................................. 9
Unit Two: Types of Crystallizers .............................................................................................. 12
2.1 Air-Cooled Crystallizers ............................................................................................... 12
2.2 Water – Cooled Crystallizers ........................................................................................ 12
2.3 Vacuum Crystallizers .................................................................................................... 14
2.4 Batch and Continuous Crystallizers .............................................................................. 15
2.5 Massecuite Reheating ................................................................................................... 19
2.6 Crystal Percent Brix in Massecuite ............................................................................... 20
Unit Three: Molasses Exhaustibility ......................................................................................... 35
3.1 What is Molasses?......................................................................................................... 35
3.1.1 What is the Composition of Molasses?.................................................................. 36
3.1.2 Physical Properties ................................................................................................. 36
3.2 Factors Influencing Exhaustibility of Final Molasses .................................................. 39
3.3 The “Nutsch Bomb” Experment ................................................................................... 42
3.4 The Importance of Factory Set-Up ............................................................................... 44
3.5 Losses in Final Molasses ................................................................................................. 44
3.6 Calculation of the Quantity of “C” Massecuite ............................................................... 47
3.7 Decomposition of Molasses ............................................................................................. 50
3.8 Sugar Produced From Molasses.................................................................................... 51
3.8.1 Introduction ........................................................................................................... 51
3.8.2 The Principle behind the Process .......................................................................... 51
3.9 Development of a Better Formula................................................................................. 55
3.10 Analysis of New Formula for Molasses Exhaustion...................................................... 62

Sugar Engineering and Manufacturing Training Team 2


Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Module Introduction

Dear trainees! I welcome you to module seven of the course “Cane Sugar Manufacturing” In this
seventh module we will discuss Massecuite-crystallization and Molasses Exhaustibility.

The module is divided into three units. The first unit deals with massecuite crystallizers. It
discuss about why crystallization is followed after vacuum pan and describes properly the uses
and different types of crystallizers. At around the end of the unit it explains about lubrication and
reheating. It also discuss about massecuite pumping and efficiency calculation of pumps.

The second unit of the module focuses on the issues of the advantages and disadvantages of
different crystallizers. It compares and contrasts the batch and continuous crystallizers. In
addition to these it explains by giving illustrative example how to calculate the crystal percent
Brix in “A”, “B” and “C” massecuite.

The third unit, the last unit of the module, is mainly devoted on the exhaustibility of final
molasses. It deals at the beginning of the unit about molasses and its composition and
calculations to gain in sugar if the purity of final molasses is reduced. It also deals about factors
influencing exhaustibility of final molasses and how to determine the performance of
crystallizers using “Nutsch Bomb”. Finally it describes the influence of the factory set-up and
types of equipments on recovery of sucrose.

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Unit One

General
Unit Objectives

At the end of this unit training, the trainees will be able to:

Explain properly why crystallization is followed after vacuum pan.


Describes properly the uses of crystallizers.
Discuss briefly the lubrication and reheating of massecuite.
Calculate the efficiency of the Rota pumps.

1.1 Introduction

After completion of a strike, the massecuite is still saturated or slightly supersaturated at the
temperature in the pan (70 to 75 0C). On cooling, it becomes supersaturated and further growth
of the crystals is possible. This is the reason why vacuum pans are followed by crystallizers.

Figure 1.1: The effect of Temperature on Supersaturation

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

The effect of temperature on super-saturation is illustrated in graph above.

Assume the massecuite is cooled from point at point “B”, which corresponds to a temperature
drop of “∆t”. At point “B”, the supersaturation has increased and is proportional to the distance
“Bx”, while at point “A”, it was only “Ay”. If the massecuite is cooled further, there would be a
danger that point “B” would move into the labile zone and false grain could be formed.

The massecuite from the pans (“A”, “B”, or “C”) is dropped into a strike receiver under the
pans, from which it is pumped to the cooling crystallizers. In modern factories, massecuites are
gravitated to crystallizers. The massecuite, after some cooling in the receiver, is supersaturated.
If allowed to stand undisturbed, the crystals will continue to grow until the mother liquor in the
crystal vicinity is exhausted. Migration of sucrose molecules will be inhibited by the viscosity of
the mother liquor and crystal growth will stop.

Crystallizers are, therefore, fitted with agitators to:

a) Renew the layer of mother liquor around the crystals and ensure uniform supersatuation

b) To bring fresh massecuite in contact with the cooling surface.

The effect of cooling is to maintain as high a level of super-saturation as possible in order to


increase the driving for crystallization.

There are practical limits to the temperature to which a massecuite can be cooled in crystallizers.
Viscosity is inversely proportional to temperature (it doubles for every 5 – 10 0C drop in
temperature), and a point reached at which the power required for agitation and the strength of
the equipment limits operation at lower temperatures. In addition, crystals growth rate is also
reduced at higher viscosities.

Cooling can be achieved by natural cooling (air-cooled), or by circulation of water in cooling


elements (water –cooled). Cooling by refrigerated water has not been successful because of the
formation of a layer crystal on the cooling surface.

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

1.2 The Use of Crystallizers

Crystallizer capacity and the use of crystallizers on various massecuites vary from country to
country. In all, crystallizers are always used on “C” massecuites because they are essential for a
good exhaustion of final molasses.

Another approach to crystallization is to recover the maximum amount of sugar at each strike
(starting with the “A” strike) by cooling, to reduce sugar recirculation in the factory. This
practice is followed in Mauritius and in all sugar producing countries.

1.3 The Operation of Crystallizers


The operation crystallizer is the same for all types of massecuites, but the retention time in the
crystallizers varies according to the purity and the viscosity of the massecucites.

“A” massecuites are cooled from a strike temperature of about 70 0C to about 40 0C, and are
centrifuged at this temperature without any reheating.

“B” massecuties are normally cooled to about 40 – 50 0C, and again there is no reheating before
centrifugation.

“C” massecuites are cooled to between 30 and 40 0C in Mauritius and centrifuged with or
without reheating, in some cases. In some countries, the massecuites cannot be cooled to below
40 0C because of high viscosities and have to be reheated to 60 0C before centrifugation.

The retention time in crystallizers varies for the various types of massecuites and also with the
viscosity. It is obvious that retention time is shorter in water cooled than in air-cooled units
(Ratio of 1:3). Optimum retention times are listed below.

Mauritius Southern Africa

“A” Massecuites 4 - 6 Hours 10 - 12 Hours

“B” Massecuites 6 - 10 Hours 18 - 24 Hours

“C” Massecuites 18 - 36 Hours 36 - 48 Hours

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

The optimum retention time should be determined for each massecuite at every factory by
running NUTSCH purities at various retention times.

With very viscous massecuites, it may be preferable to cool the massecuites to the temperature at
which it can be centrifuged, and to hold it at this temperature than to cool further and then have
to lubricate the massecuties on to reheat in crystallizers.

1.3.1 Lubrication and Reheating of Massecuites

Massecuites should not be boiled at Brixes that causes problems with pumping and in
crystallizers. On the other hand, inadequate equipment should not be the reason for lower Brixes
in massecuite. Addition of water of lubrication should be discarded.

Reheating of massecuites in crystallizers should be avoided because crystals dissolution is a


function of temperature difference x time. Heating with warm water should only be restores to
after long stops. Warm water with a temperature difference of not more than 5 0C should be
used, and steam should never be used.

When reheating before centrifugation is required because of high viscosity, a properly designed
massecuites re heater should be used.

1.3.2 Power Requirement to Derive Crystallizers

The power will vary with the design and shape of the agitators, the speed of rotation and
massecuites viscosity.

Speed of rotation is usually kept at 1/3 to ½ to reduce power. Faster rotation does not appear to
improve exhaustion. At this low speed, heavy reducers are required with an electric drive and
several attempts have been made to use hydraulic motors or hydraulic rams. They have met with
limited success.

Power required to drive cooling agitators in U-shaped crystallizers varies from 0.12 to 0.3 hp/m3.

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

1.4 Pumping of Massecuites

Because of their high viscosity and crystals content, masseccuites can only be pumped by
special positive displacement pumps.

The most commonly used type of pump is the ROTA. It is a very simple and sturdy pump. Rotary
gear pumps are more commonly used on molasses. (See Figure 1.2 and 1.3)

Rota pumps when used on massecuites rotate at slow speeds: 30 to 60 rpm.

Massecuites pumps should be sized for handling peak flows of not less than 35 to 50 % above
normal.

At the high viscosities involved, the pressure drop across bends, valves, etc. can be very high,
and pipe lines should be kept as straight as possible with are radius bends. These pumps are
positive displacement pumps and there should be no valves in the delivery line.

The pump suction should always be submerged and the pumps and pipelines should be steamed
out (low-pressure steam) and drained after use.

Because of the influence of viscosity on power and flow, massecuites should be pumped hot, i.e.
from the strike receiver immediately after striking, and then allowed to gravitate through the
crystallizers to the centrifugals. The high cost of staging for crystallizers may influence this
layout and in some modern factories. “C” massecuites flows from the last crystallizers into a re
heater from which it is pumped to the centrifugals. It would be better to let massecuites gravitate
to the centrifugals through the re heater.

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

1.4.1 Calculation of the Output of a Rota Pump

π D2
W = 60 ( − S ) L . n . Pv
4

Where/ W = Litres/hour
D = Diameter of Pump (dm)
S = Cross Section of Impeller (dm2)
L = Width of Pump Parallel to Shaft (dm)
n = R.P.M
Pv = Volumetric efficiency of Pump = 0.6 - 0.75 depending on the Viscosity

Example:

Calculate the efficiency of a Rota Pump for “C” massecuite with the following Characteristics:

W = 40,000 Litres/hour
D = 381 mm
S = 3.0 dm2
n = 31 R.P.M
L = 346 mm

W
Pv =
π D 2
60 ( − S) L. n
4

40,000 40,000
Pv = =
3.14 × 3.81 2
60 × 8.402 × 3.46 × 31
60 ( − 3.0) 3.46 × 31
4

40,000
= = 0.74
54,074

Volumetric Effeciency = 0.74

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 1.2: Rotary Pump for Massecuite (Fletcher and Stewart).

Figure 1.3: Rota Pump

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Self Check Exercises

1. With the help of a supersaturation diagram, explain the principle behind the use of
crystallizers.

2. Why are the crystallizers fitted with agitators?

3. If it not possible to cool all massecuite (“A”, “B”, and “C”) which one would be
more important to cool and why?

4. Describe the two types of pumps generally used to pump massecuites and give the
advantages and disadvantages of each type.

5. Give a brief description of the principle of operation of an efficient massecuite reheater.

6. Discuss why massecuites are pumped hot after the receiver.

7. Explain with the help of diagram what can happen if a massecuite is cooled too rapidly
after the dropping from the vacuum pan.

8. With the help of diagram describe briefly the two kinds of pumps which are used for
pumping massecuite.

9. Give a brief description of a principle of operation of an efficient massecuite reheater.

10. Explain why reheating massecuite in horizontal crystallizers is not recommended.

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Unit Two
Types of Crystallizers
Unit Objectives
At the end of this unit training, the trainees will be able to:

Describe the different types of crystallizers.


Explain the advantages of vertical crystallizers.
Compare and contrast the batch and continuous crystallizers.
Discuss about massecuite reheating after crystallization.
Calculate the crystal percent Brix in “A”, “B” and “C” massecuite.

2.1 Air-Cooled Crystallizers


Air-cooled crystallizers are usually U-shaped troughs with agitators. They are mounted on
staging in well-ventilated areas to increase the cooling rate.

2.2 Water – Cooled Crystallizers


Water –cooled crystallizers can be divided into two main types, horizontal and vertical.

a) Horizontal
Horizontal crystallizers are U-shaped with a horizontal hollow shaft through which water flows
to tubes which are welded at right angles to the shaft. The best known of this type is the
BLANCHARD, with S-shaped tubes arranged in a spiral on the central hollow shift. Water
circulates from tube to tube due to the rotary movement.

A simplified copy of the Balnchard with straight tubes is common in Mauritius and in many
countries.

b) Vertical

Vertical crystallizers are a relatively new development. They are cylindrical towers with a
vertical shaft to which are fitted scraper arms which may or not contain cooling elements. In

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

some models, finned tubes have been used as cooling elements. In others, hollow plates are used,
but the most common is the Toury type which is described below:

It consists of a tower about 4.5 to 5 m in diameter with fixed banks of tubes set about 900 mm
apart. The tubes can vary in diameter from 75 mm to 50 mm. the tubs’ banks are scraped by
rotating arms attached to a central shaft. Water flows from bottom to top and massecuites from
top bottom. The temperature drop across a “C” massecuites vertical crystallizer is about 15 0C
and the heat transfer about 215 watt/m2. These crystallizers can be set in series, but because of
head loss, the number of units in series is usually limited to two. Liquidation pumps are required.
A typical installation is shown in Fig.2.1.

The advantages of vertical crystallizers are:

Lower cost because of absences of staging

Good plug flow characteristics

Large heating surface to volume ratio

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.1: Typical Vertical Crystallizer Installation

2.3 Vacuum Crystallizers


Vacuum crystallizers are a new development which have been very successful on refinery strike,
and which have also been applied on “A” massecuites, but are not common in factories.

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Massecuite from strike receiver or straight from discharge of a continuous pan is fed in to
cylindrical crystallizers, which is kept at a higher vacuum (lower temperature) than that in the
pan. The massecuites flashes and the crystallizers is fed from the bottom with green “A”
molasses which has previously been re heated (plate heat exchanger) to a higher temperature
than that in the crystallizer. It, therefore, also flashes and contributes to agitation in the
crystallizers.

Vacuum crystallizers have a short retention time (± 20 minutes), and produced a good increase in
crystals size, with a large drop in purity. They require a temperature difference of at least 12 0C
between the temperature of the massecuite in the pan and in the crystallizer. Because of viscosity
limitations, they cannot be used on low grade products.

2.4 Batch and Continuous Crystallizers


The main advantages of continuous crystallizers are:

A Substantial Increase in Capacity

Labour Saving

Constant Head on Centrifugals

The only serious disadvantage is the difficulty of taking one unit off line for repairs.

A typical layout of continuous crystallizers and cooling water is shown in Figs.2.2 and 2.3.

Three points should be noted:

1. Short circuiting should be avoided by the use of baffles (both overflow and underflow)

2. there must be sufficient head for flow of massecuites (crystallizers at different levels)

3. the connections between units should be large and deep with weir plates for flow
adjustment

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.2: Continuous Crystallizer System (Batch Conversion)

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.3: Typical Continuous Crystallizer System

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.4: Continuous Crystallizer with Underflows and


Overflows

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Additional massecuites gutters and crystallizer drainage valves can be used to convert batch
operation of one unit has to be discharged.

Continuous crystallizer should be operated full at all times, and the tendency of operators to
centrifuge massecuites faster than it is fed to the crystallizers to get spare capacity at the back
should be resisted. Automatic level controllers are advisable.

The use of the last crystallizers as a massecuites re heater as shown in Figs. 2.2, 2.3 and 2.4 is
not recommended, but it is advisable to be able to circulate warm water in all the crystallizers to
prevent the massecuties from becoming too viscous in case of long stops.

2.5 Massecuite Reheating


If the massecuite is too viscous, it must be reheated before centrifuging to increase the capacity
of the centrifugal and to improve sugar curing. In Mauritius, viscosities are generally low and
massecuite re-heaters are not common.

The main types of massecucite re heaters are:

a) Water –cooled crystallizers through which hot water is circulated (not recommended for
reasons already discussed).

b) Electrical heaters, in which massecuites is heated by an electric resistance. These


heaters usually consist of an annular and concentric element between which the
massecucite flows. They are placed in the feeding each centrifugal and provided almost
instantaneous reheating. They have been abandoned because of short circuiting caused
y pieces of metal ion the massecuite.

c) Specially designed heaters with hot water flowing in tubes and the massecuite outside.
Finned tubes are used. The temperature of the water should not be more than 2 to 3 0C
above that of the massecuite and large surface areas are therefore required. Channeling
of massecuite can easily occur. The head loss through massecuite re heaters can be
important, hence proper design is required.

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

2.6 Crystal Percent Brix in Massecuite


The Crystal Percent Brix in Massecuite can be calculated from the formula:

Apparent Purity Mas sec uite − Apparent Purity Molasses


= × 100
100 − Apparent Purity Molasses

“A” – Massecuite:
Crystal Percent Brix in Massecuite after Dropping

98.5 − 74.9 13.6


× 100 = × 100 = 54.2
100 − 74.9 25.1
Crystal Percent Brix in Massecuite after Crystallizers

98.5 − 64.2 24.3


× 100 = × 100 = 67.9
100 − 64.2 35.8
Gain in Crystal % 13.7
“B” – Massecuite:
Crystal Percent Brix in Massecuite after Dropping

75.8 − 62.6 13.2


× 100 = × 100 = 35.3
100 − 62.6 37.4
Crystal Percent Brix in Massecuite after Crystallizers

75.8 − 56.6 19.2


× 100 = × 100 = 44.2
100 − 56.6 43.4
Gain in Crystal % 8.9
“C” – Massecuite:
Crystal Percent Brix in Massecuite after Dropping

57.4 − 42.9 14.5


× 100 = × 100 = 25.4
100 − 42.9 57.1
Crystal Percent Brix in Massecuite after Crystallizers

57.4 − 32.4 25.0


× 100 = × 100 = 37.0
100 − 32.4 67.6
Gain in Crystal % 11.6

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.5: Series of Three Vertical Crystallizers (B.M.A)

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.6: Static Cooling Elements in Vertical

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.7: View of the Upper Bank of Cooling Elements of a Vertical Crystallizer

Figure 2.8: O – Type Crystallizer

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.9: Cooling System with Stationary Tubes

Figure 2.10: U – Type Crystallizer

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.11: Crystallizer Cooled Along Outside Wall

Figure 2.12(a): Cooling System with Revolving Tubes (Ragot – Tourneur)

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.12(b): Cooling System with Revolving Tubes (Karlik - Czapikowsky)

Figure 2.11(c): Cooling System with Revolving Tubes (Hehrison)

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.13: Cooling System with Revolving Discs. (Werkspoor)

Figure 2.14: Cooling System with Stationary Discs. (Ned. Ind. Industrie)

Figure 2.15: Revolving Crystallizer with Stationary Tubes. (La. Feuille)

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.16: Blanchard Crystallizer. (Fletcher Patent, Made by Babcock Atlantique)

Figure 2.17: Disc of Werkspoor Crystallizer

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.18: Crystallizer with “Flag” Stirrers (Fives Lille – Cail)

Figure 2.19: Crystallizer with Spiral Plates (Fives Lille – Cail)

Figure 2.20: Graphs of Temperatures in Kerkspoor Crystallizer

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.21: Continuous Operation Fully Countercurrent Water/Massecuite Flow Action

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.22: North Coombes Design

Figure 2.23: Leclezio Design

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Figure 2.24: Unice Rapid Crystallizer

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Self Check Exercises

1. With the help of diagram give a description of the Toory type vertical crystallizer.

2. Draw a setup for three vertical crystallizers installed in series and show the cooling water
and massecuite path.

3. Give the advantage of using vertical crystallizers against the horizontal ones.

4. Discuss the relative importance of cooling surface area in a vertical crystallizer as


compared to heating surface area in a well designed massecuite reheater.

5. How would you asses the working of crystallizers?

6. Using the following figures:


Purity of the massecuite = 60o
Purity of the mother liquor at dropping = 46o
Purity of the mother liquor after crystallization = 36o
Calculate the crystal % Brix across the crystallizers.

7. What are the advantages and disadvantages of vertical crystallizers compared to batch
crystallizers?

8. Using the following figures:


Purity of the massecuite = 60o
Purity of the mother liquor at dropping = 46o
Purity of the mother liquor after crystallization = 36o
Calculate the crystal % Brix across the crystallizers.

9. What is the relation between temperature and viscosity in cooling crystallizer?

10. Explain why cooling by refrigerator water has not been successful.

11. Explain with the help of a diagram the set-up for the two vertical cooling crystallizers
installed in a series. Show the path of the cooling water and the massecuite.

12. How does viscosity affect the working of crystallizer?

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

13. Explain the main difference in the design principle behind a crystallizers and an
efficient massecuite reheater.

14. Using the following figures:


Purity of the massecuite = 58o
Purity of the mother liquor at dropping = 45o
Purity of the mother liquor after crystallization = 35o
Calculate the crystal % Brix across the crystallizers.

15. Using the following figures:


Purity of the massecuite = 58o
Purity of the mother liquor at dropping = 43o
Purity of the mother liquor after crystallization = 33o
Calculate the crystal % Brix across the crystallizers.

16. Give a brief description of the principle of operation efficient massecuite reheater.

17. Explain why reheating massecuite in a horizontal crystallizer is not recommended.

18. Give a brief description of a working principle behind a continuous vacuum crystallizer.

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Unit Three

Molasses Exhaustibility

Unit Objectives

At the end of this unit training, the trainees will be able to:

Describe what a molasses is and explain its composition.


Discuss the relation of viscosity and temperature for various concentrations.
Calculate the gain in sugar if the purity of the molasses is reduced based on the weight of
cane crushed.
Explain all the factors that influencing exhaustibility of final molasses.
Describe briefly how the “NUTSCH BOMB” experiment determines the performance of
crystallization.
Discuss the importance of factory set-up and the types of the equipments on the recovery
of sucrose especially concerning low grade massecuite.
Explain the factors that will influence the sucrose losses in final molasses.

What is Molasses?

Molasses is one of the by-products of the sugar industry. Hence, as all by-products, it will
contain a certain amount of sugar will be lost when molasses is evacuated from the factory.
Losses in molasses can be very high-in practice it amounts to more than 50 % of all losses i.e.
losses in bagasses, losses in filter –cake and in undetermined losses.

Examples taken from laboratory reports:


Losses Expressed in Percentage
Sucrose in Bagasse % Cane 0.38 24.00
Sucrose in Filter Cake % Cane 0.03 2.00
Sucrose in Molasses % Cane 0.86 54.00
Undetermined Lossess % Cane 0.31 20.00
Total Lossess % Cane 1.58 100.00

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

3.1.1 What is the Composition of Molasses?

Molasses is composed of:

Water 20 %
Sucrose 35 %
Glucose 7%
Fructose 9%
Ashes 12 %
Nitrogenous and Non-nitrogenous Compounds,
Wax, Colourants, Carbohydrates 17 %
100 %

3.1.2 Physical Properties

VISCOSITY is one of the most important factors that will affect the exhaustibility of molasses.
From Fig.1 below, we can see that at a high Brix (80) the viscosity at 40 0C is more than double
of the viscosity at 50 0C.

Figure 3.1: Viscosity versus Temperature for Various Molasses Concentration

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What should be done to produce a molasses with low viscosity?

The problem does not start in the factory itself but much earlier, for example:

Does the cane contain white tops?


Does the cane contain a lot of impurities , such as soil and other foreign matter/
If the fields have been burnt, how long has the cane remained in the fields before
being transported to the factory for crushing?
Has the stock been renewed daily?

Now let us consider factors in the factory:


Is mill sanitation a common practice?
Is clarification of juice carried out without using excess lime?
Is pH control correctly applied?
What is the temperature of the massecuites during boiling?
What is the purity of the low-grade massecuites?

All the factors mentioned above will directly and indirectly affect the exhaustibility of final
molasses due to viscosity.

Calculation to Show the Gain in Sugar for a Crop of 300,000 Tons of Cane with One Degree Fall
in Molasses Purity

Data
Weight of Crushed Cane 300,000 tonnes
Purity of Mixed Juice 88.20
Purity of Final Molasses 37.70
Purity of Sugar 99.00
Mixed Juice % Cane 105.00
Sucrose in Mixed Juice % Cane 13.02
Sucrose Extracted % Juice 12.00
Sucrose % Mixed Juice 12.40
Polarization of Sugar 98.50

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Calculation:
12.00
Pr actical Boiling House Re cov ery = × 100 = 92.17
13.02

99.0 (88.2 − 37.7)


Theorotical Boiling House Re cov ery U sin g S .J .M : = × 100 = 92.47
88.2 (99.0 − 37.7)

92.17
Hence, Boiling House Efficiency = × 100 = 99.68
92.47

Now, if the purity of final molasses was 36.7 instead of 37.7, then theoretical B.H.R. would be:

99.0 (88.2 − 36.7)


= × 100 = 92.7
88.2 (99.0 − 36.7)

Then practical B.H.R. would be;

92.79 × 99.68
= 92.49
100

Weight of additional sucrose recoverable on 300,000 tonnes of cane crushed.

105 12.40 (92.49 − 92.17)


300,000 × × × = 125 tonnes
100 100 100

100
And weight of sugar @ 98.5 O Polarization = 125 × = 127 tonnes
98.5

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3.2 Factors Influencing Exhaustibility of Final Molasses


The boiling of low-grade massecuite requires particular care for adequate results, since this final
stage of the process determines the degree of exhaustion of the final molasses. The importance of
good exhaustion of final molasses is obvious since sugar losses there cane be very high.
The importance factors are:

a) The purity of the “C” massecuite. It should be neither too high nor too low. If too high,
sufficient drop in purity will not be obtained in practice. If too low, viscosity of
massecuite will necessarily be very high and crystals will be small, thus aggravating the
difficulty of molasses separation in the centrifugal. A purity of 59 - 60 is recommended
for Mauritius. However, depending on prevailing conditions the required purity of “C”
massecuite may be different (See Fig. 3.2 below: Graph –Purity of “C” Massecuite).

Figure 3.2: Purity of Massecuite

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b) The Purity of the “C” sugar should be at least 84 - 85 otherwise too much molasses and
impurities are re circulated and crystallization is rendered very difficult because of
increasing viscosity of the mother liquor.

From experience and by calculation, it may be proved that the volume of “C” massecuite is
highly influenced by the purity of “C” sugar.

Purity of “C” Sugar % Increased in Volume of “C” Massecuite for


“C” Sugar Purities below 90
86 5.4
82 12.4
78 21.9
74 35.8
70 5.8

N.B. Very often people think that when the purity of the “C” sugar is low this means that they
are losing less sugar in their final molasses. For the reason given above this observation is NOT
TRUE at all, because recycling a lot of impurities is like getting involved in a vicious circle, and
sometimes it is better to accept losing a bit of sugar in the final molasses by “washing” the “C”
sugar crystals in the centrifugal for a few days so as to remove more impurities to get things back
to normal.

A normal situation exists when a good “C” sugar is produced, having a purity of 85 without
using too much water in the “C” centrifugal and so avoiding re dissolving sucrose in that
important stage of the process.

c) The temperature of massecuite at the time of curing should not be higher than 55 0C,
which is considered the near optimum temperature when curing heavy density
massecuites.

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d) The size of the crystals should be around 0.25 - 0.30 mm. However, if the viscosity of
massecuite is snot too high, smaller grain will give better exhaustion of molasses due to a
greater area of crystals.

e) The massecuite should contain crystals of the same size and from any false grain. False
grains will block the passage of molasses and more water will have to be used in the
centrifugals in order to produce a “C” sugar of the required purity. When false grin
passes through the screen, they contribute to the increase of the purity of final molasses.

f) The “C” centrifugal screen should be examined regularly and damaged screens should be
replaced at once.

g) The reducing sugar/ash ratio should be greater than 1.5. It has long known that the
solubility of sucrose is decreased in the presence of reducing sugars and that most
inorganic salts tend to increases its solubility. Hence the importance of aiming at the right
pH during clarification thus avoiding the use of excess lime.

The Dowes –Dekker formula is a good index of exhaustibility of final molasses.

P = 36 - 0.08 r + 0.26 C

Where/ P = The purity obtainable with normal exhaustion


r = Reducing sugar % non sucrose in the molasses
C = Ash, expressed as sulphated ash % non sucrose ion the molasses

Note: Non Sucrose = Dry Substance – Sucrose; and “P” is usually less than “P1” ( which
is the purity of molasses produced). “P” is compared with the true purity “P1” of the
molasses obtained in practice; the difference (P - P1) indicates the gain in purity. Which
remains to be realized in order to attain theoretical exhaustibility.

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Example: If “P1” = 38 and “P” = 35.5, the potential gain impurity (38 - 35.5) is 2.5
points. This means that every effort should be made to decrease “P1” so as to come
closer to or even less than “P”.

In Mauritius, since 1996, a formula was developed by M.S.I.R.I., which reads as follows:

4 × R
Re ference Purity ( R.P) = 44.6 −
A
Where/ R = R.S % non sucrose

A = Ash, expressed as sulphated ash % non sucrose in the molasses.

However, this formula has been revised recently and a new equation has been developed and it is
equal to:
R 3.72 R
Re ference Purity ( R.P) = 36.82 + 157 −
Nse log A
Where/ R/Nse = Ratio of R.S. to non sucrose

A = Ash, expressed as sulphated ash % non sucrose in the molasses

3.3 The “Nutsch Bomb” Experment

In order to asses the performance of the water-cooled crystallizers and that of the centrifugal, a
molasses separator is used and it is called a “NUTSCH BOMB” or a massecuite filter (See
Fig.3.3).

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Figure 3.3: Nutsch Bomb or Massecuite Filter


After a strike is dropped from the pan a sample of hot massecuite is brought to the laboratory and
filtered in the Nutsch Bomb. The mother liquor is analyzed for purity.

When the massecuite in the water –cooled crystallizer is ready for centrifuging another sample is
taken. The mother liquor is separated by the same means and is analyzed for purity. The
difference between the two purities represents the exhaustion attained in the crystallizer.

Example:

Purity of Mother Liquor at Dropping = 40

Purity of Mother Liquor after Crystallization = 35

Difference in Purities = 5

However, if the difference in purity decreases in relation to an average constant figure, it is an


indication that there may be a leakage somewhere in the water cooling elements. The matter
should be investigated without delay.

The use of the Nutsch Bomb is also very interesting to explain the drop in purity between a “C”
massecuite and its final molasses. The total drop in purity is made up of the sum of:

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Drop in purity between massecuite and mother liquor after boiling


+ Drop in purity between mother liquor after boiling and after cooling
+ Drop in purity between mother liquor before and after centrifuging.

3.4 The Importance of Factory Set-Up


The designs of a factory and the type of equipment used as well as the available plant capacity
have a direct impact on the recovery of sucrose especially concerning low-grade massecuites.

Pans used in boiling c massecuites must have very good circulation and have sufficient capacity
for the hours of operation required to obtain good results. massecucites must be cooled after
striking for a minimum of 30 hours in water cooed crystallizer . The equipment must be strong
enough to handle high brix massecuites increasing in viscosity during cooling. After cooling “C”
massecuites should be reheated to a temperature of 55 0C or more if required under controlled
conditions. Massecuites should be made to gravitate through the crystallizers, massecuites hater
and the centrifugals. No dilution should be done. Obviously, good pan work resulting in
massecuites with the required crystals content high Brix as well as form crystals without false
grain should always e the aim.

3.5 Losses in Final Molasses


Losses in final molasses are not only due to high purity of the latter, but also to the quantity of
molasses that is produced by the factory, since.

Sucrose Lost in Final Molasses = Weight of Molasses × Sucrose % Molasses

It is well known that molasses % cane depends mainly on the quality of the coming in the
factory; however, this is not only reason. There are certainly other factors that will influence the
weight of the molasses in the factory.

These factors are:

a) Clarification Efficiency

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b) Impurities Developed in the Proceeding

c) Impurities Introduced With Lime, Water, etc.

d) The Weighing and Sampling of the Molasses.

a) Clarification Efficiency

The clarification process is well known to eliminate impurities (mostly inorganic matter) from
juice (i.e. the ashes). If the ashes are not removed with the scum, they will find their way through
the whole sugar process and will be found in the final molasses where over and above their
weights, they are going to maintain more sugar in solution. It is well known that in all target
purity developed, the ashes content has a tendency to increase the purit5y of the final molasses.

b) Impurities Developed in the Processing

If during the processing, reducing sugars are destroyed or sucrose is inverted and sometimes the
two happen at the same time, we can say that, as a result of such, impurities are developed during
the processing. This is why wee must pay careful attention to the following

Reduce to a minimum retention time whenever this is possible


Avoid recirculation of products (especially poor and rich runnings)
Control the exhaust steam temperature at the evaporator and vacuum pans.
Get assure that he barometric condenser is working well, i.e. the vacuum obtained is
sufficiently high to obtain a maximum of 65 0C.

c) Impurities Introduced in the Factory

The latter may not highly influence the level of ashes, but they can be more easily controlled.
River water, which may sometimes contain a high concentration of impurities, should e replaced
by condensate whenever this is possible, i.e. for the imbibition on the mills, for the preparation of
flocculant, for the injection water in the centrifugals. Water that has been used for the wet
scrubber in the decompression chamber to remove ashes from flue gasses of the chimney should
never be re-used in the factory for the process. Similarly, the utilization of ashes in the filtration
process is NOT recommended.

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d) The Weighing and Sampling of Final Molasses

The molasses scale must e as accurate as possible. Even if the price of that product is much
lower than the price of sugar, its exact weight must be known in order to have a good chemical
control ion the factory.

Careful attention must also be paid to the sampling method of final molasses. The pipe used to
collect the sample of molasses must be big enough to allow the samples to flow quite easily.
Otherwise, the sample will contain a greeter proportion of molasses at a lower Brix. A small
volumetric pump is the best alternative to have a representative sample of final molasses.

For a factory crushing 400,000 tonnes of cane per crop, if the loss of molasses % cane can be
reduced by 0.5, this will represent a gain of six million rupees on its profit.
Calculation:

0.5 × 400,000
Difference in the Weight of Molasses = = 2,000 tonnes
100

If that molasses contain a minimum of 30 % saccharose, hence the weight of saccharose in that
weight of molasses will be:
30 × 2,000
= = 600 tonnes
100

0 .5 × 100
Equivalent of Sugar @ 98.50 Pol = = 609 tonnes
98.50

If the price of sugar is Birr 10,000 per tonne, gain in money is:

609 × Rs 10,000 = Birr 6,090,000 i.e. Birr 6 Million

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3.6 Calculation of the Quantity of “C” Massecuite


The quantity of “C” massecuite produced per ton of cane depends on two main parameters,
which are the BRIX and PURITY of the mixed juice. By means of a simple calculation the
theoretical volume of “C” massecuites produced per ton of crushed can be worked out.

Data

Mixed Juice % Cane 105

Purity of Molasses 36

Brix of Mixed Juice “B”

Purity of Mixed Juice “P”

Purity of “C” Massecuite 58

Brix of “C” Massecuite 95.3

Purity of Commercial Sugar 99

Purity of “C” Sugar 85

Calculation:

If Weight of Cane Considered = 100 Kg

Then Wegitht of Mixed Juice = 105 Kg

B
Kg Brix in 105 Kg of Mixed Juice = 105 ×
100

105 B
Now using Cobenze’s diagram, the weight of Brix in molasses to be obtained from Kg
100
Brix in mixed juice of purity “P” can be calculated thus:

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99 − P
Hence Solids or Brix in Molasses % Brix in Mixed Juice = × 100
63

105 B
Then for Brix in Mixed Juice there are;
100

99 − P 100 105 B (99 − P) 105 B


× × = × Kg Brix in Molasses
63 100 100 63 100

Now, if from “C” massecuite we obtain “C” sugar and molasses, using Cobenze’s diagram we
can calculate the weight of “C” massecuite that would yield.

99 − P 105 B
× Kg in Molasses
63 100

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27
Hence Kg Brix in Molasses % Brix in " C" Mas sec uite = × 100
49

49
and Kg Brix in " C" Mas sec uite per 100 Kg in Molasses = × 100
27

(99 − P) 105 B
and for × Kg Brix in Molasses there will be :
63 100

49 100 99 − P 105 B
× × ×
27 100 63 100

3.025 100
× B × (99 − P) ×
100 95.3

3.174
× B × (99 − P) Kg of " C" Mas sec uite
100

Now, the volume of “C” massecuite is obtained by dividing by the specific gravity at 95.3 Brix
which is 1.519. This will give the weight of c massecuite per 100 Kg cane.

The volume of “C” masecuite per 100 Kg of cane is given by:

3.174 1
( × B × (99 − P) × × 10 ) Litres / Tonnes of Cane
100 1.519

Volume = 0.20894 × B × (99 − P ) Litres / Tonnes of Cane

If Brix % Mixed Juice = 13 (= B)

and Purity of Mixed Juice = 85 (= P)

Then, Volume Massecuite = (0.2089 × 13 × 14)

= 38.02 Litres/tonnes of Cane

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N.B. this calculation is purely theoretical. However, it is based on factual factory performance
figures. It is important in the since that it will help to have an estimate of the volume of “C”
massecuite and this will help to fix crushing rate to cope with the amount of “C” massecuite to
be expected.

However, it is better to rely on the volumes of massecuites given by the laboratory in its weekly
report. These volumes are based on those of massecuites, which have been boiled and cured
during factory operations.

3.7 Decomposition of Molasses


Molasses can be destroyed rapidly if the temperature of storage is around 40 – 45 0C. CO2 is
liberated due to the Maillard reaction. This makes the volume of the molasses raise dramatically
and cane eventually double nit after some days.

Sometimes, molasses decomposes very rapidly and as the reaction is exothermic, there is
obviously destruction of the molasses, i.e. the molasses becomes a carbonized mass.

In 1955, a whole reservoir of molasses (2,990 m3) was destroyed at Porto Rico.

Here below is what happened:

In the afternoon of 5 June, preliminary signs of the problem became apparent. In fact there was
like a heavy explosion coming from the reservoir where the molasses was stocked since 4 April.
After the explosion, the molasses overflowed from the reservoir of the capacity of 7,570 m3.
They tried, without success, to empty the reservoir in a nearby river. An intense heat came from
the reservoir and this rising temperature evaporated a large quantity of water and acid vapour.
After all the water from the molasses was evaporated, the latter was transformed in a solid
carbonized mass.

There was an investigation following this accident and the report presented showed the following
points:

i) Molasses must never be stocked at a temperature exceeding 40 – 45 0C

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ii) It is recommended to re circulate the molasses with the aim to reduce the possibility of
heat liberation in stagnant molasses which otherwise would raise the temperature.

iii) The cause of the accident was due to the rising temperature of the molasses during
storage.

3.8 Sugar Produced From Molasses

Chromatographic Separation by Simulated Mobile Bed

3.8.1 Introduction

The industrial chromatography is developed due to the use of the simulated mobile bed technic
which has allowed a fundamental optimization of this new technology.

Among the most recent application, the recuperation of saccharose presents in the molasses is
certainly the most attractive, both industrially and economically. However, the molasses has to
undergo a pre-treatment for the removal of calcium and certain colloidal matter.

3.8.2 The Principle behind the Process

The principle behind the separation of two or more components is very well known. It is based
on the difference in affinity of an absorbent, such as an iron-exchanged resin, for components in
a mixture. These different affinities are related to the speed of migration equally different at a
resin bed.

Example:
Molasses are composed of sugar and non-sugar. The affinity of the resin is more important for
the saccharose. Its speed of migration will thus be slower than the speed of the “non -sugars”.
Hence, in a column of resin, if we introduce molasses which is continuously washed with water.
The fact that the speeds of migration are different, we observe the flowing curve.

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At the beginning, the effluent will be richer in non sugars; then after some time, the remaining
sugars will eventually come out. However, this technic does not allow an optimum use of the
resin bed and needs a significant difference in affinity amount the component in order to obtain a
more important separation. And in order to do so, the overall resin bed is divided into multiple
columns having different points of injection as well as extraction as shown below:

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The resin used in chromatography should be in the K+ form to obtain the ideal separation and
this implies that the molasses does not contain any Ca++ ions.

This is why sugar factories must be equipped with a deliming unit (which is the best
solution) or the molasses should be delimed before its passage through the chromatographic
separator.

During the process, the molasses has to be diluted a lot (to each tonne of molasses, seven tonnes
of water are added). This of course contributes to make the process very expensive because of
the steam needed to evaporate water for saccharose recovery. The water used is usually
condensate. The quantity of sugar recovered is 90 %, with a purity of 920.

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3.9 Development of a Better Formula

To Determine a Good Exhaustion of the Molasses

The study was done at the Mauritius sugar Research institute by Mrs L.Wong Sak Koi and Mr S.
Sakurdeep.

Summary: Samples of molasses were taken from the 19 sugar factories of Mauritius during
sugar campaign 1990 – 1991 and were analyzed for their Brix sucrose, reducing
sugar and ashes of sulphate.

An analytical study of the data obtained, taking into account the fraction of non
sucrose and non sugar, was done to look for any simple or multiple linear relations.
The following equation was obtained for calculating the reference purity of the
molasses:

157 R 3.72 R
3.82 + −
NSE Log A

Where/ R = Reducing Sugars


NSE = Non Sucrose
= Dry Matter – Sucrose
= 0.821 Brix + 9.65 Sucrose
A = Sulphated Ashes

This new equation gives a better indication of the exhaustion of the molasses than that calculated
in 1968, which is:

4R
Re ference Purity = 44.6 −
A

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Introduction

It is nowadays known all thought the would that the principle source of sugar loss during the
processing of sugar lies in the molasses. However, the quantity of sucrose that can be extracted
depends to certain on some factors which are:

(a) Viscosity

(b) Crystal Content of the Massecuite

(c) The Saturation Temperature of Crystallization

(d) The nature and Quantity of Non Sugar Present in the Molasses ,mainly:

(i) The Reducing Sugars


(ii) Inorganic Salts, such as Potassium, Sodium, Calcium and Magnesium

After the publication of the famous formula of Dowes –Dekker (1949) concerning the theoretical
maximum exhaustion of molasses which equal to 35.886 – 8.088 R/NSe + 26.047 A/NSe,
many countries have developed their own equation in such a way to be able to predict the aiming
purity of the molasses after determination of the nature and amount of non sucrose present ion
the molasses.

The formulae for calculating the exhaustion of molasses were determined from analytical study
of data obtained concerning the real purity of molasses and the quantity of non sucrose present.
Some of these formulate were derived form results obtained in laboratories using adequate
specialized equipment for exhausting, as far as possible, the molasses samples (like this is done
in South Africa and Hawaii). The purity of the molasses which we can predict from these
formulae are well known by the name of target purity , even through it would have been more
appropriate to call if the reference purity. It must also be said that in practice, these reference
purities are sometimes higher than the true purity obtained.

The formula used in Mauritius recently was calculated in 1968 by J.D. de Rivaltz de St. Antoine
and his team, and was equal to:

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4R
Re ference Purity ( R.P) = 44.6 − .......... ......................(1)
A

With a correlation coefficient of 0.45.the difference between the true purity and the reference
purity gives a good indication of molasses exhaustion.

but with the improvement brought gradually in the factory at the boiling and centrifuging
department , the possibilities of molasses exhaustion had changed the data and it was time to
review the formulate developed in 1968.

Experimentation Done In 1990 and 1991

The composite samples of final molasses coming from 19 factories (collected throughout a
period of 15 days) were analyzed for their refractometric Brix, sucrose, reducing sugars and
sulphate ashes (See graph below).

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True Purity Vs. Reference Purity For Harvest 1990 and 1991 Equation 1 = 44.6 – 4R/A

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Results and Comments

The tables (1990 and 1991) give the average, maximum and minimum of the differences in
reference purity * obtained from each of the 19 factories.

*The reference purity has been calculated with the formula of equation I.

Table 1 1990 Crop average of parameters analyzed and RPD for each factory

Foc Noof Brix R S A R% A% Time Reference RPD(1)


Samples purity purity1 Mean Max Min
1 10 87.83 15.32 33.65 17.06 17.4 19.4 41.2 41.0 0.2 1.7 -0.8
2 10 80.59 15.60 29.30 15.08 19.4 18.7 38.7 40.5 -1.8 0.6 -3.2
3 10 85.03 16.39 30.44 16.32 19.3 19.2 38.3 40.6 -2.3 0.5 -3.5
4 9 82.2 13.15 32.47 15.96 15.9 19.3 41.9 41.3 0.6 2.0 -2.3
5 9 86.08 15.67 36.63 14.16 18.2 16.4 45.6 40.2 5.4 9.5 3.6
6 8 87.39 15.92 32.80 16.42 18.2 18.8 40.3 40.7 -0.4 0.3 -1.4
7 10 85.18 14.12 33.33 15.74 16.6 18.5 41.9 41.0 0.9 4.0 -0.6
8 11 84.99 14.56 32.10 15.74 17.1 18.5 40.4 40.9 -0.5 3.1 -1.4
9 11 82.46 14.23 33.86 14.81 17.3 18.0 43.8 40.8 3.0 7.5 1.1
10 10 81.67 12.15 32.07 17.36 14.9 21.3 41.8 41.8 0.0 1.1 -0.9
11 11 88.90 14.64 35.21 16.99 16.5 19.1 42.6 41.2 1.4 4.5 -0.3
12 10 89.93 14.70 30.61 19.49 16.3 21.7 36.7 41.6 -4.9 -4.1 -5.8
13 9 85.41 12.77 34.27 16.51 15.0 19.3 43.0 41.5 1.5 3.5 -0.4
14 10 86.18 11.58 33.21 17.72 13.4 20.6 41.3 42.0 -0.7 4.8 1.0
15 11 87.12 13.22 35.67 17.57 15.2 20.2 43.9 41.6 2.3 4.8 1.0
16 9 87.79 14.22 32.46 17.90 16.2 20.4 39.7 41.4 -1.7 -1.0 -3.0
17 10 84.10 14.02 31.12 17.08 16.7 20.3 39.5 41.3 -1.8 -0.7 -3.0
18 10 81.71 12.99 30.07 16.77 15.9 20.5 39.2 41.5 2.3 0.3 -3.2
19 10 85.88 11.61 32.85 16.86 13.5 19.6 41.0 41.8 0.8 1.3 2.1
AVG 85.31 14.04 32.74 16.61 16.5 19.5 41.1 41.2 -0.10

Table 2 1991 Crop average of parameters analyzed and RPD for each factory

Foc Noof Brix R S A R% A% Time Reference RPD(1)


Samples purity purity1 Mean Max Min
1 9 89.04 14.22 34.81 18.25 16.0 20.5 42.1 41.5 0.6 8.0 -1.1
2 8 81.58 13.06 30.48 17.39 16.0 21.3 39.8 41.6 -1.8 -0.5 -2.9
3 10 82.84 15.21 30.29 16.75 18.4 20.2 39.0 41.0 -2.0 0.3 -2.3
4 7 78.41 10.26 30.38 17.99 13.1 22.9 40.9 42.3 -1.4 0.4 -2.5
5 7 87.63 12.43 37.86 16.88 14.2 19.3 46.4 41.7 4.7 8.5 1.9
6 6 88.76 13.68 33.99 18.65 15.4 21.0 41.2 41.7 -0.5 0.1 -1.1
7 7 85.54 11.65 34.63 17.62 13.6 20.6 43.4 42.0 1.4 1.9 0.7
8 13 85.08 13.66 33.71 16.84 16.1 19.8 42.4 41.4 1.0 5.1 -0.5
9 12 77.76 12.72 32.05 14.83 16.4 19.1 43.6 41.2 2.4 5.4 1.2
10 13 82.80 14.20 33.05 17.31 17.1 20.9 42.6 41.3 1.3 3.3 0.1
11 10 88.87 13.71 35.64 17.36 15.4 19.5 43.1 41.4 1.7 4.7 0.5
12 10 89.64 14.61 30.65 20.23 16.3 22.6 36.8 41.7 -4.9 -2.9 -5.8
13 13 86.28 14.41 34.25 16.66 16.7 19.3 42.6 41.1 1.5 4.2 -0.5
14 11 86.36 12.83 32.79 18.24 14.9 21.1 40.7 41.8 -1.1 1.0 -2.7
15 13 85.59 12.78 35.00 18.43 14.9 21.5 43.8 41.8 2.0 4.2 1.1
16 11 88.43 14.27 32.83 18.66 16.1 21.1 39.9 41.5 -1.6 -0.6 -2.9
17 10 83.05 13.85 30.39 17.72 16.7 21.3 39.0 41.5 -2.5 -0.9 -3.1
18 12 84.97 12.85 31.58 18.25 15.1 21.5 39.8 41.8 -2.0 0.7 -3.3
19 11 86.03 11.79 34.90 16.94 13.7 19.7 43.5 41.8 1.7 2.7 -0.1
AVG 85.19 13.27 32.96 17.63 15.6 20.7 41.6 41.6 0.0

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

If we now look at the individual mean of the 19 sugar factories for the two consecutive years, we
see that the reference purity dos not vary much and is equal to 41 ± 1 and can therefore make
us draw erroneous conclusions (the general mean of the reference purity for the whole island was
41).

This observation proves that there is an urgent need to review the whole question.

If we make a list of all the formulae used throughout the world to calculate the reference purity.
We observe the following.

Table 3
Different Equations to Calculate the Reference Purity (RP)
Used throughout the World

COUNTRIES MOLASSES EXHAUSTION FORMMULA

Australia TP = 40.67 – 17.80 Log (R/A)


Hawaii TP = 20.0 – 13 R/Nsr + 28 A/NSr
India TP = 28.57 – 11 R/A + 135 moisture /NSr
Java, Philippines TP = 24.0 – 11 R/NSr + 26 A/NSr
Mauritius TP = 44.6 – 4 R/A
Porto Rico Total Sugar % Brix = 55 + (R % Brix – 15)/2
Reunion island Reference Purity = 40 – 4 R/A
South Africa GLC purity = 33.9 – 13.4 Log (F + G) /A
Taiwan TP = 19.787 + 23.33 R/Nse + 46.95 A/Nse

After having done a statistical analysis by computer, it was decided to use the following
equation:

R.P. = 36.82 + 157 R/Nse – 3.72 R/Log A …………………..(II)

Which has a correlation coefficient of 0.75

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

When applying the new formula to the values obtained in 1990 and 1991, we obtain, for the
molasses from the sugar factories in Mauritius, a reference purity which is more realistic as
shown by the graph below.

Regression between True Purity and Reference Purity (II) for 1990 and 1991 Data
Equation II: 36.82 + 157 R/Nse – 3.72 R/Log A

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

3.10 Analysis of New Formula for Molasses Exhaustion

Favorable Influence of Reducing Sugars

With the utilization of Equation II, the higher the reducing sugar content, the lower is the amount
of sucrose as well as the reference purity. This corresponds well to the fact that the reducing
sugars reduce the solubility of sucrose in the molasses and, therefore, contribute to the decreases
in molasses content.

Unfavorable Influence of the Mineral Salts (Ashes)

The higher the ash content, the higher is the reference purity. This is due to the fact that the
principal components of the mineral slats (potassium and sodium) which are well known for
increasing sucrose solubility increase the amount of molasses.

Can We Further Exhaust Molasses?

From the point of view of Dr. N.Deer (1921), in a well exhausted molasses: for one part of non
sugar, there is 0.455 part of water in order to keep it in solution, and for each unit of water, there
is 1.8 parts of dissolved sucrose Therefore, there is 0.82 part of sucrose for each part of non
sucrose

But if we calculate the ratio S/NSe for all the sugar factories of Mauritius, we observe that the
ratio is around 0.70.

1 N.S. = 0.455 H2O or for 0.455 part of H2O, there is 1 part of N.S.

1.8 Sucrose = 1 Part H2O


1
∴ 1 Part of H 2 O = = 2.2 Part of N .S .
0.455

∴ For 2.2 Parts of N.S. = 1.8 Parts of Sucrose

1.8
And for 1.0 = × 1.0 = 0.82 Part of Sucrose
2.2

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Table 4
Ratio for All these Factories
FACTORY Crop Average of S/NSe Ratio
1990 1991
1. 0.70 0.73
2. 0.63 0.66
3. 0.62 0.64
4 0.72 0.70
5 0.84 0.87
6 0.67 0.70
7 0.72 0.77
8 0.68 0.74
9 0.78 0.77
10 0.72 0.77
11 0.74 0.76
12 0.58 0.58
13 0.75 0.74
14 0.70 0.69
15 0.78 0.78
16 0.66 0.66
17 0.65 0.64
18 0.64 0.66
19 0.69 0.77
Average 0.70 0.72

It is also interesting to note that factory No.12 has a very low ratio which is 0.58 and which
proves that there is always room for improvement ion the exhaustion of molasses.

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Conclusion

The new equation is certainly more precise for indicating the theoretical exhaustion of the
molasses, but it must not be forgotten that these formulate were derived from statistical data. The
possibility of obtaining, in practice, a lower purity for the molasses is large since the molasses
used for the analysis is not and will it self never be completely exhausted.

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Module 7: Massecuite-Crystallization and Molasses Exhaustibility

Self Check Exercises

1. What are the different factors that will directly influence exhaustibility of final molasses?

2. With what apparatus and how can we explain the drop in purity between a “C”
massecuite and its final molasses?

3. What are the factors that will influence the weight of molasses in the factory?

4. What should be done to produce molasses with low viscosity?

5. With are the different factors that will influence exhaustibility of final molasses when
boiling low grade massecuite?

6. What is Maillard Reaction? How can it be prevented during storage of final molasses?

7. Why is the purity of “C” sugar important and what is its influence on the volume of “C”
massecuite produced?

8. Explain the importance of “C” massecuite purity in the exhaustion of final molasses.

9. What will be the loss in the sugar, for a crop of 500,000 tonnes of cane with two degrees
if molasses purity of:

Purity of Mixed Juice = 88.2


Purity of Final Molasses = 37.7
Purity of Sugar = 99.0
Mixed Juice % Cane = 105.0
Sucrose in Mixed Juice % Cane = 13.02
Sucrose Extracted % Cane = 12.00
Sucrose % Mixed Juice = 12.40
Polarization of Sugar = 98.50

10. What is the “Froth Fermentation”?

11. Describe the importance of factory set up on the exhaustibility of molasses.

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12. What is the importance of control of “C” - Magma?

13. (a) Explain the importance of reducing sugar and ashes content in the exhaustibility of
final molasses?
(b) Why is it important to determine the target purity of molasses?

14. Calculate the gain in sugar at a Pol of 98.50 after having reduced the purity of final
molasses by one degree for a factory with the following data:

Weight of Cane Crushed = 600,000


Purity of Mixed Juice = 87.0
Purity of Final Molasses = 38.0
Purity of Sugar = 99.0
Mixed Juice % Cane = 110.0
Sucrose in Mixed Juice % Cane = 12.16
Sucrose Extracted % Cane = 10.94
Sucrose % Mixed Juice = 10.94
Polarization of Sugar = 98.50

15. What is the influence of “C” – Magma or “C”- Sugar purity on the volume of “C”
massecuite produced?

16. How can we avoid the development of impurities during processing?

17. How can we asses the performance of a water cooled crystallizer?

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