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1987-Rein-Syrup Clarification In Raw, Notas de estudo de Engenharia Química

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Proceedings
of The
South
African
Sugar
Technologists'
Association
-June
1987
SYRUP
CLARIFICA
liON
IN
RAW
SUGAR
MILLS
By P. W. Rein, and M. G. S. Cox
Tongaat-Hulett
Sugar
Limited,
La
Lucia
and G. Montocchio
Tongaat-Hulett
Sugar
Limited,
Felixton
Abstract
The results of a laboratory investigation into clarification
of syrup by flotation are described, as wellas a comprehen-
sive test programme on a full-scale unit installed subse-
quently at Empangeni mill. The benefitsto be achieved from
syrup clarificationhave been established. Factorsinfluencing
the performance of syrup clarification are described, which
have proved useful in the design of further full-scale units.
Preliminary results from a syrup clarifierinstalled at the new
Felixton mill are given.
Introduction
The mill at Empangeni always suffered from poor cane
quality. This led to extreme difficulty in producing VHP
quality sugarand to highlyviscousmassecuites, whichmeant
that exhaustion of final molasses was also poor. Juice clar-
ification was generally poor, and although some additional
processes such as high pH liming and sulphitation were
looked at in the laboratory, there was an understandable
reluctance to make the processing sequence any more com-
plicated or more expensive.
Clarification of syrup by settling is not possible because
of the high density and viscosity ofsyrup. However, flotation
clarification is a well-established process in both sugar re-
fining
and water treatment. In this process, very
fine
sus-
pended matter which will not settle can be floated
off.
The
mechanism involves physical capture of the air bubbles
within the
floes
and intramolecular attractions across the
air/liquid interface. Scum can be floated off with bubbles in
the clarifier. The degree of separation achieved depends on
the surface properties of the solid particles.I
Considerable work was done in South Africaon flotation
clarification of juice, both under vacuum and under atmos-
pheric conditions. The process showed some considerable
promise and results were reported by the Sugar Milling Re-
search Institute (SMRI).2However, the scum formed was
apparently not as stableas that obtained in syrup clarification.
In 1974,a Tate &Lyle syrup clarification processwas put
into operation at Noodsberg. This showed that the process
led to an improvement in sugar quality and a reduction in
massecuiteviscosity, but no boiling house improvement was
evident.3Since sugarquality was not a concern at Noodsberg
at that time, this process was discontinued. Similar results
were obtained at Belle Vue sugar mill in Mauritius.' Sugar
quality was improved and the
effect
on the downstream re-
finery
processwasextremelymarked. Massecuites werefound
to be less viscous and easier to cure, but they were not able
to show the benefit of the process on
final
molassespurities.
They reported that the process led to a small increase of 5 %
in colour, but a reduction in turbidity of the syrup of 67%.
Following the work done on a syrupclarifierin Honokaa,
Hawaii,' it appears that flotation clarification can be oper-
ated without the addition of phosphoric acid. This reduces
considerably the cost of the process and it was decided to
look at this in the laboratory.
22
A comprehensive laboratory investigation was under-
taken, which showed very promising results as regards tur-
bidity removal and viscosity reduction. This laboratory
investigation established some of the design parameters nec-
essary for the design of a full-scale unit. This was subse-
quently put in at Empangeni and operated for two years
before the mill was closed down. During this period, the
syrup clarifier showed significant benefits as regards sugar
quality and massecuite viscosity. Subsequently, when the
new Felixton mill was built, a syrup clarifier was installed
there as
well.
Operating experience at both Empangeni and
Felixton has given a better insight into the process and has
enabled it to be optimised.
Results
of
laboratory
work
A laboratory test was devised which involved rapid stir-
ring of syrup in a water bath at 85'C for 3 minutes. The
stirring arrangement was such that air was entrained into
the syrup to saturate it with air. Polyelectrolyte was added
and the syrup was then left standing for 20 minutes.
It
was found that turbidity reductions of 80 to 90 %could
be consistently obtained. The measurement of turbidity in
syrup was found to be affected by a number of different
factors, including brix of the solution being measured. The
method in the laboratory manual for South African sugar
factories was found to be unacceptably sensitive to small
changes in pH. Therefore the procedure given in Appendix
1 was developed and used in this work.
Since the initial series of tests were carried out, a large
number oflaboratory tests have been carriedout on a variety
of syrups from a number of factories in South Africa and
Zimbabwe. Some slight variations in turbidity removal are
noted, due probably to the different natures of the particulate
material. Nevertheless, turbidity removals have always been
in the range of 80 to 95
%.
These laboratory trials, however, showed that there was
no significant purity improvement and that the amount of
ash removed was very small. In addition, no improvement
in syrup colour was measured.
These tests were done without the addition of phosphoric
acid and lime. The
effect
of these additional chemicals on
turbidity removal was investigated in detail. Results are
shown in Table 1, but the general conclusion is that the
addition of phosphate and lime did not improve removal
of impurities or colour and actually gave worse turbidity
removal. This indicated clearly that the simple clarification
without the addition of any additional chemicals, other than
polyelectrolyte, would be a viable proposition.
Laboratory trials showed the optimum flocculant dosage
to be around 10to 15 ppm. Theseresultsare shown in Figure
1, and indicate that any higher dosage
figures
do not make
any material improvement. No
effect
of different type of
polyelectrolytes was established initially. Later tests, how-
ever, showedthat Talosep A3and Separan gavebetter results
than Magnafloc
LT27.
In general, it has been found that the
pf3
pf4
pf5
pf8
pf9
pfa

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SYRUP CLARIFICA liON IN RAW SUGAR MILLS

By P. W. Rein, and M. G. S. Cox

Tongaat-Hulett Sugar Limited, La Lucia

and G. Montocchio

Tongaat-Hulett Sugar Limited, Felixton

Abstract

The results of a laboratory investigation into clarification

of syrup by flotation are described, as well as a comprehen-

sive test programme on a full-scale unit installed subse-

quently at Empangeni mill. The benefitsto be achieved from

syrup clarification have been established. Factors influencing

the performance of syrup clarification are described, which

have proved useful in the design of further full-scale units.

Preliminary results from a syrup clarifierinstalled at the new

Felixton mill are given.

Introduction

The mill at Empangeni always suffered from poor cane

quality. This led to extreme difficulty in producing VHP

quality sugar and to highlyviscous massecuites, which meant

that exhaustion of final molasses was also poor. Juice clar-

ification was generally poor, and although some additional

processes such as high pH liming and sulphitation were

looked at in the laboratory, there was an understandable

reluctance to make the processing sequence any more com-

plicated or more expensive.

Clarification of syrup by settling is not possible because

of the high density and viscosity of syrup. However,flotation

clarification is a well-established process in both sugar re-

fining and water treatment. In this process, very fine sus-

pended matter which will not settle can be floated off. The

mechanism involves physical capture of the air bubbles

within the floes and intramolecular attractions across the

air/liquid interface. Scum can be floated off with bubbles in

the clarifier. The degree of separation achieved depends on

the surface properties of the solid particles.I

Considerable work was done in South Africa on flotation

clarification of juice, both under vacuum and under atmos-

pheric conditions. The process showed some considerable

promise and results were reported by the Sugar Milling Re-

search Institute (SMRI). 2 However, the scum formed was

apparently not as stable as that obtained in syrupclarification.

In 1974,a Tate & Lyle syrup clarification process was put

into operation at Noodsberg. This showed that the process

led to an improvement in sugar quality and a reduction in

massecuiteviscosity, but no boiling house improvement was

evident. 3 Sincesugar quality was not a concern at Noodsberg

at that time, this process was discontinued. Similar results

were obtained at Belle Vue sugar mill in Mauritius.' Sugar

quality was improved and the effect on the downstream re-

finery processwasextremelymarked. Massecuites werefound

to be less viscous and easier to cure, but they were not able

to show the benefit of the process on final molasses purities.

They reported that the process led to a small increase of 5 %

in colour, but a reduction in turbidity of the syrup of 67%.

Following the work done on a syrup clarifier in Honokaa,

Hawaii,' it appears that flotation clarification can be oper-

ated without the addition of phosphoric acid. This reduces

considerably the cost of the process and it was decided to

look at this in the laboratory.

A comprehensive laboratory investigation was under-

taken, which showed very promising results as regards tur-

bidity removal and viscosity reduction. This laboratory

investigation established some of the design parameters nec-

essary for the design of a full-scale unit. This was subse-

quently put in at Empangeni and operated for two years

before the mill was closed down. During this period, the

syrup clarifier showed significant benefits as regards sugar

quality and massecuite viscosity. Subsequently, when the

new Felixton mill was built, a syrup clarifier was installed

there as well. Operating experience at both Empangeni and

Felixton has given a better insight into the process and has

enabled it to be optimised.

Results of laboratory work

A laboratory test was devised which involved rapid stir-

ring of syrup in a water bath at 85'C for 3 minutes. The

stirring arrangement was such that air was entrained into

the syrup to saturate it with air. Polyelectrolyte was added

and the syrup was then left standing for 20 minutes.

It was found that turbidity reductions of 80 to 90 % could

be consistently obtained. The measurement of turbidity in

syrup was found to be affected by a number of different

factors, including brix of the solution being measured. The

method in the laboratory manual for South African sugar

factories was found to be unacceptably sensitive to small

changes in pH. Therefore the procedure given in Appendix

1 was developed and used in this work.

Since the initial series of tests were carried out, a large

number oflaboratory tests have been carried out on a variety

of syrups from a number of factories in South Africa and

Zimbabwe. Some slight variations in turbidity removal are

noted, due probably to the differentnatures of the particulate

material. Nevertheless, turbidity removals have alwaysbeen

in the range of 80 to 95 %.

These laboratory trials, however, showed that there was

no significant purity improvement and that the amount of

ash removed was very small. In addition, no improvement

in syrup colour was measured.

These tests were done without the addition of phosphoric

acid and lime. The effect of these additional chemicals on

turbidity removal was investigated in detail. Results are

shown in Table 1, but the general conclusion is that the

addition of phosphate and lime did not improve removal

of impurities or colour and actually gave worse turbidity

removal. This indicated clearly that the simple clarification

without the addition of any additional chemicals,other than

polyelectrolyte, would be a viable proposition.

Laboratory trials showed the optimum flocculant dosage

to be around 10to 15 ppm. These resultsare shown in Figure

1, and indicate that any higher dosage figures do not make

any material improvement. No effect of different type of

polyelectrolytes was established initially. Later tests, how-

ever, showed that TalosepA3 and Separan gave better results

than Magnafloc LT27. In general, it has been found that the

polyelectrolytes with a higher degree of hydrolysis do give 90 ~---,---'~---r----r--r--r---.---r--r----, better results.

x

x

a

x 65 ex Syrup

o 60 ex Syrup

a

x

50

80

co 70 o^ > E ~

-... ' ii

t-

  • 60

88, 78, 77, 80, 62, 33, 33, 39,

Av. turbidity removal %

a

50 100 200 300 400 500 600 800

Phosphate dosage (mg/Q)

Effect of phosphoric acid/lime addition on turbidity removal

100 r---_r---r----_r--~r----r--..,

Table 1

eo

90

40 L-.L.-.L--..L...-..J.-..J.-....L..~...L.....L.....J

40 50 60 70 eo

Temperature ee) FIGURE 2 Effect of temperature on turbidity removal.

From Figure 2 it can also be inferred that turbidity re- moval is independent ofthe brix and viscosity of the syrup.

The viscosity of the 65' brix syrup is about 50 % higher than

that of 60' brix syrup used in the results shown in Figure

  1. Clearly, therefore, viscosity values, within the range en- countered, do not have any effect on this process and the better results at higher temperatures are not due to viscosity reduction, but due to the effect on the formation of floes or on the intramolecular attractions across air/liquid interfaces. Further tests confirmed that liquid viscosity does not affect the removal process. Both clarified and unclarified syrup were subjected to la- boratory boilings. The viscosities of the molasses produced were measured and the results are shown in Figure 3. The viscosity of the clarified syrup and molasses after boiling

was lower by up to 25 %.

The effect of settling time in the laboratory test was in- vestigated. This showed that there was a tailing-off of % turbidity removal between 10 and 15 minutes, and that a retention time above this was unlikely to lead to improved results. It has been found in refinery phosphatation that it is nec- essary to employ dissolved air flotation rather than the sim- pler dispersed air flotation process." Again, laboratory trials indicated that there was no advantage in dissolved air flo- tation and, if anything, the dispersed air flotation gave better results.

5 30

0L.--I.. L...-...L..__--l ....L.. __-J o 10 15 20 25 Flocculant dosage - ppm on brix

FIGURE 1 Turbidity removal measured in the laboratory as a func- tion of flocculant dosage.

70'

10

30

Temperature was found to have a significant effect on tur- bidity removal. This is shown in Figure 2, which indicates that a progressive improvement is obtained up to 85 'C, at which point the effect of temperature levels off.

20

co 60

o E e ~ 50 ' :e::J t-

  • 40

at the correct density level, with the minimum of inlet energy so that turbulence is not created. The depth of the clarifier is important only in providing sufficient height to be able to maintain separate froth and clear liquid zones. Flotation cells in refineries have been built in depths ranging from 0,25 to 1,5 m and Saranin- suggested that a depth of the order of 0.9 m could be optimum. What is more important he suggests,is that sufficient cross-sectional area should be provided to facilitate separation of the scum and that the depth should be fixed by the required retention time.

The Empangeni clarifier was built with an average depth of 1,5 m and a diameter of 4,1 m. A sketch is given in Figure

  1. Ideally, plug flow of syrup should occur so that there are no stagnant zones of long residence time. For this reason, the offtakes were located at the extremities of the clarifier furthest from the feed inlet.

Providing these requirements are adhered to, it is not im- portant whether a round or rectangular clarifier is used. In this case, a circular clarifier was used with a rotating scraper to scrape the scum off the edge of the clarifier and into a launder. In order to allow the scum a certain degree of thickening before being removed, the liquid level is maintained slightly below the sides of the clarifier. The variable level control on the clear liquid outlet was provided to enable control of the thickness of the scum layer to be regulated.

Aeration of the syrup There are three methods of flotation currently in use.' The first is dispersed air flotation where gas bubbles are generated by introducing the gas phase through a revolving impeller or through porous media. Bubble size is of the order of 1 000

MJ. TANK

OLIVER FILTERS TREATED SVRUP

PAN FLOOR

MIXER

REHEL T

SYRUP

TREATED SYRlW

FLOCCULANT

AIR

CRAIN

CRAIN

FIGURE 5 Flow diagram for Empangeni syrup clarification.

HEATER

V

AERATOR

microns in diameter. The second is dissolved air flotation, where bubbles are produced as a result of the separation of the gas from a supersaturated solution. Average bubble sizes are smaller and range from 70 to 90 microns. The third method is to produce gas bubbles by electrolysis. Under th~se circumstances, the bubble size can be smaller than 50

microns,

The third method mentioned above was found to be im- practical in the laboratory. It might be expected that dis- solved air flotation should be more efficient than dispersed air flotation in that the bubbles are smaller and better dis- persed within the liquid. However, the simple aeration pro- cedure used here must be classified as dispersed air flotation. Dispersed air flotation is commonly achieved by injecting air into the suction side of a pump operating at high speed. However, this process has its limitations. If more than about

8 % by volume of air is injected, air binding will occur in

the pump.' In addition, only about 40 % of air injected into the suction of a pump is dispersed in the liquid, and the remainder consists oflarge bubbles which cause undesirable turbulence; thus it was necessary to install a small air release tank immediately before the clarifier. The requirements of the system should be to add the cor- rect amount of air to the suspension as well as to ensure a good dispersion of bubbles throughout the suspension. Initially, air was introduced into a pump running at 2- pole motor speed. Better results were subsequently achieved when a separate aeration pump was introduced. This was specially designed with radial fins and blades in the volute

to ensure considerable shear, thus achieving the necessary air dispersion.

Empangeni syrup clarifier system

The flow diagram of the system used is shown in Figure

  1. The clarifier itself was installed in the top of a syrup tank which was previously a juice clarifier and therefore very much larger than necessary. This tank was divided in two by a concentric partition to separate treated and untreated syrup. This lead to a low cost installation, the total costs for the whole system being of the order of R80 000. Syrup was pumped at a steady flow rate through a flow control valve and a heater in which the syrup was heated to about 85 'c. This was then aerated in a special aerator where air was metered in through a rotameter into the suc- tion of the aerator pump. Following the air release tank, flocculant was added to the aerated syrup and gently mixed into the syrup through the specially designed in-line mixer. This was designed to induce good dispersion of the flocculant within the liquor without significant shear which could lead to breakdown of the floc. Finally the syrup entered through a central feed pipe, the diameter of which increases as the syrup enters to reduce inlet velocities to a minimum.

Operating Results

The turbidity removal achieved over the two seasons for which the syrup clarifier operated, are shown in Figures 6 and 7. Initially, turbidity removal was low, but it can be seen how it increased as design and operational problems were

100 ....... ------.

90

80 %^ Turb.^ Removal

Sugar Pol

(ij

o E 50 e ...^ >-

~ 40

I-

cf. 30

20

10

o

oc,

25 30 35

'--I.--L.-&.-.....................---I-....L-..L.-.L--L.-I--..L-JL-L.-L-..J.--.L-.l........L.....L-..l--JL..-L-I-..J.--.L.....l--..L......L-..L..-JL..-L-I-..L.-a-...a.......I.......L-J 98. 4

o (^5 10 15 ) FIGURE 6 Operational results at Empangeni, 1981/82 season.

o. 35 r-----r---.,..-----'T--......---r----.----r--~--...,-_,--_r-.........,

0 e Before Modification

"

K After Modification

(^61) ....... Cl .s c (^0) 0. °i... ...c Q)o C 0 o E0. ::J £ :.J

o 15 30 45 60 75 90 105 120 135 150 165 180 Time after addition of tracer (mins.) FIGURE 8 Residence time distribution of syrup measured in the Empangeni syrup clarifier before and after modification to the offtakes.

Boiling down tests were also undertaken on the second week molasses composite samples. The final target purity from these tests was not found to be significantly different. Although no significant difference in target purity differ- ence was recorded, a higher molasses brix was generally ob- tained with the clarifier on. The reason for this is evident in Figure 9, which shows that the operation of the syrup clarifier gave a decrease in final molasses viscosity ranging

from 25 % at high solids, down to less than 10 % at low solids

content. Thus the mill had been able to take advantage of the lower viscosities either by boiling higher brix masse- cuites or using less steam and water on the centrifugals. A series of factorial tests was carried out in 1982, to in- vestigate the effect of air quantity, temperature and polye- lectrolyte dosage on performance. Provided the minimum quantity of air was introduced (of the order of 0,04 rnvm! syrup), the effect of quantity of air seemed to be insignificant. However, temperature was found to have a very significant effect, as established in the laboratory. Also, better results were obtained with 30 ppm flocculant on brix, rather than 10 ppm, although this difference disappears at higher tem- perature. These effects are shown in Figure 10. In general, it was found that the syrup clarifier was always able to achieve the same degree of turbidity removal as that obtainable in the laboratory. Subsequently, it has been found that this provides a useful check as to whether the plant syrup clarifier is performing as well as it should by com- parison with the results obtainable in the laboratory. The scum from the syrup clarifier was generally returned to mixed juice. Scum quantity varied considerably, but was

of the order of 5 % by volume. A trial was undertaken where the scum was returned to the filter muds. However, this overloaded the filters and led to a higher pol loss in cake and so this was subsequently discontinued. Empangeni mill was closed down during 1983. Some per- formance results are given in Table 3. The syrup clarifier enabled Empangeni to produce consistently good quality sugar meeting VHP specification and for the first time in many years to achieve molasses exhaustion results compa- rable with the best mills in the industry. Since Empangeni cane was to be delivered to the new Felixton mill, it was felt to be essential to install a syrup clarifier at Felixton II as well. Table 3 Factory performance results at Empangeni 1980/81 1981/82 1982/

EM Industry EM Industry EM Industry

Sugar pol 99,32 99,40 99,17 99,38 99,45^ 99, Export sugar: Colour a*c 560 0,49 0,30 0,47 0,26 0,29^ 0, Ash 0,19 0,12 0,18 0,15 0,16 0, Boiling House Recovery 85,0 87,5 85,7 87,7 86,5 87, Tons sugar- Refinery 66300 93325 50718 Export 6246 7125 66088 MJ Purity 83,3 84,8 84,2 85,7 84,0 85, RS/Ash ratio 1,0 1,1 0,9 1,1 0,8 0, TPD 9,4 6,7 5,5 4,2 3,9 3, Syrup clarification No (^) - Partial (^) - Yes (^) -

90 100

o

FLOCCULANT a 10 ppm on br1x

a

x

o

ox

a

40

o"--........---a..........-->-'--........---a..........-->-"--........---a._.........--o 30

10

x 30 ppm on br1x

50 60 70 BO Temperature ('C)

FIGURE 10 Effect of temperature and flocculant dosing level on performance of the Empangeni syrup clarifier,

100

90

80

70

co> 60

0 E ~ .!:^ >- (^50) ' :e~ l- '#. 40

30

20

(^75 7677 78 ) % Dry solids

FIGURE 9 Final molasses viscosities measured at Empangeni during the 1981/82 season.

200

1600

600

1800

400

2000

G 1400

oN ...<ll Q) Ul 1200 ' e:. .~ Ul 1000 oo Ul :> 800

Further Experience with Syrup Clarification

A small syrup clarification system was installed in the old Felixton mill, shortly before it also closed, during a period of extremely poor cane quality occasioned by a drought. This was done quickly and at low cost, but since scum removal was purely by overflow and not with the aid of the scraper mechanism, results were somewhat below that achieved at Empangeni. A 45 m- syrup clarifier, based on a 20 minute residence time, was installed at the new Felixton mill. Details of the design and installation were very similar to that employed at Empangeni. However, a separate polyelectrolyte system was installed so that different flocculants can be used for juice and syrup clarification. In addition, a plate heater was installed to heat the syrup up to 85 'C immediately before the clarifier. Unfortunately this plate heater has been plagued by blockage of the channels in the plates, due to the fact that small quantities of fibrous bagasse are present in the syrup and form a mat in the inlet ports, effectively blocking the heater. Thus, for most of the time, the syrup clarifier has operated at a temperature of around 58 'c. Figure II shows turbidity removal achieved at Felixton II during a period when attempts were made to optimise the operation of the clarifier. Once attention was given to proper

dosing of polyelectrolyte, turbidity removals of 65 to 70 %

were achieved. Laboratory tests during this period indicated

that at 85 'C, turbidity removal should be 85 %. The tur-

bidity achieved in the plant is only 80 % of that obtainable

at 85 %. Data in Figure 2 and Figure 10 indicate that at

58 'C, turbidity removal should be between 85 and 90 % of

that achievable at 85 'c. Thus it appears that the lower tur- bidity removal which had been achieved at Felixton is due largely but maybe not entirely to the lower temperature. Various options for screening before the plate heater have been investigated at Felixton, and during the comingseason it is anticipated that temperatures will be up at 85 'c. In spite of the fact that turbidity removal is lower than it should be at Felixton, no problem has been experienced in making VHP specification sugar, even when mixed juice purities have been as low as 75. Although it is believed that the continuous A-pans also assist in reducing sugar colour, the syrup clarifier has ensured that sugar quality has been con- sistentlyacceptable. During a period of two weeks, the syrup clarifier was shut down to see whether it had any influence on undetermined loss. No effect could be detected, but there was an immediate effect on sugar quality. Sugar colour re- corded at the Hulett Refinery during this period is shown in Figure 12. The increased colour can be shown to be sta- tistically significant at the 99 % confidence level. Experiments have also been undertaken at Felixton to in- vestigate the method of air addition. A simple sparger in- stead of the dispersing air pump has been investigated. Although the simple sparger appears to give the same kind of turbidity removal, the appearance of the scum suggests that the aeration pump system should give much better re- sults. This will be repeated once higher temperatures have been achieved, and on different qualities of syrup.

2000

1500

E c

oN '<t

(^10) .. 1000 ~ o < o

Syrup Clar Off

oL-...L------J'-----.£---J,~____L__..........__~.,....-.........--....L.---....., o

500

FIGURE 12

TREATED SYRUP OUTLET

LEVEL

IN-LINE MIXER

DRIVE

OUTLET

SYRUP OUTLET

POLYELECTROLYTE INLET

~

-f--.....-. RAW SYRUP INLET

FIGURE 13 Sketch of the syrup clarifier installed at Triangle, Zimbabwe.