Professional Documents
Culture Documents
MARCHES 565
In the absence of the author the Chairman Dr. Douwes Dekker presented
the following paper.
Paper
LIMING OF CANE JUICES
J. MARCHES
Tiedeman and Van Kerchem, Surahaia, (Indonesia)
INTRODUCTION
In the liming of cane juices for the manufacture of raw sugar the amount
of milk of lime added to the mixed juice results in a weakly alkaline reaction
(in Java from pH 7.3 to pH 7.8). The result ,of this liming process is a purification
of the juice ; the resulting clarified juice can be used without any difficulties for
the manufacture of standard raw sugar. This purification is cheap. The amount
of lime used as an average by the Java sugar industry is 0.75 kg. CaO per metric
ton of cane, corresponding with 5 liters of milk of lime of 15"Be' per m3 of mixed
juice.
For a good understanding of the liming process it is necessary to know
exactly the reactions taking place in the liming. When a certain amount of
milk of lime is added slowly to cold or heated mixed juice, the formation of a
precipitate can be observed, in the beginning a small quantity but very
voluminous. With an increased addition of lime the formation of flocks
can be obser ed, settling easily. If this liming is demonstrated in a glass vessel,
?
we observe hat after a certain time of settling the precipitate sinks to the bottom
of the vessel and the juice is practically clear, having a yellow to reddish brown
colour. The turkidity and suspended impurities have all been concentrated in
the settled flocculated precipitate.
These changes in mixed juice as a result of the addition of lime and the
application of heat are partly physical and partly chemical. In the precipitate
are eliminated the suspended non-sugars in mixed juice but together with
a certain amount of organic and inorganic non-sugars present in solution
in the mixed juice. The removal of the different types of non-sugars in clarification
is incomplete, E-ut it is satisfactory for the manufacture of raw sugar. The number
of studies on the chemisty and the physical chemistry of clarification is extremely
great and we know at this moment in how far it is possitjle to remove certain
types of inorganic and organic non-sugars by the liming process. But what is lacking
is the predetermination of the maximum conditions for non-sugar removal, if
a mixed juice has to be processed of which we know nothing as to its composition.
The criteria used commonly by sugar technologists to judge the rqsults of the
clarification are : rapid settling of the formed precipitate, light coloured clarified
juice of a p H of approximately 7.0, free of turbidity and a maximum concentration
of the settled muds.
566 SYMPOSIUM CANE JUICE CLARIFICATION
The main factors determining the results of the clarification are : the
composition of the mixed juice, the temperature to which the juice is healed before
and after liming, the p H traject and p H levels used in liming, the time the juice
is subjected to certain temperatures and pH values, the regularlity in processing
and the quality of the milk of lime. To prevent decomposition of reducing
sugars and inversion of sucrose the processing of cane juice sets certain limitations
to the acceptable combinations of time, p H level and temperature. But even with
these limitations a great variation is possible in the liming technique.
COMPOSITION OF THE MIXED JUICE
TgmperatUfV :
The increase of the temperature of the mixed juice to be limed accelerates
the different reactions and particularly the realization of certain reaction equilibria.
The old practice was cold liming, after which limed juice was heated to a
temperature slightly above 100" C. and boiled in a defecator to eliminate air in
a the hot limed juice before it was transferred to the settling tanks. This method of
liming makes it practically impossible to obtain a constant p k of the clarified
juice. This was partly the result of the fluctuating pH differences between limed
juice and clarified juice. Hot liming has resulted in a tremendous progress to have
a constant p H difference between the limed mixed juice and the clarified juice.
Hot liming resulted in an improved control of the pH of the clarified juice. A
secondary effectis that hot liming, under practically all conditions, results in an
improvement in th: non-sugar elimination particularly of proteins and the
precipitation of the inorganic phosphates.
i
The present technique is liming at high temperatures either at boiling
I temperature or somewhat lower, as for as 70°C. The heating of the mixed juice
has as advantage that microbiological reactions are completely suppressed. A
disadvantage mentioned occasionally in the literature is that the haating of acid
mixed jutce would cause ,some sucrose losses by inversion. But a calculation
shows that with modern juice heaters the time during which rlze juice has been
subjected to a high temperature at a p H between 5 and 7 is so short that the sucrose
losses by inversion are negligible (see the paper by Dr. P. Honig in this Symposium
"Chemical Reactions in the Settling of Limed Cane Juices"). If factories wish to
compromise on3kis point, there is no objection to lime the juices at 90°C.
pH:
To obtain the maximum removal of non-sugars and to prevent a
non-admissible destruction of reducing sugars it is necessary that the amount of
milk of lime to be added to the mixed juice should t e such that it results in
a clarified juice to be sent to the evaporators with a p H of 7.0 or slightly over
it. Between 1934 and 1940 the average p H of the clarified juice of the Java raw
sugar mills was 7.0 to 7.2. The limed mixed juice had an average pH of 7.3 to
7.5. Considering this final pH of limed mixed juice and clarified juice it is evident
that the mixed juice can go through a large p H traject. , We assume that 1 m3 of
mixed juice with a pH of 5.5 has to be mixed with 5 litres of milk of lime of
15" Be' to obtain a pH in the limed juice of 7.5. The mixing of juice and milk
of lime can be done in the two following extreme ways :
(1) Gradual addition of juice to the milk of lime.
(2) Gradual addition of milk of lime to the juice.
If homogeneous mixing of the two con~ponentsis assumed, we will have
in case no. 1 : the first added juice will reach a pH of 12.5, decreasing with the
SYMPOSIUM CANE JUICE CLARIFICATION
addition of juice to a pH of 7.5. In case no. 2 the juice will go gradually from
a p H of 5.5 to 7.5, therefore, no high alkaline reactions will occur in this liming
process. It has, however, to be understood that homogeneous mixing is a
technological problem in itself and even in case~no.2 it will be unavoidable that
some of the juice particles will be exposed to a high alkalinity.
Another system of liming is by the use of saccharate. In this method 10%
of the cold mixed juice is mixed with all th.e lime to be used in the clarification,
the lime will dissolve in the juice to saccharate and this saccharate solution is
applied for the akalination of 90% of the heated mixed juice. In this case a part
of the juice will reach. a high alkalinity at a low temperature which alkalinity
decreases to a pH of 7.5, In the main part of the juice the pH increases from
5.5 to 7.5 in the liming process. This pH increase is instantaneous if the liming
with saccharate is done continuously under perfect conditions of mixing.
Time :
The holding times of the juice in the different steps of the purification process
are determined by the juice volume of the reaction vessels and crushing rate. This
holding time will be determined by the variation in the grinding rate. It is still
an unanswered question which holding times have to be considered as maximum.
In liming tanks we can observe that the different factories go to very great extremes.
The smallest liming tank we have ever seen in operation had a juice content of
only 200 litres, or a holding time of only 15 seconds. At another factory we have
seen a liming tank of 15,000 litres juice volume for a juice capacity of 16 litres
per second, or with a holding time of 938 seconds.
The experience has shown that for the preparation of saccharate a holding
time of 5 minutes is sufficient to dissolve milk of lime of good quality quantitatively
in cold mixed juice.
Quality of the milk of lime :
It is essential in the liming of juices that the milk of lime is of the highest
quality and has a uniform composition. We have to understa 8 under these
R
characteristics the purity of the lime, the density of the milk of lme, the degree
of dispersion of Ca (OH), and the reactivity of the lime. The best results are
usually obtained with a milk of lime of 5 to 7"Be'.
In using saccharate as alkalising agent it is customary to mix cold mixed
juice with milk of lime in a ratio of 9 volumes of mixed juice with 1 volume of
milk of lime of 15" Be'. The exact and accurate dosage of saccharate is easier than
the use of milk of lime of 5" Be'.
I
In juice heaters it is essential that the off flow of condensate is uniform and
that there is a satisfactory removal of uncondensable gases, as the quantity of
uncondensable gas in using juice vapours can be quite considerable. Theuse of
recording thermometers to control the juice temperatures is absolutely necessary
in modern mills. Which deviations are permissible in the heating juices to be
subjected to hot liming is a subject for further investigations. Furtheron we refer
for the heating of juices to the paper presented by Mr. Chs. G. M. Perk " Systems
of heating juices ".
Liming tanks : /
The addition of milk of lime or saccharate of lime to the heated mixed juice
is usually done in defecators. To maintain a uniform pH in the out flowing limed
juice, a good mixing of the defecator contents is required. The mixing is done
in different ways. As a rule the equipment is considered to be satisfactory when
the limed juices show a good settling and the clarified juices are clear. However,
well defined specifications as to the mixing of juice and lime, leading to optimum
clarification, are not known,
In Figures 2-b, we give a number of installations as used in Java for the
liming of mixed juice.
(a) In Fig. 2, a small tank of 200 litres juice content for a juice capacity of 13
litres per sec., is used as liming tank. The mixing is achieved via the energy of the
flowing juice. Tt is possible with this kind of arrangement to get a good mixing of
lime and juice, but it is occasionally very difficult to maintain a uniform p H of the
outflowing limed juice. Therefore, a buffer tank of 5000 litres was put before
J. MARCHES 57 1
the liming tank. Furtheron an indicating p H meter was used. Nevertheless, the
operator had to give his full attention, as the system is rather sensitive. A small
change in lime addition causes a rapid change in p H of the limed juice.
(b) In Figure 3 we have given a liming tank of a larger dimension. If the
mixing in this kind of tank is insiufficient, there is always a certain lag in the p H
of the outflowing limed juice. This system is preferred where the operator is
a little bit slowly acting and lazy. The liming tank given in Fig. 3 is an old pan
used for a capacity of 33 litres of mixed juice per second. This system is used for
hot liming. The juice is kept at boiling point temperature by the admission o f
steam to the calandria. The evaporation by the calandria results in a satisfactol y
mixing of mixed juice and milk of lime. The p H control and the attendance of
the dosage of milk of lime have to be located on the same spot. But this last
principle has to be applied in all liming installations.
CPOARGE.LINE OF
WEAfE.0 MIXED JUICE
6 A 95°C
pump. The juice delivered via these pumps is introduced at high velocity via
nozzles or spray pipes into the diffuser. This results in a juice circulation as
.indicated in Fig. 4. The capacity of this installation is 16 litres of juice per
second. The circulation pump has a capacity ,of 19 litres per second. The
juice voiume of the liming tank is 15,000 litres, being according to our opinioll
very large.
-
RCULATION SYSTEM *MILKOF LIME
OLD PAN USED DOSAGE
As DEFEcArnW UME
\
\
1
I
I
I
1
1 1 I
INLET OF MIXED
JUICE OF f 9 0 e C
VlA SPRAYER
IN R3WUSOQ
OUTLET OF
DEFECATED
SUBSIDERS
OVERFLOW
TO SUBSIDER
JUICE VOLUME OF
OEFECAVOR
6580 L I T E R S
circulation, we can use as an indicator for the circulation intensity the circulation
number. This is the number of times che juice content circulates pzr minute.
We have found that good mixing performance is obtained if the circulation number
is 2.5 to 4.
J. MARCHES
A liming tank as given in Fig.6, juice volume 3000 litres, was used with good
results for a capacity of 16 litreslsec. Fig. 7 gives the main dimensions of such a
liming tank. The propellor velocity was found empirically. To reach this
end the tank was filled with water, the propellor set in action and then a bucket
full of KMnO, solution pas emptied at once (time=O) into the concentrical tube.
means of a stopwatch was found how many seconds were needed until the
KMnO, colour became visible after one complete circulation of the tank content.
NOW the velocity of the propellor was adjusted until one circulation lasted 15 to
20 seconds, giving a circulation number of 4 to 3. This means the capacity of
the circulating liquid is 4 to 3 times the tank content. Assuming the latter as 3000
litres, they circulate in the tank 12000 to 9000 litreslmin.
The use of circulation pumps mounted outsige the reaction vessels has not
e' always been an engineering success in Java in prewar time, especially if kearings
came into contact with alkaline juices. If a mixing device is installed as given in
Fig. 6, it is advisable to mount the propellor similar to a suspended centrifugal.
It can be stated that the maintenance of a constant pH in the limed juice
is better if a more perfect circulation exists. It is also certain that a number of
on the destruction of reducing sugars has been influenced by imperfect
mixture of mixed juice and milk of lime. The better the mixing in the liming
tank, the less is the possibility for locally high alkalinities and a destruction of
reducing sugars. It is a logical conclusion that with perfect mixing in liming
tanks higher temperatures can be applied in the liming of juices without danger
for nonpermissible destruction of reducing sugars.
Dosage of millc of lime and sacchal*ate.
The purpose of the dosage of milk of lime or saccharate is to add so much
reagent to the mixed juice that the mixed limed juice has a pH between 7.3 and
7.8. The amount of milk of lime necessary to obtain this final pH varies with the *
composition of the mixed juice. In Java this variation is between 2 and 6 litres
milk of lime of 15" Be' per 1000 litres of mixed juice. It is impossible to realize
a constant pH of the limed juice with a constant and prefixed addition of milk
of lime. Automatization of the dosage of milk of lime is only possible by using
the pH fluctuations of the limed juice as impuls for the adjustment of the dosage
mechanism for the milk of lime. It is possible to use a constant amount of milk
of lime per 1000 litres of mixed juice but only as a prel'iming or first liming, to be
followed by a second liming adjusted to the lime requirements of thejuice processed.
The common system in Java is to add the milk of lime hand operated.
For the dosage are in use ; common plug cocks, y-shaped valves Nielsen plug
cocks or nozzles with regulator pins. The p H of the limed juice (determined
calorimetrically or electrometrically) is an indication for the operator how the
regulating mechanism for the addition of milk of lime has to be adjusted. The
regulation mechanism for the addition of milk of lime has to be sufficiently
sensitive but not oversensitive. Furtheron it must be possible to correct a too
J. MARCHES 577
low pH rapidly by opening the dosage mechanism to the full extent. Is the p H
value too high, it is necessary to shutoff or to reduce the flow of milk of lime
and to wait that a sufficient amount of mixed juice has entered the liming tank to
obtain the correct pH. It is, , of course, understandable that the regulating
mechanism for the milk of lime has to be adjusted to the juice volume of the
liaing tank. A regulating mechanism has to operate under all circumstances
in such a way that in the same position the same amount of milk of lime is
deiivered per unit of time. For this it is necessary that the milk of lime has
a constant composition and also that the pressure of the milk of lime before the
regulating mechanism is constant. A simple solution to realize this is to use a
small reservoir (net volume 150 to 250 litres) with a continuous overflow as given
in Fig. 9. It is posssible to use with such a reservoir a small pressure height for
the milk of lime, enakling us to apply a larger outflow opening in the regulating
mechanism. The opening of the outflow is reciprocal mith the velocity of
outflow or reciprocal with the r o 6 o f the pressure height : V=cl/2gh*).
This means that if the pressure height of the milk of lime is 9 cm., the
outflow opening can t e twice as large as at 36 cm, and three times as large as
at 81 cm. The outflow co-efficient c for milk of lime increases with increased
pressure heights. For circular outflow openings and milk of lime of 11" Be' this
co-efficient increases for pressure heights from 10 to 50 cm. from 0.90 to 0.95. As
a rule we use the co-efficient of 0.90.
Besides by the application of small pressure heights of the milk of lime, a
larger outflow opening can ke obtained by the use of more diluted milk of lime.
An example may illustrate this point :
A factory with a capacity of 1500 tons of cane per day produces an amount
of mixed juice of approximately 15 litres per second. The average lime addition
is equivalent to 5 litres of milk of lime of 15" Be' per m3ofjuice. We have to add
the following amounts of milk of lime per unit of time :
15 x 5=75 ml. milk of lime of 15" Be' per second
148
or : 75x-=118,,
94
,, ,, oflOoBe' ,, ,,
148
or : 75 x --=241
46
,, ,, ,, of 15" Be, ,, ,,
or : 750 ml. saccharate 1 : 10 per second.
Manual dosage of milk of lime.
Assume we want to calculate the dimensions of a nozzle with an adjustable
pin regulator as given in Fig. 8 for a factory with a capacity of 1500 tons of
cane per 24 hr., with a liming tank of 3000 liters the uEe of milk of lime of 5"Be'
and a pressure height of the milk of lime of 20 cm., the calculated velocity of
outflow of milk of lime is :
~=c2/%h=0.92/2 x 9.78YT2-1.78 m./sec.
- - m . .
OISCHA!&€ INLET OF
OF 6RIT MILK OF LIME
Fig. 8. Tank for milk of lime with nozzle and regulator pin.
We want to calculate also the desired maximum outflow area when the full
opening of the nozzle is applied. For this calculation we suppose that the
juice in the liming tank has to be br~ught from 6 to 7.5 pH in one minute,
I
3. MARCHES 579
A nozzle diameter of 2.75 cm. corresponds to this area. For the practical
construction of the nozzle we take as the diameter 30 mm. The adjustable pin,
a smooth cone, has to be made of such dimensions that if a length of 150 mm.
is put into the nozzle, the opening is completely closed, as shown in Fig. 9. The
mechanism for moving the regulating pin upwards and downwards has to go
smooth, so that the pin cone can easily be brought to a known p~sition. It is
important that the pin position is indicated to the operator in a clear way. This
can be done by a vertical or horizontal scale, depending on the means of
transmission between the hand operatedlever or hand wheel and the regulator pin.
The extreme positions of the pin, full open and closed, should be easily reached
without too much turning of the lever or wheel.
The normal (average) position of the adjustable pin,in the nozzle corresponds
to a ring-shaped opening of 1.35 cm2. In the normal position the pin has to close
a cross section 0 , to be calculated from :-
n/4 x 32-0=1.35
0=5.72 cmV2
This area belongs to a diameter of 2.7 cm. In the normal position of the pin
therefore the opening between nozzle andpin cone is 1.5mm. clogging ofthis
opening is exceptional if well screelied milk of lime of 5"Be' is used.
H~wever, it is recommendable to let thi milk of lime from the nozzle flow
580 SYMPOSIUM CANE JUICE CLARIFICATION
DOSAGE APPARATUS
FOR MILK OF L I M 6
H OF maousn ? L o w OF
OR MILK OF LIME
IM~,TION JUICE HEATER ? I O ~ * C
TANK FOR
LIMED JUICE
I Fig. 10. partial automatization of the addition of milk of lime to mixed juice.
I Liming exclusively with saccharate is possible, if every moment only the needed
amount of saccharate can be prepared. The liming equipment as given on
SYMPOSIUM CANE JUICE CLARIFICATION
Fig. 11. Partial automatization of the addition of saccharate in the liming process.
The mixed juice not used ill the preparation of saccharage flows via nozzle
A, tank, pump and heaters (lOO°C.) into the liming tank. If nozzle A is given
a large diameter and is provided with a regulating pin, this pin can be used to
adjust for considerable changes in milling capacity.
The ratio mixed juice to milk of lime for the preparation of saccharate can be
chosen and fixed as desired, using for instance 5, 10, 20 or 30% of the mixed juice
I
PIETER HONIG
f DISCUSSION
Mr. S. N. Gundu Rao referred to the present day availability of proportioning pumps for
liming of cane juices which where necessary can also be linked to the juice flow.
Dr. H. W. Kerr referred to the variation in the quality of juices in Queensland and said
that it is the p H controlled unit that takes care of such variations.
Mr. Clayton referred to the several factors working to the detriment of the defecation system
and in particular to staleness which also affects the bufferring capacity of the juice. Experiments
have indicated the desirability of adding some stronger alkali in addition to lime. With the
adoption of hot liming the problem of adding lime to hot solutions under pressure introduces
further difficulties. The relative importance of proportional addition and fixed addition needs
study.
Dr. Doss stated that while using partly strong alkali may have advantages, the possible
contribution of alkali to molasses formation should be kept in mind.
Mr. Gundu Rao pointed out that in the sulphitation system of clarification proportioning
is of great importance.
Mr. ~ e l f iposed the question what is clarified juice and considered that the chief objects
of controlling pH are prevention of inversion and of destruction of reducing sugars.