Professional Documents
Culture Documents
1974 Lu A Study of Crystal Content in Automatic Sugar Boiling
1974 Lu A Study of Crystal Content in Automatic Sugar Boiling
ABSTRACT
The successful application of automatic methods of sugar boiling has
been hindered by some factors which are not clearly understood. Actual
measurement of crystal content has been made and a mathematical
relationship between crystal content, inter-crystal distance and crystal size
was established. It is shown that during sugar boiling the distance between
crystals decreases linearly with size as the crystals grow, while the crystal
content increase is proportional to the cube root of crystal size. Before the
feeding of sugar solution to the pan is started, the crystal space should be
adjusted until equal to the crystal size, if a smooth boiling is desired. Low
grade molasses requires a reduced distance between crystals to maintain
suitable supersaturation when the circulation slows down due to the
increasing massecuite volume.
Three conventional methods of instrumentation are experimentally tested
and compared. Mobility control which responds to both viscosity and crystal
content, gives a better picture of the sugar growing environment and operates
more reliably than other methods of control. Comparing the actual measured
crystal content value with the value calculated from the mathematical
equation, a fairly accurate operational guide can be obtained.
Two examples of a mobility control system for low grade massecuite
boiling are presented. By maintaining an optimum growing environment
with regard to the viscosity and crystal content, a mobility control system
involving repositioning of the control point in relation to the crystal content
can be applied t o all stages of boiling whether the feed material is low or
high grade.
INTRODUCTION P
I n sugar boiling, supersaturation is the most important factor in both pure
and impure sugar solutions. An uneven distribution of supersaturation2
results in problems in the operation of a factory pan. Factors causing an uneven
distribution of supersaturation in a pan are material purity, circulation velocity,
crystal content and pan design. A complete sugar boiling cycle consists of
4 phases, namely; evaporation, seeding, growing and tightening. Each phase
has its characteristic features and different requirements. I n practice, the
circulation, crystal content and supersaturation distribution play equally
important roles in the smooth operation of a pan. The circulation velocity and
the flow patterns of massecuites of different grades of material have received
a great deal of attention as indicated by the work of B o ~ w o r t h ,Wright1°
~
and others. However, the effects of circulation and the behaviour of the crystal
content are yet to be clarified. Successful application of automatic sugar boiling
using various measurement techniques has been reported from time to time.
Generally speaking, successful application of these methods such as boiling
1340 MANUFACTURING - PROCESSING
4) Purity of mother-liquid.
Some simple techniques are introduced to determine quickly the above
4 parameters which together with continuous recording from 3 conventional
instruments are used to provide a clear picture of the boiling process.
Four calandria type vacuum pans with a working capacity of 50 m3
each are used for different sugqr liquids. The boiling materials used are raw
sugar, syrup and A- and B-mol$$ses. The test runs were first operated manually
and then conducted by automatic operation based on one instrument'with the
others recording only. To meet conventional TSC practice, boiling of low-
grade liquid (B-molasses) from seeding up to a crystal size of 0,25 mm is called
a Cs-strike. Further growing of the crystals is conducted in other pans after
cutting, up to a size of 0,35 mm. A- and B-strikes continue the growing up to
0,6 mm. The final size of extra refined granulated crystal is about 0,35 mm.
The above tests on AB-, C-, Cs and R-strikes have been conducted over 4 years
since 1968.
A frequency of sampling of the massecuites of 2-5 minutes during the
seeding stage (2 min for R-strike, 5 min for Cs-strike) to 10-15 minutes during
the growing or tightening stage was employed. Part of the sample was spread
immediately on a microscope slide. An inverted microscope attached with a
Philips closed circuit. T V displayed enlarged images on a 585 mm screen
and with the aid of a precalibrated scale, the length of the crystal b-axis
could be easily and precisely measured. The crystallisation rate in units of ylmin
was easily calculated from the sizes of consecutive samples. Photographs were
taken for the calculations and to check the coefficient of variation. False
grain or remelting could be clearly and immediately checked to prevent abnor-
mal operation. The remaining part of the sample was used to fill a specially
designed sampler shown in Fig. 1, from which the mother liquor was separated
from the crystals by vacuum. Attention has to be paid to the screens for accurate
measurements. Nylon filter cloth is recommended for high grade massecuite,
while a metal centrifugal screen is suitable for medium and low grade masse-
cuite. A laboratory centrifuge was used for separating extra fine seed below
0,07 mm in the low grade Cs-strike.
The K-ratio was calculated by volume as shown in Fig. 1. The void space
between crystals was ignored because of the irregular shape and CV of the
CHEIN-JAN LU
- --
cD Strike I D mm 1 H mm
25
35
crystal
mother-liquid
(H - Ho)/Ho by
volume
Wc/Wmq by
weight
FIGURE 1. Massecuite sampler.
RESULTS
Behaviour of crystal content
A massecuite is a solid-liquid mixture and changes in the physical pro-
perties of either crystal or mother-liquid or both change the characteristics
of the massecuite. Supersaturation is very important in sucrose crystallisation.
However, too much emphasis on the supersaturation of mother-liquor without
regard for the crystals cannot yield a reliable sugar boiling. An optimum crystal
growing environment should consider not only supersaturation but also crystal
'"I
content and circulation.
crystal
crystal
surface
(1
1342 MANUFACTURING - PROCESSING
The supersaturation profile in the mother-liquor between crystals is
schematically shown in Fig. 2.
The film close to the surface of the crystal is known as the reaction layer 6,
and the surrounding layer is called the diffusion layer 6,. The supersaturation
within these layers decreases towards the crystal surface. Beyond these layers, at
a certain distance from the surface, say 1,the supersaturation Sh should always
be strictly maintained within the metastable zone, otherwise false grain would
appear if any shock or disturbance occurred. This is the case during seeding,
when the seeds are extremely small. However, the supersaturation Sg in the
neighbourhood of the diffusion layer can be raised and maintained close to
the upper limit of the metastable zone, if h is regulated to be sufficiently small,
i.e. h 6 6, + 6, without significantly restricting the free motion of the masse-
cuite. G.V.Genie3 estimated the optimum value of h to be 0,l mm.
The crystallisation rate depends mainly on the supersaturation in pure
solution (Noyes-Whitney equation) and in impure solution.ll I t is rather
difficult to adjust h to the proper value to maintain an optimum supersaturation
a t the highest crystallisation rate, when there are so many other factor^^>^>^
involved which tend to limit the maximum crystallisation rate.
From Fig. 2, it is clear that the crystal content and h are somehow inter-
related. An empirical approach to the investigation of the behaviour of the
crystal content was undertaken. A relation between h and crystal content can
be derived, based on the following assumptions.
1) The crystals contained in the massecuite are uniformly distributed so
that the number of crystals per unit volume is everywhere the same.
2) The b-axis is taken to represent the cube length of a n irregular crystal.
3) There is little change in the numbers of crystals from seeding to the
final growing stage. I t is estimated that a variation in numbers of less
than 40% occurs-if there is full seeding under normal automatic opera-
tion.
*--- ---------.---.
4
Crystal
1"
L-,-, 1 FIGURE 3. Size of single cube crystal.
Fig. 3 shows a single cubic crystal of size ,!with increment A,!. 6 is taken
for the average half distance between 2 crystals and A6 the change in 6 during
the boiling. The total volume of the massecuite Ms in a pan, is equivalent to
the total number of crystals Ns times the volume of a n individual crystal
together with surrounding mother-liquor :
-
CHIEN-JAN LU 1343
Ms = Ns (R + 2AR + 2 (6 +
The volume of mother-liquid M is ,
M, = Massecuite - crystal = Ms - N, (R + 2AR)3
Rearranging
Mq -
- - (1 + 2AR + 2 (6 + A6))3 - (R + 2AR)3
In our case, the crystal to mother-liquor ratio by volume is the K-ratio,
which is easily determined by the sampler shown in Fig. 1. Let n and m,
stand for the numbers of crystal and the amount of mother-liquid respectively
in the sampler.
K =
n(R+2AR)3 m,
or - =
(R +2 ~ 4 3
*4
n K
From assumption 1, the K-ratio is the same whether it is in a pan or
from the sampler. Thus M,/N, = m,/n
Let L be the length of an incremented crystal i.e. L = R 2AR. The actual +
distance between crystals is given by 2 h = 2 6 +
2 8 6 . Then the half-crystal
distance h may be written in terms of L and K as
L /I
A=-
2
(d- +1
K ,.,
- 1)
(1)
TABLE 1. Sample data of crystal content, size and distance. %,
Strike Refined A Cs C
samp.
No. L m m K mm Lmm K mm L m m K mm L mm K mm
1 0,09 0,114 0,151 0,25 0,22 0,110 0,04 0,lO 0,246 0,20 0,135 0,103
2 0,14 0,130 0,070 0,30 0,35 0,085 0,lO 0,14 0,051 0,29 0,39 0,078
3 0,16 0,238 0,058 0,40 0,58 0,080 0,11 0,13 0,053 0,30 0,43 0,074
4 0,18 0,258 0,062 0,42 0,56 0,082 0,12 0,23 0,044 0,30 0,50 0,066
5 0,22 0,666 0,039 0,42 0,68 0,073 0,13 0,21 0,052 0,35 0,58 0,070
6 0,23 0,739 0,039 0,46 0,95 0,064 0,14 0,31 0,043 0,35 0,66 0,063
7 0,32 1,163 0,037 0,50 0,90 0,070 0,14 0,34 0,041 0,35 0,76 0,057
8 0,32 1,294 0,033 0,50 1,OO 0,065 0,16 0,43 0,039 0,35 0,88 0,054
9 0,36 1,786 0,029 0,55 1,21 0,060 0,16 0,50 0,045 0,40 1,OO 0,052
10 0,36 2,900 0,019 0,55 1,73 0,046 0,17 0,50 0,038 0,41 1,31 0,043
11 0,39 3,667 0,015 0,55 1,80 0,040 0,17 0,53 0,036 0,42 1,30 0,042
12 0,40 4,571 0,013 0,60 1,80 0,044 0,17 0,49 0,038 0,40 1,73 0,034
13 0,60 2,33 0,036 0,18 0,75 0,039
14 0,66 3,20 0,029 0,19 0,70 0,033
15 0,65 4,OO 0,022 0,19 0,80 0,027
16 0,70 6,OO 0,017 0,20 1,00 0,026
Legends: L - crystal size (mm)
h - Crystal half distance
K- Crystal to mother-liquid ratio
I ' I 1 I I
I 1 / Strike b rn r2 Purity
R 0,087 0,184 0,89 96-92
I 1 A 0,156 0,195 0,93 84-75
Cs 0,079 0,255 0,87 68-58
1 C 0,157 0,277 0,92 64-50
J
L = crystal size rnrn
I I 1 I I I
0 0,l 02 0,3 0,4 03 0,6 0,7
FIGURE 4. Crystal size vs crystal distance.
Actual determinations of the crystal size L and the K value were carried
out under automatic mobility control, from which the crystal distance h was
calculated using equation (1) as shown in Table 1. Fig. 4 shows a family of
h - L curves from Table 1. Two significant conclusions can be derived.
1) Whatever the kind of strike or initial crystal size, the critical point
a t which crystal growing is started lies along a dotted line with the
I F
same K ratio such that the factor (f/ -
K
+ 1 - 1) is equal to 1,
-
Supersaturation
\ Crystal
distance
Temperature
I TI Mother Crystal
ring]
Crystal
ji content
C
Legends :
BPE = Boiling point elevation
C = Conductivity
M = Mobility
p = Purity of mother-liquid
pm = Mother-liquid density
p, = Sugar solution density
q, = Mother-liquid viscosity
T = Temperature
V = Vacuum pressure
S = Steam pressure
or quality of feed material show different effects on these curves from which
some evaluation of the measurement methods is possible.
Figure 6 shows 3 conventional measurement methods each of which is
influenced by certain variables. The measurements change when the main
variables (double line) vary. These main variables are for example the mother-
liquid density and purity in boiling point elevation, viscosity in conductivity,
viscosity and crystal content in mobility. Both indirect variables (solid line)
and operational variables (dotted line) may affect the measurements. From
Fig. 6, it can be readily seen that operating variables have more influence on
BPE than conductivity or mobility, that both BPE and conductivity lose their
sensitivity during the tightening stage, and that the conductivity is very sensi-
tive to purity.
The measurement methods so far developed cannot fully meet the control
requirements for a n optimum growing environment. BPE and conductivity
have a very good relationship with s u p e r ~ a t u r a t i o n .BPE
~ > ~is therefore excellent
for seeding but is unstable in the face of vacuum and/or temperature changes.
Conductivity is good for seeding and growing of low and medium grade material
and is popular because of its simplicity, although it frequently requires a
purity check. D. Aharil discovered that the resistance decreases slightly with
increasing crystal size. Mobility is the only method that can actually respond
to both parameters - viscosity and crystal content. Because of this characteris-
tic, the mobility may theoretically provide better control than the other two,
but only if the behaviour of the crystal content is clearly established.
I n practice, the response of the mobility curve (Fig. 7) to intermittent
feed and/or operating variables is very reliable. The relationship between
mobility and crystal content under constant viscosity (control by conductivity)
is shown in Fig. 8. Two dotted lines indicate the upper and lower limits for
safe operation. Beyond the limits, false grain or remelting occurs. Due to the
purity drop (Fig. 7, 9, 10) point B has more room for operation than point A.
This is the reason why low grade material is easy to boil to yield good crystals.
I t is reasonable to conclude from Fig. 5 that an increase in level is solely
a n external disturbance which upsets the crystaI adjusting ring. The purity
also upsets the balance of the mother-liquor loop. However, the extent of this
effect is evidently not as large as that of level. This is the reason why mobility
can supply more reliable information than conductivity or BPE. Because an
increase in level is the main initiation for boiling, there is therefore no doubt
that a continuous resetting of the mobility control point according to the level
signal can lead to a satisfactory result. The proportioning level signal does not
exactly match the mobility pattern due to the crystal content. However, the
difference is very small during the whole growing stage. Practical operational
tests prove that no significant deviation appears if the mobility control point
is set a little bit lower than the middle of the metastable zone.
-- N P o, Time co
9 I I I I I I I I r-
g. -
P I
N P o, Time m
1350 MANUFACTURING - PROCESSING
Figures 9 and 10 show basic mobility control systems for the low grade
seeding-growing operation and the low grade growing-tightening operation
respectively. The heart of the system in Fig. 9 is a 2-pen mobility recorder con-
troller (MRC),which records both level and mobility signals at the same time.
These 2 signals tell the whole story of the sugar boiling cycle. The mobility
signal is obtained from the torque transmitted from a pilot mixer. M R C
delivers a n output signal to the control valve CV,, which regulates the molasses
feed to maintain the growing environment according to the mobility control
point. The control point is continuously reset through a ratio level signal from
a computing relay (R). Control valve CV, has two purposes - one is to feed
water for footing preparation, which may be excluded if molasses is prepared to
65 Bx outside the pan, and the other is to balance the evaporation just after
seeding to bring h together. Under normal conditions, a timer T can be pro-
vided with a fairly accurate estimate of h to let Lo = 2h0. The sequential
operation of the Cs-strike is set up by many simple components such as pres-
sure switches PS to energise (dotted arrow) solenoid valves SV which in turn
start or terminate feeding.
Automatic operation is started by pushbuttons SW, and SW, which
energise SV1 and SV, allowing 103 kPa air pressure to open CV, and CV,
for the footing. When the footing preparation is finished, PSI and PS, turn off
SV, and SV,, once the level signal and mobility signal reach the points L,
and M,. When the steam supply starts the concentrating of liquid, the^ mobility
rises continuously. When the mobility signal reaches point M,, PS,, actuates
a pilot light and an alarm to announce seeding. Point M, should be set in the
lower part of the metastable zone in order to secure really full seeding. As soon
as mobility reaches M, (upper part of metastable zone), PS3bactuates a timer T
which energises SV,. The ohtput control signal from MRC passes through
SV,, SV,, SV, to CV, and throttles balancing water to maintain proper super-
saturation for seed growing. Thfiduration of the water feed is set by timer T,
which shuts off SV, to switch the control signal directly to CV1 for molasses
feeding. From now on, mobility gradually rises up to M, in response to the
level increasing from L, to L,. The range span between M, and M, should be
precalibrated relative to the total'level increase. The actual determination of
K for comparison with the calculated value would be very helpful for span
setting. Once the span of the mobility control point is set, the sugar boiling
runs smoothly and repeatedly without any further attention. When the level
reaches La, PS, is actuated and energises SV4to close CV, and the pan is ready
for cutting or continuous tightening until the mobility reaches M, before
discharge.
he control system of a C-strike is basically the same as a Cs-system, except
for the use of balancing water for tightening instead of seeding, and the footing
preparation system is not necessary. The strike is ready to start growing as soon
as PSI turns on the light, when the footing level reaches point L,. The mobility
gradually rises from M, to M, in response to the level signal. L, actuates PS,
to block the output control signal through SV, which in turn shuts off the feed.
Because the pan continues evaporating, the mobility rises sharply from M,
to M,. M, actuates PS,, and initiates timer T, for the first automatic addition
of balancing water into the pan to reduce the consistency of the massecuite for
better exhaustion of sucrose from the mother-liquor. The drop in M, is deter-
CHIEN-JAN LU 1353
mined by the time duration set on the timer. If there is too much of a drop due
to the low water temperature or a sudden large vacuum drop, PS,, automatic-
ally turns off the timer a t point M, and stops water feed to prevent crystal
remelting. A second addition of water is carried out in the same way. I n TSC
practice, two drinks of water are sufficient. The amount of water to be intro-
duced should be determined individually for each pan. Full utilisation of water
is more effective when the drinks are distributed before the middle half of the
tightening stage as shown in Fig. 10.
The Cs-seeding control system can be successfully applied to the high
grade boiling R-strike, when the footing preparation is omitted. The control
system of the C-strike without the water system for tightening is workable for
the medium grade boiling -AB-strike. The only differences are the range and
slope of the set point.
low grade material. Factory tests have proved the reliability. One eighth of
the cycle time is saved in a C-strike and one fifth in a n AB-strike. The purity
drop of each cycle varies within 2 degrees in comparison to 6 degrees by manual
operation of C-strike. Conglomeration including twins drops down below 15%
with the extension of the water boiling period after seeding in order to equalize
crystal size and crystal distance in high grade boilings. The systems tested can
tolerate fluctuations in the exhaust steam pressure o f f 50 kPa about an average
of 147 kPa and fluctuations in vacuum pressure of f 3,3 kPa and feed density
of + 3 Bx without a sigdificant reduction in the product quality. Fluctuations
larger than above valued bhould be removed by separate control loops.
b
FIGURE 11. Crystallisation rate of high and low grade sugar boiling.
1
,
CHEIN-JAN LU 1355
REFERENCES
1. Ahari, D. and Genotelle, J. (1966). Automatische Regelung der Kristallisation in
Kockapparate, Zeitsh. Zuckering. 18(9) S 47 1.
2. Foster, D. H. and Wright, P. G. (1962). Control of crystallization in vacuum pan,
Proc ISSCT, 11 :940.
3. Genie, G. V. (1962). Theoretical consideration on sugar boiling Int Sug J, 64(8):232.
4. Honig, P. (1958). Principles of sugar technology Vol 11, Elsevier, Amsterdam pp 386,
373 and 260, Vol I p. 26.
5. Holven, A. L. (1942). Supersaturation in sugar boiling operation, Ind Eng Chem,
34(10):1234.
6. Joseph, A. (1969). Automation of low and high grade massecuite crystallization pro-
cesses. S Afr Sug J, 53(5) :350.
7. Lu, C. J. (1966). An analysis of sugar balance in sugar manufacturing process, Annual
Rep of TSES, p 180.
8. Nicol, W. N. (1969). The effect of superheating on BPE measurement, Int Sug J,
71 :315.
9. Thiele, Von H. and Langen, A. (1968). Zuckerkristallisation mit der Rheometer
Kockautomatik, Zeitsh. Zuckerin. 18(9):S 47 1.
10. Wright, P. G. (1966). Circulation movements in sugar pans. Proc QSSCT, 33 :179.
11. Zagrodzke, S. and Zaorska, H. (1965, 1968). Influence of the decolorization of sugar
juice and products on the crystallization rate in impure solutions. Int SugJ, 67 :300,337 and
70:229,268.
I RESUMEN
4esde hace ahos muchos sistemas de cocimiento con instrumentos han
sido I~ntroducidos.Sin embargo, la aplicacidn 6xitosa de estos m6todos es
todavia limitada debido a factores que no son del todo claros. A trav6s de
la medicidn del contenido de cristales, puede establecerse una relaci6n
matemgtica entre contenido de cristales, distancia entre cristales y tamario
de cristales. Durante el cocimiento a medida que aumenta el volumen de
masoco~ida,la distancia entre cristales disminuye en funcidn linear con el
crecimietto de 10s cristales, mientras que el contenido de cristales aumenta
en funcio,n de raiz cuadrada. Antes de empezar a alimentar la solucidn de
azOcar, $1) espacio de 10s cristales debe ser ajustado de acuerdo con el
tamaho dg\los cristales, si se desea hacer un buen cocimiento. Las rnieles
de baja prll;eza requieren mayor distancia decreciente para mantener una
sobresaturabj6n adecuada cuando disminuye la circulacidn debido al incre-
mento del vodumen de la masacocida.
Se pruetjqn experimentalmente y se comparan tres metodo instrumentales
convencionaleg. Control de movilidad que responde a dos variables, viscosidad
y contenido de cristales, tiene un mejor cuadro de crecimiento del medio y se
opera con m&or confiabilidad. Al comparar el contenido de cristales
actualmente medido con el contenido calculado por la ecuacidn matemiitca,
puede obtenerse una guia operativa bastante exacta.
Se presentan dos ejemplos decontrol de movilidad aplicados a cocimien-
tos de baja pureza. Con la meta de manten,er un medio de crecimiento dptimo
en base a la viscosidad y al contenido de cristales, e l sistema de control de
movilidad en el cual el 'reajuste del pu,nto de control se hace en relaci6n al
contenido de cristales es apropiado para,todas las etapas de cocimiento sea
el material alimentado de baja o alta pureza.