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Despite the substantial improvement of beet quality which Trotz der deutlichen Verbesserung der Rübenqualität ver-
has been achieved, still a relatively high content of nonsug- bleibt immer noch ein relativ hoher Gehalt an Nichtzucker-
ars remains in the raw juice extracted from sugar beet. New stoffen nach der Extraktion im Rohsaft. Neue analytische
analytical methods and instrumentation have helped to bet- Methoden und Instrumente helfen, die in den einzelnen
ter understand the various physical and chemical reactions Phasen der Saftreinigung stattfindenden physikalischen
taking place during the different steps of juice purification und chemischen Reaktionen besser zu verstehen und zu
and so how they can be affected. beeinflussen.
Some examples of developments over the past 20 years by Während der letzten 20 Jahre hat die Abteilung Forschung
the R&D departments of the Südzucker Group, related to und Entwicklung der Südzucker verschiedene Verfahren
the optimization of the juice purification system, are illus- zur Optimierung der Saftreinigung entwickelt: Rohsaft-
trated: raw juice viscosimetry, raw juice pre-alkalization, Viskosimetrie, Rohsaftvorkalkung, Bestimmung des opti-
optimal pH value of flocculation in the prelimer, optimal malen pH-Wertes des Flockungspunktes in der Vorkalkung,
course of pH value in the prelimer, optimal temperature/ optimaler Verlauf des pH-Wertes in der Vorkalkung, opti-
retention time in the prelimer and main limer, optimal pH male Temperatur/Verweilzeit in Vor- und Hauptkalkung,
value of 1st carbonatation, milk of lime optimization system optimaler pH-Wert der ersten Carbonatation, Kalkmilch-
(LIMOS) to reduce limestone consumption, lime salts ana- optimierung zur Reduzierung des Kalksteinverbrauchs
lyzer (LISA), optimization of decalcification, SZ/RT-juice (LIMOS), Kalksalzanalyse (LISA), Optimierung der Ent-
purification system with separation of the colloid fraction kalkung, SZ/RT-Saftreinigung (Abtrennung der Kolloid-
after the prelimer. fraktion nach der Vorkalkung).
Key words: extraction, raw juice, nonsugars, juice purification Schlagwörter: Extraktion, Rohsaft, Nichtzuckerstoffe, Saft-
reinigung
1 Introduction remains in the raw beet juice. The presence of these nonsugars
requires a rather complicated and costly purification process
Improvement of beet quality, increased requirements of sugar in order to enable the production of white sugar of the right
quality (such as reduction of ash and turbidity of sugar) and quality, as well as to limit any unnecessary sugar loss to molas-
the demand for reduction of both energy and processing aids’ ses. The task of juice purification is – above all – to increase
(e.g. limestone) consumption have been important challenges the juice purity by neutralization, coagulation, degradation
over the past 20 years, asking for further optimization of juice and separation of particular dissolved and colloidal nonsugar
purification in beet sugar manufacture. Numerous investiga- substances in raw juice. After juice purification a thin juice is
tions have been performed to optimize the different process aimed with higher purity, low color and lime salts content, and
steps of juice purification. More recently, the processing of good thermostability. New analytical methods and instrumen-
deteriorated beet came into focus due to prolonged beet pro- tation have helped to better understand the various physical
cessing campaigns as a result of the reform of the EU Sugar and chemical reactions taking place during the different steps
Regime. of juice purification and so how they can be affected.
Juice purification is an important step in sugar technology. Classical juice purification uses milk of lime in the pre-liming
It has a significant impact on sugar quality and sugar yield. and main liming and subsequently CO2 in the 1st carbonata-
Despite the substantial improvement of beet quality in recent tion and 2nd carbonatation in order to achieve the above-men-
years, still a relatively high amount of nonsugar substances tioned chemical and physical reactions. The precipitated and
insoluble nonsugars are removed by filtration and/or decanta-
tion.
Some examples of developments over the past 20 years by the
* Paper presented at the XXIst Symposium organized by the Andrew VanHook Associa- R&D department of the Südzucker Group related to the opti-
tion in Reims/France, 27 March 2014.
mization of the juice purification system will be illustrated:
Table 1: Specifications of the on-line rheometer Physica Rheoswing RSD 1-1 The viscosity signals could be interpreted based on an evalu-
Parameter Technical data ation chart, which was derived from the determined viscosity
Input range medium density in g/cm3 0.400 – 3.999 and laboratory data such as dry matter and sugar content of
Pressure range in bar 0 – 150 raw juice. The factory can use the evaluation chart as an early
Frequency range in Hz approx. 8500 (this case 8550)
warning system, indicating a change of raw juice quality and
Maximum ambient temperature in °C 110
then can take the necessary actions in the juice purification.
Measuring range of the kinematic viscosity
in m2 · s–1 0.1 – 3 · 10–6
Measuring range of the dynamic viscosity
in mPa · s 0.3 – 100 3 Raw juice pre-alkalization
Measured value acquisition in min–1 max. 52
The aims of the raw juice pre-alkalization are:
– Stabilization of raw juice before the raw juice heat exchanger;
Figure 4 shows the pilot system for raw juice viscosimetry. The – Reducing the microbiological activity within the raw juice
viscosity could be measured after desanding and depulping heat exchanger before the prelimer;
of the raw juice with the help of the viscosity measurement
system Rheoswing RSD1-1.
The raw juice feeds tangentially in the
separation tank for separating suspended
big pulp particles and sand. The pre-
cleaned raw juice is pumped to the mea-
surement cell; the viscosimeter is located
in the head of the measurement cell. The
dynamic viscosity of raw juice is mea-
sured every 15 seconds and the measured
data are registered in the data manage-
ment protocol of the factory. Warm water
is used for cleaning of the system.
After optimizing the flow rate, the sepa-
ration tank for big pulp particles and
sand and the CIP (cleaning in place) sys-
tem with warm water a stable viscosity
signal was obtained (Fig. 5). Fig. 5: Viscosity signal of technical raw juice during 24 h (Shahidizenouz, 2008)
Fig. 4: Pilot system for on-line raw juice viscosimetry (Ajdari Rad et al., 2008 a)
3.2 Materials and methods juice in a 10 s interval. Table 2 shows the process conditions
during the juice purification experiments.
For the realization and evaluation of the rheological experi- Figure 10 shows the typical viscosity profile of the juice during
ments in the field of juice purification a discontinuous juice preliming.
purification system on a laboratory scale has been used The investigations of analyzing the rheological changes of
(Fig. 9). The juice purification system consists of a jacketed raw juice upon the addition of milk of lime helped to bet-
(for heating) 3 L reaction vessel (1). The raw juice is mixed ter understand the reactions during preliming. The obtained
in the reaction vessel by means of a variable-speed stirrer characteristic curve is unique and provides important infor-
throughout the juice purification process. For temperature mation concerning the structural changes of colloids and sus-
control of the juice during juice purification two thermostats pended solids during the preliming process. This investiga-
with circulators are used (2 and 3). The carbon dioxide (4) is tion shows that the physical reactions in the preliming have a
passed through a controllable valve to the gas distributor dur- significant influence on the rheological properties of the raw
ing the 1st and 2nd carbonatation. The gas distributor consists
of a circular perforated (holes diameter about 0.1 cm) copper
loop. Limed juice was continuously collected during the tests Table 2: Process conditions in the juice purification experiments
by means of a centrifugal pump (supplier company EHEIM, Process step Time Tempera- Comments
2400 min–1, flow rate of 10 L/min) via the drain valve of the in min ture in °C
reaction vessel and recirculated through a measurement flow Preliming 20 55 End pH value = 11.40
cell (5) in the reaction vessel. Main liming 20 85 Alkalinity = 1.1 g CaO/100 mL
The on-line rheometer (RSD 1-1) located in the measurement 1st carbonatation 15 85 End pH value = 11.20
cell (No. 6 at Fig. 9) determined the viscosity of the inflowing 2nd carbonatation 12 88 End pH value = 9.25
Fig. 9: Discontinuous laboratory juice purification system with rheometer 1 Reaction vessel; 2 and 3 Thermostat with circulator; 4 Carbon dioxide; 5 Flow
cell; 6 On-line rheometer (RSD 1-1); 7 Evaluation device of rheometer; 8 Monitor
Fig. 10: Course of the juice viscosity along the prelimer (Kraus, 1998; Ajdari Rad and Senge, 2002)
juice because of structure-forming mechanisms. The obtained juice alkalization. A comparison between rheological deter-
viscosity curves can be divided into 6 sections: mination and the usual photometry determination of the
– Functional stability of the juice (no change in viscosity); optimal flocculation point in the prelimer gives a very good
– Approaching the isoelectric point of raw juice colloids; correlation.
– Dehydration of the colloids with a reduction in their particle
size and viscosity;
– Flocculation and precipitation of the colloids with an 5 Optimal course of pH value in the prelimer
increase of particle size and viscosity;
– Gradual continuation of the structure formation; The practical application of the results of rheological measure-
– End of the structure formation with a more or less constant ments during the preliming is the definition of the optimal
viscosity. pH value course in a so-called progressive preliming. Figure
12 shows the recommended pH value course of preliming as
based on maximum structure formation and thus optimal
4 Optimal pH value of flocculation in the prelimer flocculation and precipitation of the colloidal components.
According to the rheological behaviour of the juice four differ-
During preliming – due to the addition of milk of lime – the ent pH ranges can be distinguished:
transition of a colloidal solution of high molecular mass com- – pH ≤ 8.5: pH range in which the charge of the colloid sub-
ponents in the raw juice into a structure of coarse particles stances changes;
takes place. The basis of the rheological measurement prin- – 8.5 ≤ pH ≤ 10.0: pH range where the dehydration of proteins
ciple is the so-called hydraulic diameter of a molecule or a begins, a necessary preliminary reaction in order to enable
particulate structure. The viscosity change in the preliming optimal flocculation at the further increasing pH value;
can therefore be used as a measure of the structure formation – 10.0 ≤ pH ≤ 11.0: pH-range in which these preliminary reac-
from colloidal components. tions continue resulting in the eventual floc formation;
The viscosity of the limed juice varies during addition of lime – 11.0 ≤ pH ≤ 11.4: the pH value is reached for the optimum
to the raw juice in the prelimer as a result two factors: flocculation, allowing the maturation and stabilization of
– Influence of the added lime on the dry substance content the colloidal floc materials before entering the high-alkaline
(density) and so on the viscosity of the juice. pH in the main liming.
– The particle size increase because of the structure forma- Figure 12 is an example of the optimal pH value profile in a
tion from the colloidal components causes a change of the Brieghel-Müller prelimer with seven compartments at a tem-
viscosity of the limed juice (Wittstock, 1953; Grabka, 1982). perature of 55 °C and a retention time of 28 min.
The change of viscosity depends on pH value, temperature of
preliming, the buffer capacity of the raw juice and the type and
concentration of the high molecular mass components in the 6 Optimal temperature/retention time in the
raw juice. For the rheological determination of the optimum prelimer
flocculation point of preliming the milk of lime is added in
equal quantities per unit of time to the raw juice (for example The precipitation and coagulation of pectins and proteins
1 mL/min for 2500 mL raw juice). Figure 11 shows an example requires a certain temperature-dependent retention time
of the rheological determination of the optimum flocculation (Teschner, 1984; Kraus et al., 1997; Madsen, 2000).
point = the pH end-point for preliming. A temperature increase in preliming at constant raw juice quality
This is based on the rate at which the viscosity of the raw juice and a similar alkalinity/pH value profile leads to an increased
in preliming changes over time. The rate of viscosity change rate of the precipitation reactions and consequently to a decrease
represents the structure formation rate as it is affected by raw in the required retention time for preliming. The temperature-
retention time correlation in the preliming has been studied by
several authors on the basis of various analysis methods.
Fig. 11: Optimal flocculation point in the preliming (Ajdari Rad and Fig. 12: Optimum pH value management of the preliming at a preliming
Senge, 2002) temperature of 55 °C (Ajdari Rad and Senge, 2002)
Fig. 13: Temperature-retention time correlation of preliming with regard This new temperature-residence time correlation on the basis
to pectin precipitation (Kraus et al., 1997) of the rheological measurement method provides a precise
adjustment possibility of the preliming in sugar production
and has been successfully tested during several campaigns in
Figure 13 shows the optimal combinations of temperature different factories within the Südzucker Group.
and retention time in the preliming with regard to a maximum
removal of pectin by precipitation (Kraus et al,. 1997).
Figure 14 similarly shows the optimal combinations of tem- 7 Optimal pH value of 1st carbonatation
perature and retention time in preliming with regard to the
structural change of all suspended solids and colloidal matter The rheological determination of the optimum pH end-point
in the juice along the prelimer, as is determined by viscosim- of the 1st carbonatation (i.e. the viscosity profile of the 1st
etry. carbonatation) has been carried out with the help of a con-
tinuous on-line viscosity measurement device with a high
resolution (Physica Rheoswing RSD 1-1). The change in juice
viscosity during a batch-wise 1st carbonatation of main limed
Table 3: Temperature-retention time-correlation in the prelimer juice was recorded against the decreasing juice pH value. Fig-
Optimal retention time in the prelimer ure 15 shows the comparison of the changes in viscosity and
Temperature at Teschner (1984) Kraus et al. Ajdari Rad and pH value in the course of the 1st carbonatation.
prelimer (1997) Senge (2002)
During 1st carbonatation a reduction of viscosity of the juice
Protein Pectin Rheology
35 23.0 58.0 45.7
is observed because of CaCO3 formation and the adsorption
40 20.0 52.5 41.3 of colloidal matter on the surface of the CaCO3 crystals. The
55 15.0 36.0 28.1 optimum pH value of the 1st carbonatation is approx. 11.2.
70 7.0 19.5 14.9 Further introduction of CO2 would cause an unwanted fur-
ther pH value decrease at which calcium
carbonate starts to redissolve. In addi-
tion, colloidal matter will desorb from
the surface of the CaCO3 crystals to the
liquid phase, which then results in an
increased juice viscosity. From the mini-
mum value in the viscosity curve the
optimum pH end-point of the 1st carbo-
natation can be readily derived.
The rheological determination of the
optimum pH value of 1st carbonatation
is an alternative way to determine the
optimum pH end-point of the 1st carbo-
natation. Both the rheological determi-
nation and the generally applied photo-
metric determination of the optimum
pH value in the 1st carbonatation agree
very well. The rheological method can be
considered as an alternative direct (in/
on-line) method with higher accuracy
Fig. 14: Temperature-retention time correlation of preliming with regard to colloid precipitation and requiring less effort than the photo-
and structure formation (Ajdari Rad and Senge, 2002) metric method.
Fig. 16: Principle of SZ/RT-juice purification procedure with separating the colloids (Deneus et al., 2008)
10 Conclusions
Author’s addresses: Dr. Mohsen Ajdari Rad, Südzucker AG Mannheim/Ochsenfurt, Central Department Research, Development
and Technological Services (CRDS), Wormser Str. 11, 67283 Obrigheim, Germany; Dr. Azar Ajdari Rad, Südzucker AG Mannheim/
Ochsenfurt, GBZS, Marktbreiter Straße 74, 97199 Ochsenfurt, Germany; Gilles Schrevel, Raffinerie Tirlemontoise, Avenue de Ter-
vueren 182, 1150 Bruxelles, Belgium; e-mail: mohsen.ajdarirad@suedzucker.de