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Production of Colorless Liquid Sugar by Ultrafiltration Coupled With Ion Exchange PDF
Production of Colorless Liquid Sugar by Ultrafiltration Coupled With Ion Exchange PDF
Semarang, Indonesia
a r t i c l e i n f o a b s t r a c t
Article history: Liquid sugar is an alternative product to crystal sugar, which is currently being considered by
Received 26 June 2015 many sugar companies. However, production of colorless liquid sugar is still a big challenge.
Received in revised form 20 This work aimed to study the performance of ultrafiltration membrane and ion exchange
November 2015 (IE) both as single and integrated processes for decoloring cane sugar solution. The exper-
Accepted 2 December 2015 iments were performed by using 10, 20, 50, and 100 kDa commercial UF membranes. Two
Available online 13 December 2015 commercial resins were used in ion exchange experiments. The results of decoloring sugar
solution using UF membranes showed that the 20 kDa UF membrane made of polysulfone
Keywords: displays the best performance in term of flux and color removal. Integrating ion exchange
Sugar decolorization process into UF membrane improves the color reduction resulting colorless liquid sugar.
Fouling The UF–IE configuration shows a better performance than both the IE–UF and UF/IE alone
Ion exchange configurations. These results provide important information about technologies that should
Liquid sugar be used for liquid sugar production.
Ultrafiltration © 2015 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
Process configuration
∗
Corresponding author. Tel.: +62 247460058; fax: +62 247480675.
E-mail addresses: heru.susanto@undip.ac.id, susanto.heru@gmail.com (H. Susanto).
http://dx.doi.org/10.1016/j.fbp.2015.12.002
0960-3085/© 2015 The Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
12 food and bioproducts processing 9 8 ( 2 0 1 6 ) 11–20
membrane for sugar cane juice clarification either stand alone combination of both technologies. The process configuration
or combined with the coagulation process (Balakrishnan et al., of UF and IE for colorant removal to obtain colorless sugar
2001; Bhattacharya et al., 2001; Donovan et al., 2002; Fechter solution was investigated.
et al., 2004; Ghosh et al., 2000; Ghosh and Balakrishnan, 2003).
In general, UF membranes offer (i) increasing the transmission
of sucrose, (ii) improving the quality of sugar, (iii) increasing 2. Materials and methods
the yield of conventional process, and (iv) reducing the chem-
ical and energy used. However, most of previous publications 2.1. Materials
of application UF membranes are dedicated to production of
crystal sugar, where permeate of ultrafiltration membrane For identification of suitable membranes, commercial poly-
will further be processed by crystallization (e.g., Balakrishnan sulfone (PS) and polyethersulfone (PES) UF membranes with
et al., 2000a,b; Chen and Chou, 1993; Jacob and Jaffrin, 2000; different pore sizes (represented by MWCO, molecular weight
Mak, 1991). In this context, the color of sugar solution result- cut off) and one UF membrane made from fluoro polymer
ing from UF permeate is not requested to be at a low level. were used in this study. The membranes tested were GR81PP
Besides its function to form sugar crystal, crystallization pro- (10 kDa, polyethersulfone, called PES-10), GR61PP (20 kDa,
cess can also play as a decolorization process via excluding polysulfone, called PS-20), GR51PP (50 kDa, polysulfone, called
colorants from sugar crystals during crystal growth as well as PS-50), GR40PP (100 kDa, polysulfone, called PS-100), and
crystal washing after being separated from the liquor. By con- FS61PP (20 kDa, fluoro polymer, called FP-20). All membranes
trast, no crystallization process is used in production of liquid were supplied by Alfa Laval, Denmark. The membranes were
sugar. initially washed by soaking overnight in water to remove
To produce high quality of liquid sugar, we need technolo- impurities or additives left from the manufacturing process
gies that can eliminate soluble non-sugar macromolecular before use. Fresh membranes were used in all experiments.
and colorants. Removal of colorants from liquid sugar is very Brown sugar crystal was purchased from the local sugar com-
important because color is the most significant quality deter- pany in Indonesia. Sodium hydroxide and hydrochloric acid
minant. Colorants in sugar cane juice can originate from were purchased from Merck. Lewatit adsorber resins, i.e., S
native of sugarcane plant such as flavonoids and melanins 6368 (R1) and OC 1074 (R2), were used for ion exchange pro-
and those developed during cane juice processing such as cess. S 6368 (R1) is strongly basic macroporous anion exchange
melanoidins and caramels (Flood and Flood, 2006; Hamachi resin (type I) with beads of uniform size (monodisperse) based
et al., 2003). This colorization increases during processing as on polystyrene. OC 1074 (R2) is a strongly basic macroporous
a result of enzymatic reactions and heat induced procedures type I anion exchange resin based on polyacrylamide. It is
involved. Sugarcane juice contains 3–5% of soluble solids in bead-shaped and has a special bead size distribution. Dem-
the form of colorants, color precursors, etc. and an additional ineralized water from home-made RO-ion exchange system
0.85–1.45% of soluble solids in the form of organic non-sugars was used for all experiments.
such as protein, polysaccharides and waxes (Chen and Chou,
1999). Several techniques can be used for removing color from
2.2. Methods
the sugar solution including ion exchange (IE), activated car-
bon and UF. Among them, UF and ion exchange seem to be of
2.2.1. Ultrafiltration experiments
highest relevance from practical point of view.
Ultrafiltration experiments were performed by crossflow fil-
UF membrane has been proposed as an attractive tech-
tration using a self-home-made laboratory scale similar with
nology for color removal in production of crystal sugar and
our previous publication (Susanto and Widiasa, 2009). The
others (Decloux et al., 2000; Hamachi et al., 2003; Jacob and
set-up consisted of a feed tank, a pump, a pressure indica-
Jaffrin, 2000; Mak, 1991). However, this technology has low
tor connected to feed side and a flat-sheet membrane cell
efficiency for removing color originating from very small
made of stainless steel. The cell has a diameter of 10 cm with
macromolecules or minerals. The use of nanofiltration mem-
a 4 cm diameter membrane holder. A simplified diagram of
brane may be able to remove such small colorants but it can
the set-up is given in Fig. 1. In each experiment, a new circu-
also reduce sugar content. Ion exchange (IE) has been applied
lar membrane disk with the effective area of 0.00125 m2 was
in many food industries (Achaerandio et al., 2002; Lyndon,
used and was firstly compacted by filtering pure water for at
1996). In principle, this technology can be used for soften-
least 0.5 h at a pressure of 3 bars. In order to maintain con-
ing, demineralization and decolorization. Application of ion
stant feed concentration, the volume of feed was much larger
exchange for sugar cane juice decolorization was reported in
than the volume taken as sample for the analysis. In addition,
previous publications (Bento, 1990; Lin and Chen, 1991). How-
the retentate and permeate were returned back to the feed
ever, the use of IE technology is limited by its high operating
tank. During UF experiments, the flux profile over time was
cost due to resin regeneration. In addition, high amount of
gravimetrically monitored. All experiments were conducted
wastewater will be resulted from regeneration process.
at room temperature (28 ± 2 ◦ C) and at a constant transmem-
In summary, UF and IE have been proposed for decolor-
brane pressure (300 kPa for PES-10 and 100 kPa for PS-20, PS-50,
ing cane sugar solution or sugarcane juice. However, most of
PS-100 and FS-20). The transmembrane pressure drop (the dif-
previous studies on decolorization of sugar solution were per-
ference between feed pressure and retentate pressure) was
formed using single process, i.e. either UF or IE alone. The
less than 0.1 bar. The sugar content, color, and absorbance of
objective of the current study was to examine the performance
feed and permeate were analyzed. The apparent color rejec-
of ultrafiltration membranes and ion exchange for the decol-
tion was calculated using Eq. (1).
orization of sugar solution. Measurements of the permeate
flux and other key parameters of the separation were also
performed to determine the viability of the UF membrane Cd
R=1− (1)
process. The important investigation was the performance of Cu
food and bioproducts processing 9 8 ( 2 0 1 6 ) 11–20 13
Fig. 1 – The schematic diagram of the cross-flow filtration set-up used in this study.
2.2.4. Analyses
The sugar content was measured as brix using digital refrac-
Fig. 2 – Schematic diagram of the ion exchange tometer (ATC-1E, ATAGO). The color of the juice was measured
experimental set-up. according to GS1–7 method, where the sugar solution was
adjusted to pH 7 by 0.1 N HCl or 0.1 N NaOH and filtered
through a 0.45 m filter (ICUMSA, 1994). Thereafter, the
where, Cd (IU) and Cu (IU) are color intensity of downstream
absorbance of sugar solution was measure at wavelength
(permeate) and upstream (feed) respectively.
420 nm using a spectrophotometer (Shimadzu UVmini 1240
UV). Beside the pH of sugar solution, the viscosity of sugar
2.2.2. Ion exchange experiments
solution was measured by using viscometer DV-II + Pro (Brook-
Ion exchange (IE) experiments included batch and continuous
field, USA). The color intensity was calculated using Eq. (2).
experiments. The batch experiment was conducted by mixing
a volume of sugar solution and an amount of resin in a closed
glass container. The mixture was then stirred at ∼300 rpm at 108 × As
a certain time. First, the adsorption capacity (in terms of color Color(IU) = (2)
b × RDS ×
reduction) of three different resins from Lewatit, namely S
6368 (called R1), OC 1074 (called R2) and mixed bead resins
comprising of S 6368 and OC 1074 with the ratio of 1:1 (called where, As is the absorbance of the sugar solution at 420 nm,
R3) was compared. After contacting the resin with sugar solu- b is the cell length of the absorbing path (cm), RDS is the
tion for 24 h, the solution was filtered using a filter paper and refractometric dry substance (the sugar content determined
then analyzed. Second, adsorption kinetics were investigated by measuring the refractive index of the solution) and is the
by measuring adsorption capacity at different times using the density of the solution (kg/m3 ).
best resin obtained from the adsorption capacity experiments. The membrane surface chemistry was analyzed by using
Third, the maximum capacity was determined by conducting the instrument IR Prestige-21 (Shimadzu, Japan). A total of 32
experiments using various color concentrations at the opti- scans were performed at a resolution of 4 cm−1 and tempera-
mum time obtained from the kinetic experiment. ture of 21 ± 1 ◦ C over the wavelength range of 500–4000 cm−1 .
The continuous experiment was performed using equip- A software program, IR solution 1.5, was used to record the
ment presented in Fig. 2. The resin was placed in the column sample spectra versus the corresponding background spectra.
with inside diameter of 25 mm. The height of resin bed was The top surface morphology of the membranes was visual-
25 cm. The adsorption experiment was carried out at room ized by using a Supra 35 VP field emission scanning electron
temperature (28 ± 2 ◦ C). A sugar solution from the feed con- microscope (FESEM) with applied voltage was 10 kV. The outer
tainer was pumped to the IE column at a constant volumetric surface of the sample was coated with gold/palladium and
feed flow rate. sputtered for 1 min before analysis.
14 food and bioproducts processing 9 8 ( 2 0 1 6 ) 11–20
0
1993; Saha et al., 2007). These components lead to fouling
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 by accessing both membrane pore and membrane surface.
Filtration time (min) If the pore size is larger than the solute(s) size, the possi-
bility of solute(s) to access membrane pores will be larger
Fig. 3 – Normalized flux profile during ultrafiltration of
leading to higher pore narrowing than pore blocking. If the
sugar solution (15 g/L.) using various UF membranes.
solute(s) size is larger than the pore size, gel/cake layer foul-
Fluxes after stopping and restarting the filtration relative to
ing will probably be formed. Readers, who are interested in
initial water flux are also included.
developing models that describe flux decline, are directed to
the references (Bhattacharya et al., 2001; Mondal et al., 2013;
3. Results and discussion Verma and Sarkar, 2015). Comparing the membranes having
the same poresize but different material (PS-20 and FP-20)
3.1. Effect of membrane pore size on flux and color showed that those membranes have significantly different ini-
reduction tial water flux, even though they had same MWCO determined
by the company but their pore sizes were practically differ-
Various UF membranes were examined to filter sugar solution ent. This is common in the membrane field, and has already
(15 g/L). The performance was expressed in term of flux and been explained in previous publications (Susanto and Ulbricht,
color rejection. Fig. 3 shows the flux as a function of filtra- 2005; Susanto et al., 2007). The FP-20 showed a slightly higher
tion time performed with constant transmembrane pressure flux ratio than PS-20 (0.65 vs. 0.57) but it had significant lower
(300 kPa for PES-10 and 100 kPa for PS-20, PS-50, PS-100 and FS- color rejection (68.0 vs. 85.7%). These results suggest that
20). Table 1 shows the initial water permeability of membranes membrane material has significant influence on the results
used, color and sugar content of feed and permeate and color of both membrane characterization and fouling behavior.
rejection. Overall, study of the effect of pore size on flux behavior and
As shown in Fig. 3, all UF membranes displayed a flux color rejection demonstrated that the separation mechanism
decline at the early stage of filtration and after about 30 min of colorants is determined not only by sieving mechanism but
they reached a condition approaching steady state flux. The also membrane-solute(s) interactions (membrane material).
flux after stopping the filtration for about 5 min showed a These results are different from the results of the previously
higher value compared to the flux before stopping the fil- reported study by Hamachi et al. (2003). They stated that the
tration, but still much lower compared to the initial water color removal of sugar solution by using UF membrane is
flux (Jo). The increase in flux after stopping the filtration was determined by pore size exclusion. Evaluation of the mem-
within the range 5–10% depending on the pore size. This phe- brane performance, which was based on both the flux ratio
nomenon indicates that concentration polarization is taken and the color reduction, suggests that the PS-20 should be
place and contributes to the flux decline. However, irreversible chosen for the further experiments.
flux decline or fouling was the dominant reason for these flux
decreases as noticed by the values of J/Jo after stopping the
filtration are still within the range 30–60%. 3.2. Effect of feed characteristics on flux and color
It was clearly observed that the extent of flux decline was reduction
influenced by the membrane pore size. For the same mem-
brane material (PS), it was seen that the pore size influences In this part, the effects of feed concentration and pH on flux
the resulting flux behavior. The PS-100 showed the lowest flux and color reduction were investigated using PS-20 kDa mem-
ratio indicating the highest fouling occurred in this mem- brane. The results are presented in Figs. 4 and 5. The pH of
brane. The PS-50 and PS-20 showed comparable flux ratios 15 g/L sugar solution (without adjustment) was 5.5. As was
but their color rejection was significantly different, i.e., 74.4% also found in the previous experiments, a rapid flux decline
for PS-50 and 85.6% for PS-20 (Table 1). The PES-10 showed followed by a steady flux was observed for all feed concentra-
a lower flux ratio compared to both PS-50 and PS-20 mem- tions. The increase in feed concentration decreased the flux
branes. In term of nominal product permeance, the PES-10, ratio indicating higher flux decline. It was clearly observed
PS-20, PS-50, PS-100 and FP-20 membranes showed 2.8, 25.5, that concentration polarization has contributed to the flux
36.5, 33.2, and 48.2 L m− 2 h− 1 bar−1 , respectively. FP-20 had the decline as indicated by the increase in flux ratio measured
highest product permeance. Thus, a higher MWCO membrane after stopping the filtration. Furthermore, it was seen that the
did not automatically produce higher permeate flux. Simi- higher feed cocentration the higher increase in flux ratio mea-
lar phenomenon was reported by other authors (e.g., Chhaya sured after stopping the filtration (the increases in flux ratio
et al., 2012; Fukumoto et al., 1998; Susanto and Ulbricht, 2008). are 3.9%, 7.8%, and 13.7% for the feed concentration of 10, 15,
Table 1 shows also brix decrease in the permeate after ultrafil- and 20 g/L, respectively). This suggests that the concentration
tration. It is believed that this decrease in brix is mostly caused polarization is increased by increasing feed concentration.
food and bioproducts processing 9 8 ( 2 0 1 6 ) 11–20 15
Table 1 – The initial water permeance of membranes used and the resulting color rejection.
No. Membrane Pure water permeancea (L m2 h−1 bar−1 ) Feed Permeate Color rejection (%)
a
Average value ± standard deviation obtained from at least three measurements.
1.1 1.1
0.9 0.9
0.8 0.8
0.7 0.7
0.6 0.6
J / Jo
J / Jo
0.5 0.5
0.4 0.4
Relative flux after
0.3 stopping and restarting 0.3 Relative flux after
the filtration stopping and restarting
0.2 0.2 the filtration
0.1 0.1
0 0
0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 0 10 20 30 40 50 60 70 80 90 100 110 120 130 140
Fig. 4 – Normalized flux profile during ultrafiltration of Fig. 5 – Normalized flux profile during ultrafiltration of
various concentrations of sugar solution using PS-20 kDa various pH of sugar solution using PS-20 kDa membrane
membrane. Fluxes after stopping and restarting the (sugar concentration 15 g/L). Fluxes after stopping and
filtration relative to initial water flux are also included. restarting the filtration relative to initial water flux are also
included.
In addition to concentration polarization the effect of feed
concentration on irreversible flux decline (fouling) was also
very clear as indicated by the values of J/Jo after stopping the layer can promote the diffusion of solid already deposited on
filtration are still within the range 30–40%. An increase in feed the membrane surface and/or membrane pores.
concentration increased concentration polarization meaning Fig. 5 shows that the flux at acidic condition (pH = 4)
that more suspended or dissolved substances on the mem- decreased more significantly compared to the flux at both neu-
brane surface. This phenomenon facilitates the formation of tral (pH = 7) and alkaline (pH = 9) conditions indicating more
fouling by altering interaction between membrane and solutes significant fouling was taken place at the acidic condition.
(= suspended or dissolved substances) as well as penetrating This observation is analogous to the results in previous pub-
of solutes into membrane pores. Further, the increase in feed lications (Balakrishnan et al., 2000a,b; Kishihara et al., 1989).
concentration increased the feed viscosity (Table 2) that will The higher flux at alkaline condition can be due to the change
add a resistance of feed flow through membrane pores. in the conformation of the protein impurities. In addition,
Beside membrane pore size, the color reduction is influ- by decreasing the pH of the solution, protonation will occur
enced by feed concentration. Increases in feed concentration and consequently, the electrostatic repulsion between the feed
were found to increase color rejection. However, further component and the membrane surface is reduced. The pH
increase in feed concentration would not increase color rejec- of the feed solution also influences color rejection. The color
tion anymore. As feed concentration increases the possibility rejection were 72.1%, 87.2%, and 80.3% for the feed pH solution
of solids to be deposited on the membrane surface and/or of 4, 7, and 9, respectively; whereas the permeate concentra-
membrane pores (via solute adsorption and pore blocking) tions were 8.2, 8.4, and 8.0 brix for the pH feed solution of
increases resulting in higher color rejection. At feed concen- 4, 7, and 9, respectively. These results indicate that the feed
tration is high enough, the accumulated solids rejected by the solution comprises of many components, which have differ-
membrane increases and is able to form a gel layer. This gel ent charge. The highest flux rejection was observed at neutral
Table 2 – The feed and permeate characteristics, flux ratio and color rejection.
No. Csugar (g/L) Feed J/Jo Permeate Color rejection (%)
1.2
3.4. Decolorization using ion exchange resins
Fresh membrane
Fouled membrane
1 First of all, three different resins namely R1 (S 6368), R2 (OC
1074) and R3 (mixture of S 6368 and OC 1074, 1:1) were com-
0.8 pared for color removal in batch experiment. The results are
Absorbance
Fig. 7 – Visualization of membrane surface morphology by using SEM: (A) PES-10 fresh membrane, (B) PS-20 fresh
membrane, (C) PS-100 fresh membrane, (D) FP-20 fresh membrane, (E) PS-20 membrane fouled by 15 g/L sugar solution
without pH adjustment, (F) PS-20 membrane fouled by 15 g/L sugar solution at pH 4, (G) PS-20 membrane fouled by 15 g/L
sugar solution at pH 7 and (H) PS-20 membrane fouled by 15 g/L sugar solution at pH 9.
a
Resin to sugar solution ratio.
b
15 g/L sugar solution.
c
Obtained from the permeate of PS-20 UF membrane.
increasing long adsorption time supports that the diffusion performed using UF permeate as feed. The ratio of resin to
into the resin pore was taken place. sugar solution was varied (by varying the amount of resin) and
color reduction was determined after 30 h of contact. As can
3.4.2. Equilibrium experiment be seen in Fig. 9, the increase in resin dose within the range
The amount of resin is critical for the application of ion 0–25 g/L significantly increased color reduction, presumably
exchange at industrial scale. In order to know the optimum by increasing the surface area. Further increases will cause
resin required, adsorption equilibrium experiments were some resins are not in maximum loading (has not reached
18 food and bioproducts processing 9 8 ( 2 0 1 6 ) 11–20
90 90
80 80
70 70
Color reduction (%)
50 50
40 40
30 30
20 20
10 10
0 0
0 10 20 30 40 50 60 70 80 0.00 0.25 0.50 0.75 1.00 1.25 1.50 1.75 2.00 2.25
Time (h) Feed flow rate (L/h)
Fig. 8 – The effect of contact time on color reduction. The Fig. 10 – The effect of feed flow rate on color reduction.
experiment used the UF permeate as feed and R3 resin
(resin dose was 25 g/L). R3 is mixed bead resins comprising
intensity ∼230.65 IU) was 25 g/L. This means that 1 L of sugar
of S 6368 and OC 1074 with the ratio of 1/1.
solution obtained from UF permeate (20 kDa), needs 25 g of
90 resin resulting in color reduction is ∼80%. This optimum dose
is higher than the result obtained by Achaerandio et al. (2002)
80
who reported that the optimum dose of resin for white vinegar
70 decolorization was 20 g/L.
Color reduction (%)
60
(1–5): Feed = Sugar solution (15 g/L), IE flow rate = 0.3 L/h, color removal based on final product and initial feed; (6): Feed = real sugar cane juice,
IE flow rate = 0.3 L/h, 0.45 mm MF membrane was used as pre-treatment before UF was applied.
a
Sugar cane juice.
b
Permeate of 0.45 MF membrane.
c
Permeate of UF membrane.
d
Product of IE using R3.
e
Color reduction based on sugar cane juice.
f
Color removal based on permeate of MF membrane.
food and bioproducts processing 9 8 ( 2 0 1 6 ) 11–20 19
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