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Article history: Osmotic distillation (OD) or osmotic evaporation (OE) is a promising membrane process generally applied
Received 7 August 2008 to concentrate solutions under isothermal conditions. In this work, this process was applied to concentrate
Received in revised form 19 December 2008 commercial noni juice (Morinda citrifolia). Several nutraceutical properties have been reported for noni-
Accepted 27 December 2008
derived products, mainly associated to the phenolic content of the fruit.
Available online 4 January 2009
The analyzed system is an osmotic distillation system where the solutions are circulated through a
hollow fiber membrane contactor operating in transient configuration with circulation rates between
Keywords:
0.1 and 1.0 L min−1 and concentrated solutions of CaCl2 were used as extraction brine. At isothermal
Osmotic distillation
Noni juice
conditions (30 ◦ C), transmembrane vapor water flux was experimentally determined from 0.090 up to
Concentration 0.413 kg h−1 m−2 . Noni juice was concentrated from 8 to 32 ◦ Brix after 60 min of treatment. The content
Mass transfer of phenolic compounds was preserved after this processing.
Modeling Simulation algorithms based on phenomenological equations of heat and mass transfer were developed
considering a resistances-in-series model to predict the performance of the process from theoretical infor-
mation. The values of transmembrane water flux obtained by simulations showed deviations between
2.35 and 16.19% with the experimental ones for the operating conditions applied in this work.
© 2008 Elsevier B.V. All rights reserved.
0376-7388/$ – see front matter © 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.memsci.2008.12.053
206 H. Valdés et al. / Journal of Membrane Science 330 (2009) 205–213
Noni is the Hawaiian name for the fruit of M. citrifolia. This plant
is native from South East Asia to Australia and it is cultivated in Poly-
nesia, India, the Caribbean and Northern South America [17,18]. The
use of M. citrifolia is steadily growing and its products are commer-
Fig. 1. Outline of the transport phenomena with the concentration and temperature cially available in health stores and the Internet. The commercial
profiles through the membrane in the osmotic distillation process.
interest in noni has tremendously grown in the last few years, this
growth reflected in the number of patents registered: in the USA
Table 1
alone there have been 19 patents registered with the US Patent and
Composition of the Tahitian Noni Juice® (89% Noni; 11% Grape and Cranberry) [23].
Trademark Office since 1976 [19]. Several publications have shown
Property European Commission 2002 that noni can be used to treat diseases [20–22]. The use of con-
Value Units centrates of this juice, in liquid and pill form has become massive
due to the medicinal properties attributed to noni, such as being
pH 3.4–3.6
Dry matter 10.0–11.0 % anti-microbial, anti-carcinogenic, analgesic and anti-inflammatory.
Total soluble solids 8.0 ◦
Brix These properties are attributed to the main nutrients in noni rep-
Proteins 0.2–0.5 % resented by phenolic compounds [22].
Lipids 0.1–0.2 %
About 160 phytochemical compounds have been identified in
Glucose 3.0–4.0 g/100 g
Fructose 3.0–4.0 g/100 g
the Noni plant the majority of the micro-nutrients are phenolic
Potassium 30–150 mg/100 g compounds, organic acids and alkaloids [20]. The main groups
Sodium 15–40 mg/100 g of nutrients found in noni are phenolic compounds from the
Magnesium 3.0–12.0 mg/100 g group of iridoids, cumarins, terpenes, flavonoids and quinones. The
Calcium 20–25 mg/100 g
most important reported phenolic compounds are anthraquinones
Vitamin C 3.0–25 mg/100 g
(damnacanthal, morindone, morindin, and others), aucubin, aspe-
ruloside and scopoletin. The principal organic acids are caproic,
files. The temperature profile can be explained by a temperature caprylic, while the main reported alkaloid is xeronine [23]. The fruit
polarization phenomenon, which involves a latent heat transfer contains 90% water and the main components of the dried solid
through the membrane. This latent heat transfer decreases the tem- matter are fibers and proteins. The protein content of the fruit is
perature at the evaporation interface and increases the temperature 11.3% of the dried matter from the juice and the main amino acids
at the condensation interface. are aspartic acid, glutamic acid and isoleucine [21].
The interfaces formed by the liquid phases and the retained gas This study used “Tahitian Noni Juice”TM even though its com-
in the pores are considered in thermodynamic equilibrium. Thus, position does not correspond to the pure juice; the European Food
taking into account the volatile condition of the components to Commission established its chemical composition in 2002 [24]. The
Fig. 2. Experimental setup with a Celgard Liquicel minimodule used in this work.
H. Valdés et al. / Journal of Membrane Science 330 (2009) 205–213 207
Table 2 be treated and the extraction solution. Each variable was evaluated
Characteristics of hollow fiber contactor modules used in this work.
in two levels taking into consideration central points.
Property Module 1 Module 2 The operation conditions for each one of the modules are
Type Minimodule Minimodule
summed up on Table 3.
Liquicel® 1 × 5.5 Liquicel® 1.7 × 5.5 The experimental runs of concentration of noni juice were done
Membrane material Polypropylene Polypropylene in Module 2 of bigger dimensions than the Module 1, applying opti-
Number of fibers 2300 7400 mum operative conditions and where the greater evaporation flux
Pore diameter (m) 0.3 0.3
was observed (Ffeed = Fbrine = 1.0 L min−1 , Cbrine = 6.0 mol kg−1 ). The
Porosity (%) 40 40
Tortuosity 3.92 3.92 noni juice treated in the concentration experiments was previously
ID of the fiber (m) 2.2 × 10−4 2.2 × 10−4 filtered using borosilicate microfiber filters MFS GC50 of 47 mm
OD of the fiber (m) 3.0 × 10−4 3.0 × 10−4 with a 99.9% efficiency to remove particles with a size of 0.3 m.
Length of the fiber (m) 0.12 0.12
In addition to the rates of evaporated volume, the concentration
ID of the Shell (m) 0.025 0.043
Contact surface area (m2 ) 0.18 0.58
of phenolic compounds was determined in function of the time
during the treatment. The phenolic content in the noni juice would
not have to be modified by this type of processing. However, it is
necessary to verify the concentration of these compounds in the
main components of this product are shown in detail on Table 1.
juice because they give its medicinal properties. In this way, sam-
Wang and Su [20] showed that commercial noni juice (Tahitian
ples (200 L) of the juice were extracted every 7 min to quantify
Noni® Juice) prevents the formation of chemical carcinogen DNA-
the polyphenol content using the modified Folin–Ciocalteu method.
adduct.
1 mL of Folin–Ciocalteu reactive was added to the samples in a ves-
sel, after 2 min 0.8 mL of Na2 CO3 (7.5%) was added. Then it is kept
3. Experimental at 30 ◦ C for 90 min. Finally, the absorbancy is measured at 765 nm
[25].
The experimental device used in this study is constituted by a
system with two independent circuits for the circulation of the solu-
4. Modeling and simulation of the mass and heat transfer
tions: one for the solution to be treated (water or noni juice) and the
other for the extraction brine. Both circuits have peristaltic pumps
4.1. Equations of mass transfer
connected to graded vessels where the volume variations of the
solutions are measured as a function of time. The vessels are sub-
The fundamentals of the osmotic evaporation process were
merged in a thermostatized bath in order to maintain a constant
explained on Section 2.1 and shown in Fig. 1. A resistances-in-series
temperature (30 ◦ C). The circuits are connected to a hollow fiber
model can explain the transport of water through the membrane.
membrane contactor. The outline of this arrangement is presented
In this work has been applied this approach based on the study
in Fig. 2.
developed by Romero et al. [8,26] about the OD process. In this
Two different types of modules are used in the experiments:
case, the equations have been considered to solve the model for
a hollow fiber minimodule Celgard Liquicel© 1 × 5.5 (2300 fibers,
simultaneous heat and mass transfer in a hollow fiber contactor.
0.18 m2 of surface contact area, called Module 1) and a hollow fiber
The flux regimes inside the pores with the main chances of
minimodule Celgard Liquicel© 1.7 × 5.5 (7400 fibers, 0.58 m2 of sur-
occurring during the osmotic evaporation process are molecular
face contact area, called Module 2).
diffusion and Knudsen diffusion. In the water–brine system mass
The characteristics of these modules are presented in the Table 2.
transfer flux (mol m−2 s−1 ) of water vapor through the membrane
To analyze the process and facilitate the theoretical analysis, the
porosity can be estimated by molecular diffusion applying the fol-
phases to be treated are water and commercial noni juice (Tahitian
lowing equation:
Noni® Juice) circulated by the shellside of the hollow fiber contactor
in order to obtain the best mass transfer conditions. 400 mL of these P εD
(2) w−air P − aEw Pw
E
solutions were treated using 1300 mL of extraction brine, which was Jw = ln (1)
RT ı F
P − Pw
circulated by the lumenside. The circulation configuration was also
chosen in order to facilitate the cleaning procedure of the module
where P is the total pressure, aw water activity in brine, Pw repre-
considering the characteristics of both solutions. The brine is an
sents vapor pressure of water at the temperature of the respective
aqueous solution of calcium chloride with concentrations of 2, 4
interface, R is the universal constant of gasses, Dw–air the diffusion
and 6 mol kg−1 .
coefficient of water in the air; ε, , ı represent membrane porosity,
The experiments lasted between 60 and 120 min, time at which
tortuosity and thickness respectively.
the change of level in each one of the vessels was registered. The
On the other hand, mass transfer flux (mol m−2 s−1 ) of water by
mass transfer flux is quantified in function of the change in the brine
Knudsen diffusion can be estimated by the following equation:
level. At each day’s end the membrane was cleaned with an ethanol
solution 30% (v/v). CaCl2 was used as solute in the extraction solu- 2 εr 8
0.5
p F
− aEw Pw
E
(2)
tion since this produces a decrease of water activity greater than Jw = (Pw ) (2)
3 ı RTMw
other salts, which allows an increment of the driving force for the
mass transfer [8]. where rp is the pore radius, T is the average temperature and Mw is
The experimental design considers 3 variables: the concentra- the molecular weight of water (1.8 × 10−2 kg mol−1 ). Mass transfer
tion of the extraction brine, the circulation rates of the solution to flux of water through the boundary layers can be evaluated by the
Table 3
Levels and characteristics of the experimental design for modules 1 and 2.
Module 1 Module 2
Solution to be treated Cbrine (mol kg−1 ) Ffeed (L min−1 ) Fbrine (L min−1 ) Solution to be treated Cbrine (mol kg−1 ) Ffeed (L min−1 ) Fbrine (L min−1 )
Water 2.0–6.0 0.1–0.5 0.1–0.5 Water and noni juice 2.0–6.0 0.1–1.0 0.1–1.0
208 H. Valdés et al. / Journal of Membrane Science 330 (2009) 205–213
Fig. 3. Structure of the simulation algorithm to predict the simultaneous heat and mass transfer in the osmotic distillation process carried out in this work. Water is used as
feed solution to evaluate temperature polarization.
H. Valdés et al. / Journal of Membrane Science 330 (2009) 205–213 209
following equations: When the tube length is very small or the flux velocity is high,
the Lévêque equation can be used [31]:
= k(1) (xbF − x1F )
(1)
Jw (3)
1/3
Nu(3) = 1.86(Re(3) Pr (3) (D/L)) (11)
= k(3) (x2E − xbE )
(3)
Jw (4)
Then, if the temperature profiles are developed practically at
where x1F and x2E are the molar fractions of the water coming in and
the entrance of the fibers and besides Reynolds number is much
going out the pores, respectively. Simulations of the water–brine
less than 2300, the heat transfer coefficient is determined using Eq.
system do not consider the application of Eq. (3), because the feed-
(10). The estimation of the heat transfer coefficient on the shellside
ing solution to be treated is only pure water.
filled with the solution to be concentrated has been estimated by
In this study has been applied different correlations of the Sher-
means of the following correlation of the Nusselt number [32]:
wood number to estimate the mass transfer coefficient on the
0.55 1/3
lumenside, k(3) , in hollow fiber contactors [27,28]. The best approx- Nu(1) = 0.36(Re(1) ) (Pr (1) ) (12)
imations between experimental and simulated values of water flux
were obtained with the correlation of Notter [27]: This equation has been proposed to estimate the heat transfer coef-
ficient on the shellside in shell and tube heat exchangers.
0.88 1/3
Sh(3) = 0.0149(Re(3) ) (Sc(3) ) (5)
4.3. Simulation of the simultaneous mass and heat transfer in OD
This equation is applicable when Sc > 100 and its application
involves average discrepancies between 150 and 200% when the
The simulation of the mass transfer and the simultaneous mass
values of calculated transmembrane water flux are compared to
and heat transfer in the OD process was carried out using Matlab®
the experimental ones. In this way, the following specific relation-
7.1, following the calculus procedure for the water–brine system
ship has been correlated in this work in order to estimate the mass
shown in Fig. 3.
transfer coefficient on the lumenside from the Sherwood number
On this procedure first the conditions of operation and the mem-
in function of the Graetz number:
brane characteristics must be introduced, then the Regula Falsi
Sh(3) = 0.090 Gz 1/3 (6) cycle (RF3) is initiated in function of the temperature at the feed
solution–membrane interface (T1F ), which is considered an itera-
Finally, it must be accepted that in a steady-state the mass trans-
tive parameter. Thus, the properties of the boundary layer of feed
port flow through boundary layer on the feeding solution side,
solution can be estimated.
through the membrane porosity and the brine side must be equal
(1) (2) (3)
The values of temperature and concentration at the
(Jw AOD = Jw Aav = Jw AID ). The mean value of the contact surface brine–membrane interface (T2E , x2E ) were generated by a sec-
area through the membrane, Aav , was estimated as the average value ond and third Regula Falsi cycles (RF1 and RF2), later on the
between the inside and outside diameter of the fibers. properties of the brine boundary layer and the transmembrane
hE (T2E − TbE )
(3) (3)
Q = (9)
Table 5
Effect of each operating variable on the experimental transmembrane water flow in the concentration of noni juice.
Operating conditions Effect Increasing interval Jw A × 103 (mol s(1 ) Increasing ratio of the flow (%)
−1 −1
Ffeed = 0.1 L min Cbrine = 2.0 mol kg 0.52
Concentration of the brine, Cbrine 380.8
Fbrine = 0.1 L min−1 Cbrine = 6.0 mol kg−1 2.48
Ffeed = 1.0 L min−1 Cbrine = 2.0 mol kg−1 0.74
Concentration of the brine, Cbrine 354.2
Fbrine = 1.0 L min−1 Cbrine = 6.0 mol kg−1 3.35
Fbrine = 1.0 L min−1 Ffeed = 0.1 L min−1 0.61
Circulation rate of the feeding solution, Ffeed 20.9
Cbrine = 2.0 mol kg−1 Ffeed = 1.0 L min−1 0.74
Fbrine = 1.0 L min−1 Ffeed = 0.1 L min−1 2.54
Circulation rate of the feeding solution, Ffeed 31.8
Cbrine = 6.0 mol kg−1 Ffeed = 1.0 L min−1 3.35
Ffeed = 1.0 L min−1 Fbrine = 0.1 L min−1 0.63
Circulation rate of the extraction brine, Fbrine 17.41
Cbrine = 2.0 mol kg−1 Fbrine = 1.0 L min−1 0.74
Ffeed = 1.0 L min−1 Fbrine = 0.1 L min−1 3.00
Circulation rate of the extraction brine, Fbrine 11.64
Cbrine = 6.0 mol kg−1 Fbrine = 1.0 L min−1 3.35
H. Valdés et al. / Journal of Membrane Science 330 (2009) 205–213 211
Table 6
Values of the concentration of CaCl2 at the brine–membrane interface and heat flows through the membrane obtained by simulations in function of the circulation rates of
both solutions. Concentration in the bulk of the brine, xbE = 18.17% (w/w).
F (L min−1 ) Simulation of exclusive mass transfer Simulation of simultaneous heat and mass transfer
quantified before and after the osmotic evaporation treatment by L length of the fibers (m)
using a Brookfield viscosimeter in order to verify newtonian rhe- M molecular weight (kg mol−1 )
ological behavior and the increase of viscosity generated by the Nu Nusselt number (–)
concentration. Noni juice at 25 ◦ C and 8 ◦ Brix presents a viscos- P pressure (Pa)
ity value of 0.905 cp, while in the concentrated juice this value Pr Prandtl number (–)
increases to 1.152 cp at 32 ◦ Brix at the same temperature; besides, Q heat flux (W m−2 )
it may be seen in Fig. 6b that the mass of phenolic compounds is r radius (m)
maintained practically constant. R gas constant (J mol−1 K−1 )
In this type of process the main technical and economic limita- Re Reynolds number (–)
tion to its feasibility is the dilution of the extraction brine, because Sc Schmidt number (–)
the reconcentration and reutilization of this solution involves Sh Sherwood number (–)
important costs. However, in the studied case these limitations T temperature (K)
could be solved by the high commercial price of the juice and the x composition in %w/w (–)
interest to offer a high quality product.
Greek letters
6. Conclusions ε porosity (–)
␦ membrane thickness (m)
In this study has been developed a general characterization of tortuosity (–)
the concentration of noni juice by means of osmotic distillation
process. The application of this membrane operation has been eval-
Subcripts and supercripts
uated with experiments and theoretically studied by simulations
(1) referred to the boundary layer of the feeding solution
of simultaneous heat and mass transfer under conditions close to a
(2) referred to the membrane porosity
real implementation using hollow fiber membranes. The influence
(3) referred to the boundary layer of the brine
of the brine concentration, feeding flow, brine flow and the com-
air referred to air
bined effects on the transmembrane flow of water were quantified
Av average
for different operation conditions in order to identify the optimum
b referred to the bulk of solutions
conditions. The most important effect on the performance of the
E referred to the extraction solution
process under these conditions is the concentration of the brine.
F referred to the feed solution
The small thickness of the membranes used in this work enhances
ID inner diameter
the mass and heat transfer and it could minimize the effect of the
OD outer diameter
temperature polarization in this process. Mass transfer through the
p pore
membrane porosity seems to be described by a transition mecha-
v vapor
nism between molecular and Knudsen diffusion.
w water
Simulations of simultaneous mass and heat transfer allow pre-
dicting the transmembrane water flux with a good agreement with
experimental data. The approach used in this work can be a reliable References
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