Chemical Engineering Research and Design 1 6 0 ( 2 0 2 0 ) 233–239

Contents lists available at ScienceDirect

Chemical Engineering Research and Design

journal homepage: www.elsevier.com/locate/cherd

Dehydrated cranberry juice powder obtained by

osmotic distillation combined with freeze-drying:
Process intensification and energy reduction

A. Plaza a , R. Cabezas b , G. Merlet b , E. Zurob a,b , A. Concha-Meyer a ,

A. Reyes b , J. Romero b,∗
aCentro de Estudios en Alimentos Procesados (CEAP), CONICYT-Regional, Gore Maule R09I2001, Chile
bLaboratory of Membrane Separation Processes (LabProSeM), Department of Chemical Engineering, University of
Santiago of Chile, Av. Libertador Bernardo O’Higgins 3363, Santiago, Chile

a r t i c l e i n f o a b s t r a c t

Article history: The aim of this work was the study of the energy efficiency of the dehydration process of
Received 7 August 2019 cranberry juice using osmotic distillation (OD) in combination with freeze-drying. To achieve
Received in revised form 21 March this process, OD was performed on a hollow fiber membrane contactor with an initial sugar
2020 content of 8◦ Brix in the cranberry juice. This solution was concentrated to four different
Accepted 4 May 2020 final concentrations (25, 35, 45 and 57◦ Brix) with the purpose of reducing the lyophilization
Available online 17 May 2020 time obtaining a 100% dried product, using as a response variable the processing time. From
these obtained results, and when comparing the 8◦ Brix juice lyophilization to the process
Keywords: achieved by the combination of OD and freeze-drying, a decrease in the total process time
Osmotic distillation could not be achieved for any experimental assay. However, the 57◦ Brix cranberry juice
Freeze-drying previously concentrated by OD presented an 86% decrease in the energy requirements to
Cranberry juice obtain the same dehydrated product. Finally, a reduction of the energy consumption for all
Operating costs the experimental runs was observed in the samples concentrated by OD, as the step previous
Energy consumption to lyophilization, achieving an intensification in the efficient energy use during this process,
maintaining the same characteristics of the final product.
© 2020 Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

1. Introduction come these drawbacks, new techniques and processes, that

Foods are usually submitted to multiple processes to increase
its duration, be easily stored and to reduce the transport
costs associated (Mahalik and Nambiar, 2010). In the case of
fruit juices, and to comply with these purposes, traditional
thermal methods are used for their concentration such as
multistage vacuum evaporator equipment (Jiao et al., 2004).
This type of processing causes a decrease in the organoleptic
and nutritional properties, such as taste, color, aroma, vita-
min and antioxidant content due to the thermal sensitivity
of some responsible compounds (Babu et al., 2006). To over-
allow the production of juices with a similar or even better
quality of the sensory and nutritional properties of freshly
squeezed juice have been developed (Zhang et al., 2017). These
new techniques include freeze-drying, and concentration by
membranes such as reverse osmosis (RO) or osmotic distilla-
tion (OD) (Zambra et al., 2014; Kujawski et al., 2013; Raharitsifa
and Ratti, 2010; Onsekizoglu et al., 2010).
Freeze-drying is a drying method that generates high-
quality products (Liu et al., 2008). This technique is based
on the freezing and subsequent sublimation of water, which
is achieved by lowering the pressure and temperature under

∗
Corresponding author at: Universidad de Santiago de Chile (USACH), Departamento de Ingeniería Química, Av. Libertador Bernardo
O’Higgins 3363, Estación Central, Santiago, Chile.
E-mail address: julio.romero@usach.cl (J. Romero).
https://doi.org/10.1016/j.cherd.2020.05.003
0263-8762/© 2020 Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
234 Chemical Engineering Research and Design 1 6 0 ( 2 0 2 0 ) 233–239
the triple point of water (273.16 K and 0.6113 kPa) (Moran
et al., 2010; Ratti, 2001). The rehydrated product has excel-
lent properties with minimal changes in its quality when
compared to the original product. However, this process has
high operating costs, limiting the use of this technique to
products with high quality and price, such as coffee and
pharmaceutical preparations. On the other hand, membrane
separation techniques such as reverse osmosis (RO) have mul-
tiple applications and advantages. The use of RO presents low
thermal damages, low costs of equipment and low energy
consumption. However, this process reaches a maximum
concentration of 25–30◦ Brix, which is very low compared to
the 80◦ Brix that can be achieved by evaporation (Jiao et al.,
2004). Other membrane separation methods, which have been
recently investigated, are osmotic distillation (OD) and mem-
brane distillation (MD). In these methods, a hydrophobic
macroporous membrane is used, which contains air in their
pores producing a water mass transfer through these pores,
due to a difference of potential on both sides of the mem-
brane. In the case of membrane distillation, this difference
of potential is given by a temperature difference between the
solutions of both membrane sides. On the other hand, in
the case of osmotic distillation, the driving force is given by
a difference in vapor pressure, or by a water activity differ-
ence.
With the main goal of finding an optimal process that can
achieve the dehydration of juice in a shorter time, these tech-
niques can be complemented. Therefore, an optimization of
operational cost can be made in addition to the advantage of
preserving the aromatic compounds present in the juices.
The cranberry fruit, Vaccinium macrocarpon Ait., is of great
interest in this study, due to the important participation of
Chilean production in the world (Chile is the 3rd largest
producer) (FAOSTAT, 2017). This fruit has demonstrated over
several studies, to have important beneficial health proper-
ties, such as prevention of urinary tract infections (UTIs), and
anticarcinogenic and cardiovascular benefits (Khoo and Falk,
2013; Vasileiou et al., 2013). Therefore, it is very relevant to
keep these properties intact to produce juice with a high added
value. The use of these new technologies can be increasingly
competitive with traditional production by thermal evapora-
tion.
In this work, dehydrated cranberry juice powder was
obtained by a hybrid operation, which couples osmotic dis-
tillation with freeze-drying. The first operation involves the
concentration of cranberry juice at room temperature and
atmospheric pressure; while the second one allows obtain-
ing the fruit juice powder from the concentrated juice. Both
processes operate at low temperature and their combinations
represent an operational cost reduction in the preparation of a
product with minor losses of thermolabile active compounds
(Zambra et al., 2014).
2. Material and methods
The cranberry juice used in this study was obtained from
Agrícola Cran Chile Ltda., Lanco, Chile. This commercial con-
centrated juice had an initial concentration of 70.8◦ Brix which
was diluted to 8◦ Brix. This approach was selected to obtain a
standard initial concentration of cranberry juice, using always
8◦ Brix as the fit solution. The experimental procedure for the
dehydration of the cranberries juice consisted of a two-step
process. First, a concentration by osmotic distillation (OD)
Table 1 – Characteristics of the hollow fiber contactor
module used in this work.
Property (unit) Value or characteristic
Module type Minimodule liquicel® 1.7 × 5.5
Membrane material Polypropylene
Number of fibers 7400
Porosity (%) 40
ID of fiber (m) 2.2 × 10−4
OD of fiber (m) 3.0 × 10−4
Length of fiber (m) 0.120
ID of shell (m) 0.043
Contact surface area (m2 ) 0.58
Fig. 1 – Experimental set-up of osmotic distillation
pre-treatment process.
which was used as a pre-treatment for the dehydration pro-
cess by freeze-drying.
2.1. Preparation of cranberry juice powder
2.1.1. Concentration of cranberry juice by osmotic
distillation (OD)
The OD process was performed using a polypropylene
hydrophobic microporous hollow fiber module. In Table 1, the
characteristics of this contactor module are described.
The cranberry juice (8◦ Brix) was circulated through the
lumenside of the module. In countercurrent, a 50% (w/v) cal-
cium chloride (CaCl2 ) brine solution was circulated through
the shellside. This particular circulation configuration was
chosen in order to minimize the juice volume in the sys-
tem. In a previous work by Zambra et al. (2014), researchers
found that the optimal juice/brine volumetric ratio was 1:4.
This proportion was the optimal working condition to avoid
excessive dilution of the brine. Fig. 1 shows the experimen-
tal devices used for the concentration of cranberry juice using
OD. This procedure was based on the protocol described by
Zambra et al. (2014), in which the brine solution is previously
filtered under vacuum filtration to avoid the presence of sus-
pended particles. Both solutions; brine and cranberry juice,
were fed to the system using a peristaltic pump connected to
graded vessels, where the volume variations of the solutions
are measured as a function of the time. The constant temper-
ature (25 ◦ C) of the vessels was controlled by a thermostatic
bath.
To obtain the maximum transmembrane water flux of the
system, one experimental run was made using pure water
as a feed solution (baseline) following the same procedure
described above.
 Chemical Engineering Research and Design 1 6 0 ( 2 0 2 0 ) 233–239 235

Table 2 – Experimental conditions for the osmotic Table 3 – Experimental conditions of the concentrated
distillation pre-treatment. cranberry juice by freeze-drying.
Variable Value Variable Value

Pressure (bar) 1 Pressure (bar) 0.000220

Temperature (◦ C) 25 Temperature (◦ C) −51
Initial feed volume – juice (L) 1.00 Particle diameter (mm) 5.5
Initial extractant volume – brine (L) 4.00 Total initial volume (mL) ∼15
Feed flux – juice (L min−1 ) 1.2 Initial concentration of cranberry juice (◦ Brix) 8–25–35–45–57
Extractant flux – brine (L min−1 ) 1.2
Initial brine concentration (% w/v) 50
2.2. Operational equations for concentration and
Initial juice concentration (TDS) (◦ Brix) 8.0
Final juice concentration in OD process (TDS) (◦ Brix) 25–35–45–57
drying processes

2.2.1. Estimation of transmembrane water flux in the OD

process
The estimation of the transmembrane water flux (N) in
kg m−2 h−1 , was experimentally determined, by the reduction
of the remaining feeding volume as a function of the time (Eq.
(1)):

(Vt+t − Vt ) · 
N= (1)
(t) · A

where Vt [m3 ] represents the volume at a given time, t [h]

Fig. 2 – Experimental setup of the freeze-drying laboratory
equipment used for the dehydration of cranberry juice.
Simultaneously, the concentration of total dissolved solids
(TDS) of the cranberry juice was measured using a refrac-
tometer (Hanna Instruments, HI 96801, Woonsocket, USA)
graduated in ◦ Brix. The concentration of TDS was registered
at constant intervals of volume decrease, until the required
concentration. Finally, the concentrated juice samples were
stored at −20 ◦ C. The experimental conditions of the OD pre-
treatment are shown in Table 2.
represents the time difference between each volume measure-
ment, A [m2 ] is the contact area of the hollow fiber membrane
contactor,  [kg m−3 ] is the density of water, which is consid-
ered constant.
2.2.2. Equations of the drying process
Data of the moisture content of the samples from the dehy-
dration process by freeze-drying were adjusted to different
mathematical models widely used for foods drying, such as
the Newton, Henderson-Pabis, and Page models (Vega et al.,
2007; Jennings, 1999), additional to the linear model. From
these models, the best results were chosen for each case,
under the criteria of choosing the correlation coefficient clos-
est to 1. The models used are presented in Eqs. (2)–(5):
Linear :
X
= −k · t + c (2)
X0

X
Newton = exp(−k · t) (3)
2.1.2. Freeze-drying of concentrated cranberry juice X0
After the osmotic distillation, the obtained concentrated juice
samples were rapidly frozen by dipping them in liquid nitro- X
Henderson-Pabis = a · exp(−k · t) (4)
X0
gen. The purpose of using a rapid freezing method was the
generation of smaller water crystals, which results in a better X
distribution of the pore size of the dry particles (Evans, 2008). Page = exp(−k · tn ) (5)
X0
The juice was immersed in liquid nitrogen leaking through a
buret to generate spheres of approximately 5 mm of diameter, where X represents the dry basis moisture content (d.b.) as a
as shown in Fig. 2. The juice dripped in 15-s intervals between function of time, X0 is the initial moisture (d.b.) and, t is the
each drop to avoid agglomeration. time in hours.
The equipment used in this process consisted of a 4.5 L Lab-
cono FreezoneTM freeze-dryer (Dry systems, model 7750030). 3. Results and discussion
The diagram of this experimental setup is shown in Fig. 2. The
automatic lyophilization program of the freeze-drying system 3.1. Performance of OD assays
decreased the temperature to −40 ◦ C. After this temperature
is reached, the automatic switch activates the vacuum pump Following the OD assays described in Section 2.1.1, Fig. 3 shows
lowing the pressure in the collector chamber to 0.000220 bar. the change of the concentration of the total dissolved solids
The mass of the glass flask containing the sample (freeze (TDS) of the feed solution as a function of the time.
juice spheres at different initial concentrations) was measured As dissolved solids do not permeate through the mem-
every 30 min, to obtain the moisture of the samples as a func- brane, the increase of the concentration as a function of the
tion of the time. The experimental conditions of this process time in all the experimental runs demonstrates the success of
are shown in Table 3. the permeation of water from the feed solution to the Brine.
236 Chemical Engineering Research and Design 1 6 0 ( 2 0 2 0 ) 233–239

Fig. 3 – TDS concentrations in the feed solution as a Fig. 5 – Transmembrane flux of water for distilled water
function of the time for all the different final concentrations (baseline); and cranberry juice (57◦ Brix), as a function of the
of juice. time.

Table 4 – Viscosity and density of cranberry juice (25 ◦ C)

as a function of TDS.
Water 8◦ Brix 25◦ Brix 35◦ Brix 45◦ Brix 57◦ Brix

Viscosity [cP] 0.97 0.98 1.19 1.30 3.06 7.16

Density [kg m−3 ] 998 1030 1090 1140 1186 1244

Fig. 4 – Behavior curve of the remaining volume of feed

solution as a function of time.

For all the experimental runs, the nonlinear behavior can

be explained by the changes in the transport properties,
(Table 4), as well as,the decrease in the mass transfer poten-
tial, as a consequence of the change in the concentrations of
both the cranberry juice and brine. The cranberry juice for the
concentration of the TDS shows a strong exponential behavior
after the 20◦ Brix.
The osmotic distillation reaches concentrations values
similar to those obtained by the thermal process with the
advantage that the content of polyphenols and anthocyanins
are preserved almost like fresh fruit (Zambra et al., 2014). Fig. 6 – Experimental data for the moisture ratio (X/X0) of
In order to understand the membrane processes, the water cranberry juice as a function of the time and their
evaporation rate can be studied. corresponding models: (A) 25◦ Brix initial concentration
Fig. 4 shows the behavior of the water volume of the feed (Page model); (B) 57◦ Brix initial concentration (Newton
solution as a function of the time for both the baseline test model). Dots correspond to the experimental values and
(distilled water) and the experimental runs (cranberry juice lines represent the simulated model.
concentrated to 57◦ Brix).
The fast decrease of the water volume in the baseline Fig. 6 can be used to explain the main differences in the
run compared to the behavior of the cranberry juice can be behavior of the OD process as a function of the feed solu-
explained by the major potential for the mass transfer that tion. First, the initial transmembrane flux in the baseline is
the pure water in the feed solution generates. For a better 1.3 times bigger than the results obtained with the cranberry
description of this process, the transmembrane flux of water juice, due to the lower activity coefficient of water in the 8◦ Brix
was calculated (Eq. (1)), as shown in Fig. 5. These results were cranberry juice. This generates a minor potential for the mass
obtained from the data described in Fig. 4. transfer process compared to the constant and higher activity
 Chemical Engineering Research and Design 1 6 0 ( 2 0 2 0 ) 233–239 237

coefficient of distillate water. The linear behavior of the trans-
membrane flux of water of the baseline run as a function of
the time is caused by a decrease of the mass transfer potential
that the dilution of the brine generates for the incorporation
of the extracted water. For the experimental runs with cran-
berry juice (57◦ Brix), a decrease of the transmembrane flux of
water is also observed. However, the fluxes show an exponen-
tial behavior, due to the decrease of the mass transfer potential
caused by the dilution of the brine and the concentration of
the juice. Additionally, the increase of the mass transfer resis-
tance of the feed solution is a result of the increase of the
viscosity and density caused by the concentration of the sugar
present in the juice. This effect can be easily observed after 2 h
of processing.
However, the cranberry juice has a good response to be con-
centrated by osmotic distillation. This can be explained by the
low variation in density and viscosity as the concentration of
cranberry juice is increased, when comparing with the values
obtained from the OD for other variety of fruits (Valdés et al.,
2009; Vaillant et al., 2001; Cassano and Drioli, 2007a; Cassano
et al., 2007). This is mainly because of the composition of cran-
berry juice, which is mostly fructose.
Finally, the average Transmembrane fluxes and final con-
centrations of cranberry juice obtained from the OD assays are
shown in Table 5. The average transmembrane flux (N) for each
experimental run in kg m2 h−1 and R2 correlation coefficient
obtained from the exponential regression of the experimental
data are depicted in Table 5, as a function of the required time
to reach the established concentration.
The maximum average value of transmembrane water
flux through the membrane was 0.50 kg m2 h−1 . This value
was used as a reference for the maximum potential of the
OD process. The transmembrane juice flux throughout the
membrane was between 0.33 and 0.38 kg m2 h−1 , a 25% lower
than the flux obtained with distilled water. This effect can be
attributed to the mass transfer potential decrease due to lower
water activity in the feed flow.
3.2. Freeze-drying
Freeze-drying assays were performed using the different con-
centrations of cranberry juice obtained from the osmotic
distillation concentration process. Table 6 shows the freeze-
drying operational times employed to achieve complete
dehydration. A reduction in the operating time of 5 h for the
57◦ Brix juice samples compared to the 8◦ Brix juice samples
was observed. This result represents a time saving of slightly
less than 60%. Although this represents an excellent result,
it must be taken into consideration that using samples with
lower initial water content for freeze-drying formed fewer ice
crystals. This causesless porosity in the food samples dur-
ing the primary drying, which implies a more heterogeneous
structure of the solid food matrix resulting in a more likely to
collapse sample (Jennings, 1999). On the other hand, Table 6
shows the adjusted parameters for the freeze-drying of frozen
juice samples, where R2 is the coefficient of determination and
RMSE denotes the root mean squared error. It can be seen
that the adjusted parameters for an initial concentration of
8◦ Brix are similar to the parameters obtained with an initial
concentration of 25◦ Brix. Mathematical models fitted to the
experimental data are different depending on the initial con-
centration, which may indicate that they have different mass
transfer mechanisms prevailing in each case.
Table 6 shows how the page model can represent the freeze
dehydration process for the experimental runs where the ini-
tial concentration is lower than 45◦ Brix, while the Newton
model adjusts better to the 57◦ Brix concentration. This can be
explained in terms of the drying kinetics of these solutions,
due to the unidirectional molecular diffusion described by the
spherical geometry of the lyophilized concentrated juice.
The adjustment to the Newton model described for the
57◦ Brix lyophilized samples can be understood in terms of the
rapid decrease in the moist of the samples during the initial
time in the lyophilization state, followed by a much less effec-
tive decrease in moist due to the less availability of free water

Table 5 – Resume of results obtained from osmotic distillation assays.

Feed TDS initial TDS final Time t (hh:mm:ss) N (kg m−2 h−1 ) R2
concentration, C0 concentration, C
(◦ Brix) (◦ Brix)

Distilled water 0.0 0.0 1:47:00 0.50 ± 0.05 0.9999

Cranberry juice 8.0 25.0 3:29:31 0.37 ± 0.06 0.9997
35.0 3:47:00 0.37 ± 0.05 0.9999
45.0 3:57:38 0.38 ± 0.05 0.9986
57.0 4:38:46 0.33 ± 0.04 0.999

Table 6 – Freeze-drying times established experimentally for concentrated cranberry juice by OD and parameters of
dehydration model at different concentrations of TDS.
Initial concentration Time (h) Model Parameters of Statistic
SDT (◦ Brix) the model parameters

8 8.5 Page K (h−n ) 9.76 × 10−2 RMSE 0.0379

N 1.639 R2 0.989
25 8.0 Page K (h− n ) 9.69 × 10−2 RMSE 0.0379
N 1.518 R2 0.989
35 7.0 Page K (h−1 ) 1.42 × 10−1 RMSE 0.0224
C 1.026 R2 0.996
45 4.5 Page K (h− n ) 2.27 × 10−2 RMSE 0.0594
N 3.395 R2 0.980
57 3.5 Newton K (h−1 ) 5.11 × 10−1 RMSE 0.0742
R2 0.921
238 Chemical Engineering Research and Design 1 6 0 ( 2 0 2 0 ) 233–239

or water activity. These models can be graphically observed in

Fig. 5.

3.3. Energy consumption

Fig. 7 shows values obtained in the evaluation of gross energy

consumption for the different concentrations of cranberry
juice expressed as total dissolved solids (TDS) obtained from
the osmotic distillation and subsequent freeze-dried. Energy
consumption is associated with both the mechanic work to
achieve the pump operation and, the heat for the sublimation
of ice during the freeze-drying process and the posterior re-
concentration of the brine. It can be observed that the energy
consumption is mostly given by the heat when carrying out
the primary freeze-drying operation and, the concentration
of the brine in the osmotic distillation process. Dehydration
of the concentrated cranberry juice by OD does not achieve
net savings in energy consumption. However, to analyze in
detail the type of energy consumed, particularly in the case
of the 57◦ Brix solution, where savings in mechanical energy
consumption achieve up to 45%. This result is promising since
in the system studied, the re-concentration of the brine and
the heat supplied for the freeze-drying, was provided by nat-
ural convection from the atmosphere, being the mechanical
work, the only energy form associated to an economic cost.
It also warns that excluding the consumption for the re-
concentration of CaCl2 achieved energy savings from 70–90%
in all the freeze-dried samples from the concentrated juice.
Fig. 6B and C show that most of the energy consumption of
the OD is due to the re-concentration of the brine, implying
that future studies should focus on the optimization of the
energy consumption during this stage since it is possible to
achieve savings in the gross consumption.
Fig. 6D shows that for all cases, a reduction in operational
cost was obtained. When the heat needed for the sublima-
tion step is delivered by electricity, the savings are greater
due to the great consumption of calorific heat for the freeze-
drying of fresh juice. In the reference case, in which the initial
concentration of cranberry juice was 8◦ Brix, the operational
costs were greater due to the large calorific consumption to
freeze-dry the fresh juice. In other cases, the sublimation heat
was smaller due to the removal of large amounts of water by
osmotic distillation and then the electricity consumed was
smaller. Along with that, even though the energy reduction
was greater, it must be noted that the total cost for the heat Fig. 7 – The indicated concentrations were achieved by OD
generated by electricity was always greater than the total cost and freeze-drying. In red, the time and energy consumption
for the heat supply by steam, which was almost four times of freeze-drying; in blue, time and energy consumption of
more when the freeze-drying of the fresh juice with an initial the OD process; in orange energy consumption supplied by
concentration of 8◦ Brix. electricity; in green, energy consumption supplied by
steam. (A) Sum of operation times for total dehydration of
4. Conclusions cranberry juice with an initial concentration of 8◦ Brix; (B)
gross energy consumption for total dehydration of 1 L of
It was found that the concentration of cranberry juice by cranberry juice with 8◦ Brix; (C) Gross energy consumption
osmotic distillation was competitive when comparing to the for total dehydration of 1 L of cranberry juice with 8◦ Brix,
traditional concentration thermal methods. Moreover, fresh regardless of the re-concentration of the brine solution of
cranberry juice and cranberry juice concentrated at different CaCl2 ; (D) energy cost associated with energy consumption
TDS values can be dehydrated using freeze-drying, combined estimated for total dehydration of 1 L of cranberry juice
with osmotic distillation to achieve an intensified process. with 8◦ Brix. Using electricity as an energy source for the
However, the combination of osmotic distillation with freeze- mechanical work of the OD and freeze-drying and, steam
drying did not reduce the total operation time compared with as heat supply for the freeze-drying operation and for the
just the freeze-drying. On the other hand, the gross energy re-concentration of CaCl2 brine.
consumption was not reduced compared to the energy con-
sumption due to the freeze-drying of the fresh juice. However,
a reduction of more than 70% of the energy consumption was
 Chemical Engineering Research and Design 1 6 0 ( 2 0 2 0 ) 233–239
achieved if the re-concentration of the brine was not con-
sidered. It is proposed to study the energy optimization of
the re-concentration of brine to improve these results. Finally,
reducing the operational cost based on the laboratory results,
achieving a saving of over 65% using electricity as a heat source
for the freeze-drying step was estimated.
Conflict of interest
None declared.
Acknowledgements
This work was supported by Project FONDECYT de Iniciación
11150255 and Project POSTDOC DICYT, Código 0218111RF,
Vicerrectoría de Investigación, Desarrollo e Innovación, Uni-
versidad de Santiago de Chile, Usach.
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