Drying Technology

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Porous frozen material approach to freeze-drying

of instant coffee

Wei Wang, Shihao Wang, Yanqiu Pan, Jing Yang, Shuo Zhang & Guohua Chen

To cite this article: Wei Wang, Shihao Wang, Yanqiu Pan, Jing Yang, Shuo Zhang & Guohua
Chen (2019) Porous frozen material approach to freeze-drying of instant coffee, Drying Technology,
37:16, 2126-2136, DOI: 10.1080/07373937.2018.1564759

To link to this article: https://doi.org/10.1080/07373937.2018.1564759

Published online: 30 Jan 2019.

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DRYING TECHNOLOGY
2019, VOL. 37, NO. 16, 2126–2136
https://doi.org/10.1080/07373937.2018.1564759

Porous frozen material approach to freeze-drying of instant coffee

Wei Wanga, Shihao Wanga, Yanqiu Panb, Jing Yanga, Shuo Zhanga, and Guohua Chenc
a
School of Chemical Machinery and Safety, Dalian University of Technology, Dalian, China; bSchool of Chemical Engineering, Dalian
University of Technology, Dalian, China; cDepartment of Mechanical Engineering, The Hong Kong Polytechnic University, Hong
Kong, China

ABSTRACT ARTICLE HISTORY

Porous frozen material with a certain initial porosity was prepared to explore its influence Received 14 August 2018
on freeze-drying experimentally. Soluble coffee was selected as the solute in aqueous solu- Revised 20 November 2018
tion and liquid nitrogen ice-cream making method was used to prepare the frozen materi- Accepted 28 December 2018
als. Results showed that freeze-drying can be significantly enhanced using the initially
KEYWORDS
porous frozen material compared with the traditionally solid one. By keeping the same sam- Freeze-drying; desorption;
ple mass and moisture content with sole radiation heating, drying time of the porous frozen drying time; initial
sample was about one third shorter than that of the solid one under the same tested oper- saturation; sublimation
ating conditions. SEM images of dried products revealed that the porous material had a
loose and tenuous structure that was favorable to the transportation of sublimated vapor
and the desorption of bound moisture. Appropriately increasing the chamber surface tem-
perature benefited the freeze-drying process and changing the chamber pressure had little
effect on the process. Combined radiation and conduction heating can further promote the
freeze-drying process and save as much as 36.4% of the drying time. The porous frozen
material was found to have a wider range of operating temperature and result in relatively
lower residual moisture content.

GRAPHICAL ABSTRACT

Introduction
Coffee is acknowledged as one of the most favorites
and widely traded agricultural merchandises in the
world.[1] Instant coffee refers to powder or granule
obtained from fresh coffee beans through roasting,
grounding, extracting, and drying.[2] Commercially
used drying method is either spray drying or freeze-
drying.[3] Spray drying is a well-established method of
producing dried powder directly from liquid by rapid
drying with hot gas. And most instant coffee produc-
tion comes from spray drying due to its high produc-
tion capacities.[4,5] However, Spray drying as a typical
thermal drying often brings possibilities of losing
some heat-sensitive materials, such as aroma and anti-
oxidant ingredients in coffee. Freeze-drying is a
unique form of drying that removes moisture mainly
by sublimation. It can lead to the best quality of dried
products among almost all drying techniques.[6,7]

CONTACT Wei Wang dwwang@dlut.edu.cn School of Chemical Machinery and Safety, Dalian University of Technology, Dalian 116024, China.
Color versions of one or more of the figures in the article can be found online at www.tandfonline.com/ldrt.
ß 2019 Taylor & Francis Group, LLC

Therefore, freeze-drying plays an important role in the
processing of foods, pharmaceuticals, and biological
products.[6,8] It has also found applications in the prep-
aration of new materials.[9,10] Freeze-dried coffee yields
a better quality product than spray-dried coffee.[7,11]
However, freeze-drying is an energy intensive and
expensive process due to relatively long drying time and
poor overall energy efficiency.[12–14] Reducing freeze-
drying time so as for lowering energy consumption and
raising productivity therefore become a worldwide chal-
lenge during the past decades.
Freeze-drying consists of freezing and drying, and
the latter stage includes simultaneous sublimation-
desorption, vacuum maintenance, and vapor conden-
sation. Early effort to enhance a freeze-drying process
mainly focused on the drying stage itself. The simplest
approach is the optimization of operating conditions
including heating shelf temperature and drying cham-
ber pressure.[12,15,16] This approach can now be
achieved in an automatic control system specially
designed although it only resulted in a limited promo-
tion.[17,18] Microwave-assisted heating has been
proved to facilitate the heat transfer of freeze-dry-
ing.[19,20] However, its application in freeze-drying
must be evaluated for each individual product. If solid
substrate in a frozen material does not absorb micro-
wave energy easily, microwave-assisted heating will be
less effective since ice crystals hardly absorb micro-
wave energy.[21] Dielectric material has to be used in
this case as an internal heat source, which causes an
additional operating complexity.[22,23] Latter endeavor
for the process enhancement was to improve the
freezing stage. Freezing is the first and important
stage of a freeze-drying process as it has impact on
pore size, shape, and connectivity of frozen materials.
Subsequent process performance and product charac-
teristics largely depend on this stage. Optimization of
the freezing stage includes freezing rate control, ice
nucleation regulation, and annealing.[24,25] It is recog-
nized that fast freezing gives small and numerous ice
crystals which are favorable to the secondary drying
stage;[26,27] and slow freezing leads to large and less
numerous crystals which are beneficial to the primary
drying stage.[15,28] Ice nucleation regulation was found
to produce large-size and narrowly distributed ice
crystals, and facilitate uniform freezing.[29,30]
Annealing was reported to be able to reduce the freez-
ing-induced heterogeneity, simplify the amorphous
structure, and increase the ice crystals size.[31,32] More
recently, X-ray computed tomography was employed
for the determination of mass transfer resistance to
vapor flow and the observation of glassy state relaxation
DRYING TECHNOLOGY 2127
during annealing.[33,34] A common characteristic of
these methods is that the mass transfer resistance is
decreased at the primary stage due to the increased size
of ice crystals, while the moisture desorption is weak-
ened at the secondary stage due to the decreased
internal surface area. The overall result depends on the
binding effect between the solid substrate and moisture.
If this dependency is less significant, the drying rate can
be enhanced moderately.[35,36] However, those methods
can only find limited applications in production units,
probably due to the practical difficulties in satisfying
industrial-scale requirements.
It has to be pointed out that current optimization
of the freezing stage has been implemented towards
the solid frozen material through direct freezing with-
out initial pores. In fact, a liquid material to be
freeze-dried can be first prepared into a frozen mater-
ial with a certain initial porosity and then freeze-
dried. This unconventional freezing strategy is quite
similar to the ice-cream making method.[37,38] Such a
porous frozen material is expected to facilitate the
migration of sublimated vapor in prebuilt pores and
the desorption of bound moisture due to a larger sur-
face area. The main objective of the present work is
to verify the effect of the initially porous frozen
material on freeze-drying of instant coffee. The result
obtained can help one to clarify the mechanism of
process enhancement and guide the future implemen-
tation of the proposed process.
Materials and methods
Materials and facilities
Soluble coffee powder (Nescafe, China) was selected
as the solute in aqueous solution. De-ionized water
was used as the solvent, which was provided by
Dalian University of Technology (China). Liquid
nitrogen was purchased from Dalian Institute of
Chemical Physics, Chinese Academy of Sciences.
Facilities employed here included an analytical bal-
ance (ME403E/02, Mettler, Switzerland), a draught dry-
ing cabinet (DHG-9070A, Yiheng, China), a moisture
analyzer (HR83-P, Mettler, Switzerland), and a scanning
electronic microscope (Quanta450, FEI, America).
Sample preparation
The aqueous solution of coffee was prepared by dis-
solving 40 g of coffee powder with 60 g of de-ionized
water. The initial moisture content was 1.5 kg/kg on a
dry basis. The solid frozen material without initial
pores was prepared by pouring the solution into a
2128 W. WANG ET AL.
Figure 1. Schematic diagram of sample mold.
cylindrical container of 14.8 mm in diameter with a
Teflon supporting pad of 5 mm in thickness at bot-
tom, and then placed into a freezer at –48  C for 6 h.
The porous frozen material with a certain initial por-
osity was prepared with two freezing steps, initial
freezing and further freezing. During the initial freez-
ing, the liquid nitrogen ice-cream making method was
employed, which is described as follows. The liquid
nitrogen was slowly added into the solution in a heat-
insulated barrel while mechanical stirring at about
400 rpm. The solution being processed then expanded
into a mousse-like frozen material with initial pores.
It should be pointed out that no any additive like an
emulsion stabilizer has been used in this step.[13,39]
Afterwards, such a premade material was molded in a
container with a supporting pad at bottom, and
quickly placed into the freezer for further freezing at
–48  C for 6 h. The molding allowed forming the ini-
tially solid and porous frozen samples of equal mass.
Before freeze-drying, the contained sample mold
was temporarily moved out of the freezer, allowing it
to stay at room temperature for a while or holding it
in hand for a moment to remove the container. The
sample mold without the container but with the sup-
porting pad was then placed back to the freezer for at
least 30 min to ensure a uniform initial temperature.
Thus, the sample mold was well prepared and ready
to be freeze-dried. Schematic diagram of the sample
mold is shown in Figure 1.
Two kinds of the sample molds, one for the solid
frozen material without initial pores and the other for
the porous one with initial pores, were prepared with
the same initial mass of 1.6 g excluding the supporting
pad. The concept of saturation, S, which is the ratio
between the actual pore volume of moist material and
the total pore volume of absolutely dried product, was
used to express the moisture content of the samples.
This concept has been widely adopted in porous
media transport phenomena for convenience if the
rigid solid substrate assumption is valid.[40] The solid
frozen sample had the initial saturation, S0 = 1.0 and
the height of 9.1 mm. The porous one had the meas-
ured initial saturation, S0 = 0.2 and the height of
31.2 mm due to its increased apparent volume. The
relation of the initial saturation and the intrinsic por-
osity with the initial mass and the moisture content of
the sample can be found elsewhere.[13]
Experimental apparatus
Experiments were conducted in a lab-scale multifunc-
tional freeze-dryer. Flow diagram of the apparatus is
shown in Figure 2. It consists of five subunits: a vacuum
unit, a temperature control unit, a data acquisition unit, a
freezing unit, and a pad heating unit. The vacuum unit
includes a vacuum pump (RV12, BOC Edwards, Britain),
a quartz drying chamber (2.3 L, TGP, Britain), and a
home-made cool trap. The temperature control unit con-
sists mostly of a circulator (9712, PolyScience, America), a
heat exchanger (0.72 m2, Yalong, China), a blower (60 m3/
h, 11.8 kPa, Sensen, China), and a home-made heating
cabinet. It was designed to maintain a constant tempera-
ture on the chamber surface. The data acquisition unit is
constitutive of a pressure sensor (APG100-XLC, BOC
Edwards, Britain), an infrared sensor (CI3A, Reytek,
America), a loadcell (0.3 kg, Mavin, China), a data acqui-
sition card (PCI-6221, NI, America), and a PC (M7130,
Lenovo, China). It was used to digitize the analog signals
generated by the three sensors through the LabVIEW
source code written for display, storage, and analysis of
experimental data. The freezing unit is an ultralow tem-
perature freezer (DW-GW138, Meiling, China) outside
the drying chamber.
To investigate the effect of heating mode on freeze-
drying, a pad heating unit was specially designed to
implement the combined heating of radiation and
conduction, as shown in Figure 3. A thermal rod was
installed between the sample mold and the loadcell so
that the heat can be transported from the rod onto
the supporting pad of the sample mold through con-
duction. Since the loadcell was directly connected to
the thermal rod, non-contact heat transfer had to be
adopted to avoid loadcell signal interference. The rod
was surrounded coaxially by a heating jacket within
which six electrical bars (30 W in total) were uni-
formly inserted. The heat transported towards the rod

Figure 2. Flow diagram of experimental apparatus. (1) Pad heating unit; (2) sample mold; (3) drying chamber; (4) heating cabinet;
(5) supermeter; (6) heat exchanger; (7) circulator; (8) blower; (9) regulating valve; (10) pressure sensor; (11) vacuum pump; (12)
cool trap; (13) freezer; (14) date acquisition card; (15) PC; (16) infrared sensor; (17) loadcell; (18) three-way valve; and (19)
PID controller.
Figure 3. Pad heating unit. (1) Heating jacket; (2) thermo-
couple; (3) thermal rod; (4) sample mold; (5) infrared thermo-
couple; (6) electrical bar; and (7) loadcell.
came from the radiation of the jacket. Rod tempera-
ture was monitored by a sub-miniature infrared
thermocouple (OS36-K, OMEGA, America), and dis-
played and recorded by a TrueRMS supermeter
(HHM290/N, OMEGA, America). Jacket temperature
was measured by a thermocouple (SC-TT-K-30-36,
OMEGA, America) and controlled by a home-made
PID controller.
Experimental methods
Typical operating conditions in the present tests were
35  C as chamber surface temperature, T, and 22 Pa as
chamber pressure, p. Two heating modes, one for sole
DRYING TECHNOLOGY 2129
radiation heating from the chamber surface toward the
sample mold and the other for combined heating of radi-
ation and conduction, were adopted during experiments.
By keeping the same sample mass and the same initial
moisture content under the consistent operating condi-
tions between the solid and porous frozen samples, the
experimental procedures are described as follows:
1. Switch on the circulator (7 in Figure 2, the same
below) and the blower (8) to preheat the drying
chamber (3) to the preset temperature. Ensure that
liquid nitrogen is fully supplied in the cool trap (12).
2. Turn on the pad heating unit and set the PID
controller (19) to make the rod (3 in Figure 3)
reach the desired temperature, and turn on the
supermeter (5) to monitor and record the rod
temperature if the combined heating mode is
selected. Ignore this procedure if the radiation
heating mode is selected.
3. Regulate the three-way valve (18) to connect the
drying chamber to the vacuum pump (11). Turn
on the vacuum pump and adjust the regulating
valve (9) to reach the tested chamber pressure.
4. Regulate the three-way valve to temporarily iso-
late the drying chamber from the vacuum pump.
Move the sample mold from the freezer (13) into
the drying chamber as soon as possible. Change
the three-way valve to reconnect the drying
chamber to the vacuum pump.
5. Run the data acquisition unit to record the varia-
tions of the sample weight, the chamber surface
2130 W. WANG ET AL.
Figure 4. Drying curves of two samples with different initial
saturations.
Figure 5. Drying rate curves of two samples with different ini-
tial saturations.
temperature, and the chamber pressure with time
at a given frequency.
6. Stop the data acquisition unit and the pad heating
unit (if appropriate) when there is no significant
change of sample mass displayed on the PC
screen. Turn off the vacuum pump and adjust the
three-way valve for venting. Switch off the circu-
lator and the blower.
7. Remove the dried product from the chamber and
measure its residual moisture content of
dried products.
The residual moisture content was analyzed with
the gravimetric determination of mass loss. The coffee
sample was placed on an aluminum dish and heated
at 90 ±1 C for 2 h in the drying cabinet.[1] The
switch-off mode of the moisture analyzer was set to
be less than 1 mg of mass loss within 50 s. The average
value of measured moisture contents was adopted in
the experiments.
The procedures of SEM (scanning electronic micro-
scope) characterization are briefly described as follows.
A sample of the dried cake was first mounted onto a
sample stub, and then sputter-coated with an ultrathin
layer of gold after nitrogen purging. Such a procedure
made this non-conductive material to acquire elec-
trical conductivity. Afterwards, the coated sample was
embedded to the stub holder within the SEM chamber
for scanning and imaging at 20 kV of voltage, 3.0 of
spot size, and either 12.1 or 12.9 mm of working dis-
tance at different magnifications.
Results and discussion
Effect of initially porous frozen material on
freeze-drying
Figure 4 shows experimentally measured drying curves
for the initially solid and porous frozen samples under
the typical operating conditions with radiation heat-
ing. By keeping the same sample mass, the same ini-
tial moisture content and also the same drying
conditions, the drying time for the porous frozen
sample was 3.1 h which was much shorter than 4.6 h
of the solid one. About 32.6% of drying time was
saved under the tested operating conditions. This
indicates that the proposed idea is feasible and effect-
ive, and the initially porous frozen material can
indeed enhance the freeze-drying process significantly.
Apart from the shorter drying time, the residual mois-
ture content of the dried product from the initially
porous frozen material was 0.66% on a wet basis that
was much lower than 4.38% of the initially solid one.
It is worth mentioning that triplicate tests have been
conducted to quantify the repeatability of the experi-
mental data. Excellent reproducibility was achieved for
both kinds of the frozen samples. Maximum standard
deviations of all data points were 0.0083 and 0.0044
on their respective drying curves as plotted in Figure
4. The subsequently presented drying curve data were
all from the average values of respective repeated tests
under different operating conditions. Meanwhile, no
collapse of the structure was judged from the drying
curves during freeze-drying, and no crack or deform-
ation was observed from the dried products after
freeze-drying.
Figure 5 shows normalized drying rate curves for
the two samples with different initial saturations based
on the data shown in Figure 4. For the convenience
of analysis, the relative saturation, f, defined as the
ratio of the real-time saturation to the initial satur-
ation (S/S0), is used in the presentation. The drying
rate of the initially porous frozen sample was always
higher than that of the solid one. At the very begin-
ning of drying, the drying rate of the porous sample

Figure 6. SEM images of dried products at different magnifications. (a–c) for the initially solid frozen sample; (d–f) for the initially
porous one.
was almost three times greater than that of the solid
one. It is due to the initially prebuilt pore space that
sublimated/desorbed vapor can easily migrate out-
wards. For the solid frozen sample, the drying process
experienced a constant rate period at the early stage,
and then became a falling rate period gradually until
the end of drying. For the porous frozen sample, how-
ever, the drying process was always in the falling rate
period. As a result, the primary and secondary stages
in the freeze-drying of the porous frozen material
were likely redistributed compared to those of the
solid one as seen subsequently.
SEM characterization of dried products
To examine the pore size, structure, and connectivity
of the dried cake so as to further understand the
freeze-drying processes of the two frozen materials,
SEM characterization was performed for the two dried
products. Figure 6 shows SEM images at different
magnifications.
The morphology of Figure 6(a) manifests a netlike
structure that is compact and dense. It has to be men-
tioned again that the solid frozen sample was obtained
through direct freezing in the freezer. The coffee solu-
tion first experienced a cool supercooling during
DRYING TECHNOLOGY 2131
freezing. After nucleation, ice crystals gradually grew
up and pushed the circumambient solute to their
interstices. Interstitial fluid became more and more
concentrated until transforming into an amorphous
solid eventually.[16] Inspection of Figure 6(b, c) shows
that the pore shapes are irregular and the pore walls
are thick and closed. This would impede the subli-
mated vapor to transport outside of the material
being dried.
The morphology of the dried cake from the porous
frozen sample is remarkably different from that of the
solid one. Figure 6(d) exhibits a typically spherical
structure with a bidisperse porosity that is looser and
more porous. The averaged pore size for this kind of
the material is much larger than that of the solid
material. This is because a certain amount of gasified
nitrogen has been incorporated into the material dur-
ing the initial freezing. Such a pore structure has fixed
before the further freezing. It is seen in Figure 6(e)
that the porous frozen material made with this new
method has continuous pore space and pierced solid
substrate. This porous material with a certain initial
porosity would have less mass transfer resistance, and
the sublimated vapor could escape more easily during
drying, leading to a higher primary drying rate.
Further observation of Figure 6(f) reveals that the
2132 W. WANG ET AL.
Figure 7. Drying curves of two samples at different chamber
temperatures.
Figure 8. Drying curves of two samples at different cham-
ber pressures.
solid substrate of the porous material is fine and tenu-
ous. This implies that this kind of the material pos-
sesses a larger internal surface area than the one made
with the conventional method. This would promote
the desorption of bound moisture at the secondary
drying stage. This may be because combined pattern
of moisture with solid substrate changed for this kind
of the frozen material.[13] The moisture existed largely
in the form of absorbed moisture due to the larger
internal surface area, and the part of the frozen mois-
ture decreased correspondingly with this new freez-
ing strategy.
Mass transfer resistance to vapor flow in freeze-
drying usually consists of two aspects, one from the
intrinsic resistance due to pore size, connectivity, and
tortuosity, etc. of materials,[41] and the geometric
resistance mostly due to height of thickness of prod-
uct.[42] The initially porous frozen material has dem-
onstrated to decrease the intrinsic resistance
effectively due to prebuilt porosity. It should be
noticed that the currently used sample was uncon-
tained without vials and side surface also involved
mass transfer. Since the porous frozen sample was
much higher than the solid one, the side surface
played a major role in vapor flow outside the sample.
That is most probably the reason why freeze-drying
time can be saved and the process can be enhanced
significantly using the initially porous frozen material.
Effects of operating temperature and pressure on
freeze-drying
Operating temperature and pressure are considered as
the two important parameters of a freeze-drying pro-
cess. It is essential to examine their effects on the pro-
cess, since the pore structures of the initially solid and
porous frozen materials are different, as observed pre-
viously. The same three pairs of the two different
samples were used in this part of the experiments
under sole radiation heating. Figure 7 shows the dry-
ing curves of the two samples at three different cham-
ber surface temperatures. As the temperature was
increased, the drying time decreased, as expected.
About 15.2% and 22.7% of the drying times were add-
itionally saved for the solid and porous frozen sam-
ples, respectively, when the temperature was increased
from 35  C to 45  C. The increase in chamber surface
temperature can indeed enhance the freeze-drying
process, as demonstrated by vial freeze-drying experi-
ments.[15] Under 45  C of the temperature, the drying
time of the porous sample was 2.4 h, 38.5% shorter
than that of the solid one. This again confirms the
advantageous effect of the porous frozen material over
the solid one in enhancing the freeze-drying process.
The same three sample pairs were also used to
inspect the effect of the chamber pressure on the
freeze-drying process. Figure 8 shows the drying
curves of the two samples at three different chamber
pressures under radiation heating. The chamber pres-
sure had little effect on the conventionally solid frozen
sample. This is most likely the result compromised
between the two effects. A relatively low chamber
pressure can benefit the mass transfer due to the
improved effective mass diffusivity of the material
being dried, but impair the heat transfer due to the
decreased effective thermal conductivity. The two
opposite effects counteracted each other under the
present operating conditions. For the porous frozen
sample, the case of 33 Pa attained 9% saving of drying
time. The beneficial effect of a higher chamber pres-
sure can be attributed to the existence of larger pre-
built pores. Although the porous frozen material had
a small mass transfer resistance, it largely increased
the heat transfer resistance due to the heat-insulated

Figure 9. Photos of two samples before and after freeze-drying. (a) solid sample before drying; (b) solid sample after drying at
35  C; (c) collapse of solid sample during drying at 50  C; (d) porous sample before drying; and (e) porous sample after drying
at 50  C.
effect of porous materials. Hence, a moderately high
chamber pressure is a favorable way to improve the
heat transfer and accordingly enhance the process for
this kind of the material. Compared with the chamber
surface temperature, the effect of the chamber pres-
sure can be neglected. Similar discussion can be found
elsewhere.[13]
Effects of heating modes on freeze-drying
The experimental results as seen in the last section
have proved that the appropriate increase in chamber
surface temperature can promote the freeze-drying
process and the change in chamber pressure had little
effect. It is necessary to further increase the tempera-
ture to improve the heat transfer of the process. This
part of the experiments was conducted with the same
sample pair under the same operating conditions
except that the temperature was increased from 45  C
to 50  C. The result showed that the solid sample col-
lapsed and the freeze-drying process failed. It was sur-
prising to find, however, that the porous sample
DRYING TECHNOLOGY 2133
always maintained its original structure and geometry
throughout the process. When the temperature was
further increased from 50  C to 55  C, the freeze-dry-
ing process still proceeded successfully for this kind of
the material. Photos of the two samples before and
after freeze-drying are shown in Figure 9. This indi-
cated that the porous frozen sample made with this
new freezing method had higher tolerable temperature
than the solid one during freeze-drying. Since the
solid frozen sample was prepared by direct freezing
without initial pores, sublimated vapor was difficult to
escape from inside out. This would increase the
internal pressure of the material being dried. When
the heat transported from outside in was more than
that needed for the phase change of ice crystals, the
excess portion would raise the sensitive heat of the
solid substrate and melt ice crystals. Once the solid
substrate loses its rigidity, collapse is inevitable to take
place during freeze-drying. In contrast with the solid
sample, the porous one had an intrinsic loose struc-
ture, allowing the phase-changed vapor of easy move-
ment in the prebuilt pore space and avoiding a vapor
2134 W. WANG ET AL.
Figure 10. Effects of combined heating on freeze-drying.
accumulation. This suggests that this kind of the fro-
zen material provides a wider range of operating tem-
perature and has better stability and adaptability
during freeze-drying.
To further enhance the freeze-drying process, com-
bined radiation and conduction heating was attempted
in this part of the experiments. The typical operating
conditions were still used and the temperature of the
thermal rod (Figure 3) was set to be 35  C that was
the same as that of the chamber. Experimentally
measured drying curves are shown in Figure 10. The
drying times were 3.3 h and 2.1 h, respectively, for the
initially solid and porous frozen samples, indicating
28.3% and 32.3%, respectively, beneficial effects com-
pared with the sole radiation heating. Moreover, the
drying time of the porous frozen sample was 36.4%
shorter than that of the solid one under the combined
heating. This once again demonstrates the superiority
of the porous frozen material over the solid one in
facilitating the freeze-drying process.
Conclusions
To shorten freeze-drying time, increase productivity,
and reduce process energy consumption, freeze-drying
of initially porous frozen material with prebuilt poros-
ity was proposed and investigated experimentally. A
heating unit of sample supporting pad was specially
designed to achieve the combined radiation and con-
duction heating. Soluble coffee was selected as the sol-
ute in aqueous solution to be freeze-dried and the
liquid nitrogen ice-cream making method was
employed to prepare the porous frozen materials.
Results clearly showed that the freeze-drying process
can be significantly enhanced using the initially por-
ous frozen material and 32.6% of the drying time can
be saved compared to the conventionally solid one
under the same tested operating conditions with the
radiation heating. The dried product from the porous
frozen material was found to have relatively a lower
residual moisture content than that of the solid one.
SEM images of the products revealed that the initially
porous frozen material had a continuous pore space
and pierced solid substrate with a loose and tenuous
structure. Such a frozen material with prebuilt poros-
ity and relatively a large surface area are quite helpful
for promoting the migration of sublimated vapor and
the desorption of bound moisture. Appropriately
increasing the chamber surface temperature was bene-
ficial to the freeze-drying process and changing the
chamber pressure had little effect on the process. The
porous frozen material had a wider range of operating
temperature. The freeze-drying process can be further
improved with combined radiation and conduction
heating and the drying time of the porous frozen sam-
ple can be 36.4% shorter than that of the solid one.
The proposed method is easily operable and highly
effective in improving the freeze-drying performance
and will have a significant impact on the trad-
itional process.
Disclosure statement
The authors declare no competing financial interest.
Funding
The authors sincerely appreciate the financial supports from
the National Natural Science Foundation of China (No.
21676042), the Liaoning Provincial Natural Science
Foundation of China (No. 201602167), and the
Fundamental Research Funds for the Central Universities of
China (No. DUT14RC(3)008).
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