2.1 Freeze Drying Under Vacuum or Atmospheric Pressure Vacuum freeze-drying is a well known process for highly heat-sensitive materials.. 2006 investigated the physical properties of va
Trang 1CHAPTER 2 LITERATURE REVIEW
The first part of review explains atmospheric freeze drying as a modifications
technique of the vacuum freeze drying process and covers relevant information on
modeling and experimental investigations This chapter also contains some basic
information on vibrating bed dryers along with a discussion of the vortex tube and
multimode heat transfer, which are applied in this research to develop a new integrated
atmospheric freeze drying system
2.1 Freeze Drying Under Vacuum or Atmospheric Pressure
Vacuum freeze-drying is a well known process for highly heat-sensitive materials
This method is used as a benchmark of product quality as it often gives the best quality
dried products For example, Marques et al (2006) investigated the physical properties
of vacuum freeze drying of tropical fruits and showed that this process gives high
quality products They also proved that vacuum freeze-dried (VFD) foods have high
porosity and low apparent density VFD also conserves color, flavor, and taste and
provides rapid rehydration
The main disadvantages of the freeze drying technique are its high fixed and operating
costs as demonstrated by Matteo et al (2003) The latter are due to the series of
energy-intensive operations involved in the process: freezing of the fresh product,
heating of the frozen foods at low temperature to induce sublimation, condensation of
water vapor and mechanical energy needed to maintain high vacuum Moreover,
vacuum operations are mainly carried out batchwise, which represent an additional
cost together with requirements of the apparatus operated under vacuum
Trang 2Liapis et al (2007) showed that the limiting step of the traditional freeze-drying
process under vacuum is the transfer of heat to the product due to the decrease in
thermal conductivity with decreasing the pressure of the freeze-drying chamber
Efforts have been made to improve the vacuum freeze drying method but none has
given economically satisfactory results as far as industrial applications are concerned
In particular, as disclosed in U.S Patent specification No 3,319,344, an attempt has
been made to fluidize the product using vibration to be freeze-dried under vacuum in
order to improve the heat and mass exchanges, but the major drawbacks resulting from
operating under vacuum are not overcome in this design
2.2 Atmospheric Freeze Drying – Fixed Bed Dryer
The early workers in atmospheric freeze drying, namely the works of Meryman (1959),
Lewin and Matelas (1962) and Woodward (1963), reported varying degrees of success
when fixed beds of desiccants were employed to freeze dry foods and other biological
materials in the absence of vacuum The potential for atmospheric freeze-drying was
demonstrated by Meryman (1959) He showed that the drying rate of a material
undergoing freeze drying is a function of ice temperature and the vapor pressure
gradient between the site of water vapor formation and the drying media, rather than
the total pressure in the drying chamber He invented process using either a fixed bed
water vapor adsorbent adjacent to the frozen product or a condenser in a stream of cold
air
However, drying periods were observed to be very long In order to reduce drying time,
other researchers focused attention on reducing product dimensions and on utilizing
fluidized beds through modeling and experimental investigations
Trang 32.2.1 Experimental studies of atmospheric freeze drying-fluidized bed dryer
A number of researchers have performed experimental studies on atmospheric
freeze-drying using a fluidized bed to investigate the freeze-drying performance on different size and
shape of products Quality parameters of the dried products have also been investigated
Malecki et al (1969) carried out atmospheric fluidized-bed freeze drying of apple juice
and egg white Their work supports the conclusion of Dunoyer and Larpusse (1961)
and Woodward (1963) that the drying rate in atmosphere can reach that under vacuum
if the particle size is sufficiently small However, Malecki et al (1969) found that for
apple particles the bed had to be at -34oC to prevent sticking and, at this temperature,
only 1 percent ice was sublimated per hour, which is extremely low and hence not
attractive from practical standpoint
Boeh-Ocansey,O (1985) conducted experiments to investigate the drying kinetics at
different product thicknesses, chamber temperature (-5oC, -10oC and -15oC) and using
different adsorbents on carrot slices (1.8 x 33, 3.4 x 27, 4.8 x 26 and 5.8 x 22 mm)
They carried out their experiments in a drying chamber consisting of a vertical
cylindrical column 10 cm in diameter and 100 cm high at atmospheric pressure They
obtained higher freeze drying rates with particles of activated alumina (0.4 mm
average diameter) than with activated carbon Their results showed that a higher drying
temperature (-5oC) is preferable to increase the drying rate They compared their
results with conventional vacuum drying and found that product thickness is more
sensitive in drying kinetics to a great extent in AFD then in VFD
An apparatus and a technique for spray freeze aqueous solution at very low
temperatures (-90oC) and for subsequent dehydration of the resulting frozen particles
Trang 4in a stream of cold, desiccated air was developed by Mumenthaler and Leuenberger
(1991).They investigated the influence of various operating variables on the drying
kinetics as well as the quality of the products They found a dry, stable and intact cake
of same shape and size as the original frozen mass, with sufficient strength to prevent
cracking and powdering or collapse They also observed uniform color and rapid
solubility upon reconstitution in water; increased inner surface area and good crystal
structure of the active substance They also reported an enhanced heat and mass
transfer between the circulating drying medium and the frozen sample
Alves-Filho et al (1998) used a fluidized bed as the first-stage freeze-dryer at
atmospheric pressure in a two-stage heat-pump system without adsorbent Adjusting
the heat pump dryer components to keep the air temperature below the drying
product’s freezing point controlled drying condition in the first stage fluid bed dryer
Their control strategy was based on the specific enthalpy curves developed by
Alves-Filho et al (1996) The product residence time in the first-stage dryer was selected to
reduce the moisture content to the critical values Afterwards the semi-dry product was
transferred to the second stage fluid bed to be dried at higher temperatures The
advantages of their two-stage system are that low-temperature drying reduces the
moisture content while maintaining product quality while higher-temperature drying
increases the overall heat-pump dryer capacity These authors reported excellent
quality of dried shrimp, apple pieces, carrot slices, etc., at a relatively high cost,
however
Donsi et al (2000) here demonstrated the feasibility of atmospheric freeze-drying for
shrimp and showed that the drying time is indeed an order-of-magnitude longer than
that for the vacuum process To shorten the drying time, part of the water was removed
Trang 5by osmotic dehydration Freeze-drying was carried out in a fluidized bed using a
mineral adsorbent (Zeolite particles 88 μm mean diameter) or an organic adsorbent
(wheat bran) The AFD dried shrimp dehydration properties that are similar to those
obtained in conventional freeze-drying The economics of the process were not
reported
Bussmann et al (2003) invented an apparatus for drying a product using a regenerative
adsorbent which can be carried out in an energy-saving manner According to their
invention, the product is dried by bringing it into contact with adsorbent, water being
taken up from product by the adsorbent Subsequently, the adsorbent is regenerated
with superheated steam
A detailed investigation was carried out by Matteo et al (2003) of atmospheric
freeze-drying in a fluidized bed mixed with different compatible adsorbent particles They
fluidized 1 cm long potato cylinders of various diameters with various particulate
adsorbents They measured higher heat and mass transfer coefficients compared with
vacuum freeze drying due to convective heat and mass transfer, which is absent in
VFD They showed that higher freezing (-10oC) and fluidized bed temperatures (-6oC),
compatible adsorbent (bran & bentonite), reduced sample size (6mm), smaller
adsorbent particles (400 μm), higher product/adsorbent weight ratio (1/8), moderate
regeneration temperature (60oC) are conducive to enhancing the dehydration rate
However, fluidization velocity had no significant effect on the dehydration rate Their
work also revealed that the size of the product is the key parameter in atmospheric
freeze-drying Finally, they showed that there is a significant reduction of the energy
cost relative to vacuum freezes drying due to the absence of a vacuum chamber and
ancillary equipment
Trang 6Stawczyk et al (2005) investigated the kinetics of atmospheric freeze-drying and
quality of apple dried cubes; all properties such as dehydration rate, shrinkage, color,
antioxidant content etc were reportedly very good They conducted experiments at
three different temperature increasing strategies; namely, constant inlet air temperature
(CT); inlet air at different temperature (DT) option and inlet air of ascending
temperature (AT) at a fixed airflow They found ascending inlet temperature condition
maintained a stable drying rate during the whole drying process to obtain an
economical AFD process and generally better quality dried product Their results
showed that AFD dried products at lower temperature (-10oC), had characteristics of
rehydration kinetics and hygroscopic properties similar to products obtained by
vacuum freeze drying They also found that AFD products are better than hot air-dried
products in terms of their anti-oxidative activity
Strommen et al (2005) carried out an experimental study of atmospheric freeze drying
of cod using a fluidized bed dryer coupled with a heat pump They found lower bulk
densities, higher rehydration, and light color, which is similar to vacuum freeze drying,
when dried at low temperature (-5oC) over a longer residence time of about 10 hours
They also noted that the typical specific moisture extraction rate (SMER) for
atmospheric freeze drying with heat pumps is in the range 4.6 to 1.5 kg of water per
kWh
Claussen et al (2005) analyzed the physical and quality parameters (color, water
content, rehydration properties and sorption isotherms) of traditional Norwegian
stockfish and compared them with atmospheric freeze dried (AFD) cod fillets
Sorption isotherms of several stockfish and AFD cod samples were measured with a
CIsorp water analyzer to determine the optimal storage conditions They found 4 and 5
Trang 7times higher rehydration index for atmospheric freeze dried cod compared with
naturally dried stockfish In addition they observed the atmospheric freeze dried fish
had brighter color than that of the naturally dried cod
The influence of AFD on the physiochemical properties, quality, and functional
properties (color, water content, bulk density, rehydration properties, sorption isotherm,
specific enzyme activity, solubility, protein denaturizing) of potato was investigated by
Claussen et al (2007) Their results showed that atmospheric freeze drying is a gentle
drying process than spray or vacuum freeze drying The solubility measurement gave
better results for AFD potato protein samples at pH between 3.5 and 5, while the
lowest value was obtained for spray dried samples over the whole pH range Moreover,
both enthalpy measurements and sorption isotherms indicate reduced protein
denaturizing of AFD samples, while specific enzyme activity was at same level for all
dried samples
Drying kinetics, sorption properties, shrinkage, and freezing point depression were
determined by Claussen et al (2007) in atmospheric freeze drying (AFD) of pieces of
apple, turnip cabbage, and cod They observed that drying at -5oC resulted in a greater
shrinkage than drying at –10oC Claussen et al (2007) also carried out measurement of
the physical properties of atmospheric freeze-dried cod and turnip cabbage True
density, apparent density and pore size distribution were measured using helium
pycnometry, geopycnometry and light microscopy They concluded that thawing
during drying and product shrinkage affects the drying rate and the diffusion of water
leading to poor product quality of the end product
Trang 82.2.2 Modeling of atmospheric freeze drying
Heldman et al (1974) proposed a simple mathematical model and validated it with
their results experimentally They concluded that the rate of drying, as expected, is
higher for smaller particles and by increasing the surface mass transfer coefficient
Since the drying kinetics for AFD are determined by internal resistance to heat and
mass transfer Their conclusion about effect of external mass transfer coefficient is
surprising
Boeh-Ocansey et al (1983, 1985) reported measurements of kinetics of ice sublimation
in vacuum and in a fluidized bed drying system under atmospheric condition They
showed that for ice sublimation the recommended partial vapor pressure, temperature
of drying chamber and relative humidity of air are: 4.58 mm Hg, approximately 0oC
and below 20 ppm, respectively Since there is freezing point depression with soluble
components in drying material is 0oC really the optimum temperature
A further kinetics study of ice sublimation in a fluidized-bed dryer operating under
atmospheric conditions was reported by Boeh-Ocansey and Wachet (1986)
Mathematical expressions were formulated to account for mass variation and
dimensions of ice samples during sublimation They investigated the influence of
chamber temperature and air flow rate on sublimation and showed that sublimation of
ice was obtained at drying chamber temperatures greater than 0oC (7.6oC maximum)
They also noted that there exists a correlation ice sublimation temperature and the
temperature of the fluidized bed Ice sublimation temperature can be predicted
accurately for a given fluidized-bed temperature Finally they showed that the kinetics
of ice sublimation was regulated by the expression: M/M0 = (1 – t/tT)2 where M and t
Trang 9represent mass of product and time, respectively Subscript o and T stand for initial
and final time, respectively
Wolf and Gilbert (1990b) proposed a model for atmospheric freeze-drying in a
fluidized bed of a particulate adsorbent (starch) incorporated in different mass ratios
Their model was based on uniformly retreating ice front (URIF) They found spherical
regeneration temperature of adsorbent (50oC) are most advantageous for drying They
also concluded that a mass fraction between the mass of water sublimated and the mass
of adsorbent used (mw / ma ), of the order of 0.10, or even 0.05 at higher temperatures,
seems satisfactory They validated their model with experiments with potato
parallelepipeds of different thicknesses (2, 3 & 5 mm)
Joseph et al (1996) presented two sets of nonlinear coupled heat and mass transfer
models to describe the absorption and desorption process Model I describes the
temperature and moisture distribution in a porous medium with a moving evaporation
front They reported that in the two phase system with moving boundary condition, the
rate of movement of the evaporation front decreased with deepening of the evaporation
front in the porous body They showed that the higher the value of nondimensional
vaporization parameter γ, the slower is the movement of the evaporation front The
temperature decreased and the moisture content increased as the nondimensional
vaporization parameter γ increased In model II they described a set of simultaneous
heat and mass transfer equations describing moisture adsorption during the steeping of
barely kernels
Trang 10A study of freeze drying, by immersion in an adsorbent medium both at atmospheric
pressure and under vacuum was carried out by Lombrana and Villaran (1996) They
used spherical moistened particles of commercial cereal food paste as a drying product
They employed zeolite as adsorbent particles (0.63g/cm3 density, diameter 0.7 mm)
with adsorbent to product mass ratio of 10:1 in a fluidized bed dryer They evaluated
the effect of pressure and temperature on the drying kinetics through a model by
considering a uniformly retreating ice front in spherical geometry Their model
calculated the pressure and temperature at the sublimations front in terms of the
without adsorbent, were also investigated to analyze the possibility elimination of
adsorbent when vacuum was employed They found that values of total time and
shrinkage varied from 400 to 390 min and from 0.567 to 0.573, respectively, they
concluded that adsorbent usage is recommended Also they proposed some operational
strategies which can reduce the process duration without damage to product quality
First step starts at atmospheric pressure and a temperature of -10oC followed by a
second step at where low pressure with temperature in the range 0oC to 15oC and a
third step at atmospheric pressure with temperature below 15oC
Lombrana and Villaran (1997) developed a mathematical model for AFD in a fluid bed
dryer They evaluated the effect of pressure and temperature on the drying kinetics
through a model by considering a uniformly retreating ice front in spherical geometry
Their model calculated the pressure and temperature in the sublimations front in terms
of the product moisture Good agreement was found between predicted and
experimental results