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Alternative drying of sodium sulfate decahydrate (Na2SO 4·10H2O) with

microwave energy

Article · January 2006

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(Reference: B. Ozalp, S. Tarhan, A. Seyrankaya, E. Kaya,"Alternative Drying of Sodium Sulfate Decahydrate
(Na 2 SO 4 .10H 2 O) with Microwave Energy", Proceeding of XXIII International Mineral Processing Congress (IMPC),
eds:G. Onal, N. Acarkan, M.S. Çelik, F. Arslan, G. Ateşok, A. Güney, A.A. Sirkeci, A.E. Yüce, K.T. Perek, 3-8
September 2006, Istanbul, Turkey, v:2, p:1682-1686.

Alternative Drying of Sodium Sulfate Decahydrate (Na 2 SO 4 ·10H 2 O) with

Microwave Energy

B. Ozalp, S. Tarhan, A. Seyrankaya and E. Kaya

Dokuz Eylul University, Mining Engineering, Mineral Processing Division, Bornova, Izmir, Turkey

ABSTRACT: The anhydrous sodium sulfate (Na 2 SO 4 ) is produced from the sodium sulfate decahydrate also
called mirabilite (Na2 SO4 ·10H2 O) by removing its crystal water. This provides advantages in reducing the
transportation costs and in uses in industry. Mirabilite starts to dissolve in its crystal water (i.e. crystal structure
decomposes and starts to release its crystal water) above 32.4 0C. In industrial applications, to dry off the crystal
water, sodium sulfate decahydrate is heated in steam tube rotary or fluidized bed dryers with air above about
150ºC. However, drying in rotary dryers is slow due to limitations in mixing and low gas temperatures.
Fluidized bed dryers cause dusting and powder formation as a result of attrition caused by collision of particles in
the bed.
In this investigation, microwave energy has been considered as an alternative approach to solve the problems
with current drying processes. With this alternative dehydration process, anhydrous sodium sulfate (Na 2 SO 4 ) has
been produced successfully from the sodium sulfate decahydrate with no damage to the sodium sulfate crystals.
Comparative results of dehydration of sodium sulfate decahydrate in the oven and with microwave energy will be
presented as well.

1 INTRODUCTION Although there are several production methods, a

Sodium sulfate decahydrate (Na 2 SO 4 ·10H2 O) is
produced from naturally occurring sodium-sulfate-
bearing brines or crystalline evaporate deposits that
are located in China, Canada, Spain, Mexico,
Turkey, and the United States, and as a byproduct
from different chemical processes, such as ascorbic
acid, battery acid recycling, boric acid, cellulose,
chromium chemicals, lithium carbonate, rayon,
resorcinol, and silica pigments (Kostick, 1997).
Sodium sulfate, also known as disodium sulfate
(Na 2 SO 4 ), is an inorganic chemical and widely used
in cellulose-fiber industry and in the production of
glass and detergents.
In the sodium sulfate-water system, the solid
goes through a phase transformation (peritectic
point) at 32.4°C. Above this temperature, the
anhydrous thenardite (Na 2 SO 4 (s)) crystallizes from
the saturated solution, and below it, mirabilite
(Na 2 SO 4 ·10H 2 O(s)), also called Glauber’s salt.
generalized production flowsheet of the process
starting from sodium sulfate solution is presented in
Figure 1.
Drying, including water and solvent removal, is
one of the most energy intensive processes in industry.
A typical objective in drying is to quickly remove the
water without degradation in product quality. Energy
transfer as heat from the surrounding environment to
the wet solid can occur via convection, conduction,
or radiation and in some cases as a result of a
combination of these effects (Haque, 1999). The
drying and dehydration of the decahydrate is carried
out more frequently in air, spray, fluidized bed,
rotary dryers where the crystals are dehydrated into
anhydrous sodium sulfate at 150°C to 450ºC
(Garrett, 1996; Plessen, 1993). All these dryers have
some disadvantages. In rotary dryers, gas-solid
mixing is not good and gas temperatures are low,
resulting in comparatively long drying times. In
fluidized bed dryers, the degree of particle breakage,
fine powder formation and dusting of the product is
quite high as a result of attrition caused by collision
of particles (Jones, 1992; Kocakusak et al., 1998).
With this study a new drying technique is presented:
drying with microwaves (MW).
Figure 1. Simplified flowsheet of the Na 2 SO 4
production process
Drying techniques are cornerstones of many
industrial applications and also have undergone
dramatic developments over the last 30 years. In
recent years, microwave drying is recognized as
having a demonstrated potential for the removal of
water from the industrial products, such as
agricultural, chemical, mineral processing and food
product, textile, paper, lumber and many more
(Jones, 1992; Khraisheh et al., 1997; Kingman and
Rowson, 1998).
Microwave heating occurs somewhat differently
from conventional heating. MWs propagate through
the materials and the accompanying transport
processes result in dissipation of electric energy into
heat, which lead to the term ‘volumetric heat
generation’ due to MW radiations (Jones, 1992).
Volumetric power absorption and the rate of heat
generation depends upon the intensity and frequency
of the field as well as on the dielectric properties of
the material. MWs are widely preferred over
conventional heating mainly for shorter processing
times. During conventional heating the heat is
radiated from the burner to the surface of the
material and the material is heated due to surface
heat flux whereas during MW heating, the material
dielectric loss is responsible to convert electric
energy into heat evenly distributed within the entire
volume (Basak and Priya, 2005). The unique heating
mechanisms of microwaves permit dramatic energy
savings in many instances, as well as providing
competitive benefits (Kingman and Rowson, 1998;
Haque, 1999).
In this paper, the results of the experimental work
to dry off the crystal water from the sodium sulfate
decahydrate crystal using microwave energy are
presented.
2 EXPERIMENTAL
In this study, batch conventional drying
experiements were performed using a thermostatic
stagnant air oven (Nuve, FN 500). It was operated
at different temperature levels of 100, 150, and
200°C. In addition, a domestic microwave oven
(Premier, PMO-20) with a maximum output power
of 800 W at 2450 MHz and six different microwave
output powers of 136, 168, 264, 440, 616 and 800 W
was used for the drying experiments.
In the experiments, the used sodium sulfate
decahydrate (containing 55.91 w% H 2 O, 44.09 w%
Na 2 SO 4 ) with 0.5 w% free water was obtained from
Alkim Alkali Kimya Anonim Sirketi. The
dehydration experiments were performed with 12.5,
25, and 50 g samples. A new sample was used at
each microwave output power selected for drying.
The amount of water removal from the samples
was calculated from the decrease in weight during
heat treatment. Each experiment was performed in
triplicate according to a preset microwave output
power and time schedule. Moisture loss was
recorded by taking 10 grams of samples from the
microwave and placing them in the desiccator for an
hour.
The temperature of the irradiated sample was
measured by inserting a K-thermocouple (Hanna
instruments, model HI 93551) into the sample
immediately after turning of the microwave power.
An average bulk surface temperature of each sample
was reported in this study. Although microwaves
directly heat the moisture in the samples instead of
sodium sulfate powder which is transparent to
microwaves, it is not possible to conveniently
measure the temperature of the water only. It is
highly likely, that the moisture in the sample
acquired significantly higher ‘peak’ temperatures,
especially at the higher output power rates.
The thermocouple was calibrated using a mercury
thermometer and a thermostatic water bath at
different water temperatures.
3 RESULTS AND DISCUSSION and transport of water. A maximum surface
Sodium sulfate decahydrate powder containing temperature of about 850C was measured during
about 0.5% surface moisture was dried in the drying of samples. The final surface temperatures of
conventional oven at three different temperatures the samples when all the water was removed were
and in the microwave ovens at three different energy about 420C at different microwave powers.
levels. Drying of the sodium sulfate decahydrate is
dictated by the rate of moisture removal and the rate 60
of sodium sulfate decahydrate conversion to sodium
sulfate anhydrate. 50 136 W
440 W

Moisture, %
3.1 Hot air drying 40 800 W

Drying behavior of the sodium sulfate

30
decahydrate powder was investigated in the hot air
drying oven at tempreatures of 100, 150 and 2000C. 20
The results of hot air drying tests were presented in
Fig. 2 as water removal versus time. Obviously, as 10
the temperature of the oven increased, the time
required to achieve dehydration time decreased. In 0
each plot, the major amount of the drying occurred 0 5 10 15 20 25 30
in the range of the falling rate period after the short Drying time, min.
constant rate period. Figure 3. Drying curves of 25g sodium sulfate
decahydrate samples by microwaves at different
60 power levels

50
100oC 100
Moisture, %

40 150oC 136 W
200oC 80 440 W
Temperature, C

800 W
0

30
60
20

10
40

0 20
0 100 200 300 400 500

Drying time, min. 0

Figure 2. Drying curves of 25g sodium sulfate
decahydrate samples by hot air oven at three
different temperatures
3.2 Microwave drying
In these experiments, a solid sample of sodium
sulfate decahydrate with very minor amounts of
adsorbed water was used. The effect of changing
the power output in the microwave oven on the
moisture content curve of 25 g sample is presented
in Fig. 3 and surface temperature of the samples
measured at different times is presented in Fig. 4.
The sample temperatures increased to a maximum
and then their temperatures dropped indicating the
removal of the moisture. The observed initial
acceleration of drying may be caused by an opening
of the physical structure allowing rapid evaporation
0 5 10 15 20 25 30
Drying time, min.
Figure 4. Effect of power-dependent microwave
absorption on the heating of sodium sulfate
decahydrate crystals
The effect of sample weights (12.5, 25, 50 g) on
the drying process was also investigated at constant
power output (800 W) and the results are presented
in Figures 5 and 6.
The results show that the drying times of the 12.5
g and 25g samples were shortened substantially
compared to 50 g sample. It is obvious that a
material with higher weight would have a large
moisture content, thus, a much longer drying time.
In general, with increasing sample weight, the
sample bed thickness would also increase, affecting Table 1. Comparison of complete drying times with
the water removal rate which would be slower with hot-air and microwave ovens (25g samples)
increasing bed thickness. Complete drying time
Drying method
(minutes)
100 Hot-air oven
12.5 g 1000C 480
80 25 g 0
150 C 240
Temperature, 0C

50 g
2000C 120
60 Microwave oven
136 W 25
40 440 W 7
800 W 5
20

0 3.4 Economics of microwave drying

0 1 2 3 4 5 6 7 8

Drying time, min. With conventional system, to produce 1,000 Kg

Figure 5. Changes on surface temperatures with
varying weights of sodium sulfate decahydrate
samples at constant microwave power output of 800
W steam and 37 kWh electrical energy are used
60
50
Moisture, %
of anhydrous sodium sulfate (Na 2 SO 4 ) from natural
glauber salt, about 2,300 Kg raw salt, 190 Kg lignite
coal, (with 3,750 Kcal/Kg calorific value), 1,650Kg
(Civelekoglu et al., 1987).
The economics of a microwave drying system can
be divided into capital and operating costs which are
12.5 g presented in detail in Table 2 (Schiffmann, 1995).
25 g In general, for drying systems, 1kW of microwave

40 50 g or dielectric energy will remove (i.e. dry) about

30
20
10
0 employed along with a conventional form of heat
0 1 2 3 4 5 6 7
Drying time, min.
Figure 6. Drying curves for varying weights of
sodium sulfate decahydrate samples by microwaves
at constant power output of 800 W
3.3 Comparison of the both drying methods
In general, drying times for samples are
substantially higher in the hot air oven than in
microwave oven. This is because the mass transfer
within the sample is rapid during microwave heating
because heat is generated within the sample, creating
a large vapour pressure difference between the
centre and the surface of the product. The increase
in microwave power significantly reduces the drying
time of the sodium sulfate decahydrate crystal water.
The comparison of the drying results are presented
in Table 1.
1.36Kg (3.0Ib) of water per hour.
The initial capital cost requirement for a
microwave system may become prohibitive, if the
amount of water to remove is very large and only
microwave system is employed for water removal.
However, the microwave energy system can be
8 energy to remove only the residual moisture from
the material, and in this case, at a much reduced
capital cost.
The cost of tubes varies greatly, depending upon
the microwave unit output power. In addition, the
water requirements for cooling are directly
proportional to the output power of the tube; for
example, a 6-kW magnetron at 2,450 MHz requires
5.7 lt/min (Schiffmann, 1995).
Similarly, using microwave energy to produce
1,000 Kg of anhydrous sodium sulfate (Na 2 SO 4 )
from natural glauber salt, about 1273 Kg of water
needs to be removed (i.e. dried). This requires a
total of 936 kWh of energy. This can be done with
seven 6-kW microwave oven working 24 hours a
day. The cost of one microwave oven (6kW x
$8000/kW) is about $50,000, totaling $350,000 for 7
ovens. The other capital cost items are applicator
for $70,000 cooling for $35,000, power transmission
for $18,000, instrumentation for $7,000. The total
 cost would add to $500,000. Operating cost items Publications, No 17, (1987) (Turkish).
are about $100 for electricity, $30 for tube
Garrett, D.E., Sodium Sulfates. Van Nostrand
replacement and $60 for maintenance, totaling $190 Reinhold, New York (1996).
to produce 1000 Kg of anhydrous sodium sulfate
(Na 2 SO 4 ). The operating cost to dry water is Haque, K.E., Microwave energy for mineral
calculated as $0.15/Kg. treatment processes- a brief review. International
Journal of Mineral Processing 57, 1-24 (1999).
Table 2. Capital and operating cost items for a Jones, P.L., Electromagnetic wave energy in drying
microwave energy drying system processes. Drying’92, Pt. A., A.S. Mujumdar, ed.,
Elsevier, Amsterdam, 114-136 (1992).
Capital Cost
Khraisheh, M.A.M., Cooper, T.J.R., Magee, T.R.A.,
Generator (including $4000-$9000/kW
Microwave and air drying І. fundamental
wave guides and
considerations and assumptions for the simplified
controls)
thermal calculations of volumetric power
Applicator 20% of generator
adsorption. Journal of Food Engineering 33, 207-
Cooling system (6kW) 10% of generator
219 (1997).
(350Kg water/hr needed)
Power transmission 5% of generator Kingman, S.W., Rowson N.A., Microwave
Instrumentation and 2% of generator treatment of minerals-a review. Minerals
control Engineering 11(11), 1081-1087 (1998).
Operating Cost Kocakusak, S., Koroglu, H. J., Tolun, R., Drying of
wet boric acid by microwave heating. Chemical
Electrical Energy $0.1/kWh Engineering and Processing 37, 197-201 (1998).
Tube replacement $0.06/kWh
Tube cost $3500 Kostick, D.S., Sodium Sulfates, U.S. Geological
Tube life 6000 hr survey-minerals information (1997).
Maintenance, year 2% of capital Plessen, H.V., Ullmann’s Encyclopedia of Industrial
Chemistry, Vol. A 24, 355-367 (1993).
Schiffmann, R.F., Microwave and dielectric drying,
4 CONCLUSIONS in. Mujumdar, A.S. (Ed.), Handbook of Industrial
Drying. Second Ed., vol.1, Marker Dekker Inc.,
In this investigation, sodium sulfate decahydrate
New York, pp.345-372 (1995).
crystals have been dehydrated using conventional
hot air and microwave ovens. The results show that Tarhan, S., Drying of Sodium Sulfate Decahidrate
the sodium sulfate decahydrate (Na 2 SO4 ·10H2 O) with Microwave Energy, B.S: Thesis, Dokuz
powder can be successfully dried using microwave Eylul University, (2005) (in Turkish).
energy to replace steam tube rotary or fluidized bed
driers that are currently used in the industry to
remove the excess moisture from the the sodium
sulfate decahydrate powder.
In general, drying times for samples are
substantially higher in the hot air oven than in
microwave oven. The increase in microwave power
significantly reduced the drying time of the sodium
sulfate decahydrate crystals.

5 REFERENCES
Basak, T., Priya, A. S., Role of metallic and ceramic
supports on enhanced microwave heating
processes. Chemical Engineering Science 60,
2661–2677 (2005).
Civelekoglu, H., Tolun, R., and Bulutcu, N.,
Inorganic Technologies, ITU Vakfı, Book

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