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STUDY OF DRYING CHARACTERISTICS OF GRANULAR MATERIAL

Conference Paper · November 2013

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 Paper - 69

STUDY OF DRYING CHARACTERISTICS OF GRANULAR MATERIAL

SirishaNallakukkala1*, Appala Naidu U 2, ChandrikaV1, Srikanta Dinda2
1
Department of Chemical Engineering, BVRIT, Narsapur, Medak Dist. -502313, A.P, India.
2
Department of Chemical Engineering, BITS Pilani - Hyderabad Campus, Hyderabad – 500078, A.P, India
*
Corresponding Author’s E-mail: sirisha.nallakukkala@gmail.com

ABSTRACT:

Drying plays an important role in the field of pharmaceutical, food and paper industry. In this study the drying
characteristics were studied for a pharmaceutical granular material in a fluidized bed dryer. The experiments were
conducted in a pharmaceutical industry and the data was analyzed to observe the rate of drying and critical moisture
content. A mathematical model is also developed to predict the drying time. The developed model is well suited to
know the drying time.

Key words: Drying, Fluidization, Critical moisture content, Drying rate, Mathematical model.

INTRODUCTION:

DRYING:

Drying involves the simultaneous transfer of heat, mass and momentum in which heat penetrates into the product
and moisture is removed by evaporation into an unsaturated gas phase [1]. This process is often used as a final
production step before marketing or packaging products. Drying offers the mitigation of the microbial growth in the
product, and improves structural strength and product quality. For drying the wet materials, various kinds of drying
equipments, such as tray dryer, fluidized bed dryer (FBD), Rotary dryer, spray dryer, spin flash dryer and etc, are
available in industrial practices. For enhanced drying rates, convective air is generally utilized to instigate thermal
and moisture gradients within the porous medium. In bio-products like food, grains,
and pharmaceuticals like vaccines, the solvent to be removed is almost invariably water.

FLUIDIZATION:

Fluidization is a process whereby a granular material is converted from a static solid state to a dynamic fluid state
[2, 3]. This process occurs when a fluid (liquid or gas) is passed up through the granular material. When a gas flow
is introduced through the bottom of a bed of solid particles, it will move upwards through the bed via the empty
spaces between the particles. At low gas velocities, aerodynamic drag on each particle is also low, and thus the bed
remains in a fixed state. Increasing the velocity, the aerodynamic drag forces will begin to counteract the
gravitational forces, causing the bed to expand in volume as the particles move away from each other. Further
increasing the velocity, it will reach a critical value at which the upward drag forces will exactly equal the
downward gravitational forces, causing the particles to become suspended within the fluid. At this critical value, the
bed is said to be fluidized and will exhibit fluidic behavior. By further increasing gas velocity, the bulk density of
the bed will continue to decrease, and its fluidization becomes more violent, until the particles no longer form a bed
and are “conveyed” upwards by the gas flow.

FLUIDIZED BED DRYER (FBD):

Fluidized bed processing involves granulation and drying of particulate materials. It is ideal for a wide range of both
heat sensitive and non-heat sensitive products. Uniform processing conditions are achieved by passing a gas (usually
air) through a product layer under controlled velocity conditions to create a fluidized state. In fluidized bed drying, a

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stream of heated air is used to fluidize the solid particles. The wet or granulated particles are thus dried. As the name
indicates, the drying in a FBD is done by fluidization of the particles by heated stream of fluid usually air.

HALOGEN MOISTURE ANALYZER:

Halogen moisture analyzer consists of two important components: a balance and a heater. The sample is placed in
the moisture analyzer and the balance captures the initial weight. An infrared energy heater is used to heat the
sample. During the test the balance records the weight. When the sample no longer loses weight the instrument shuts
off the heat and uses the final weight to calculate moisture. Halogen moisture analyzer is used to determine the %
moisture content [4].

LOSS ON DRYING (LOD):

LOD is laboratory method of measuring high level moisture in solid or semi-solid materials. In this technique a
sample of material is weighed, heated in an oven for an appropriate period, cooled in the dry atmosphere and then
reweighed. If the volatile content of the solid is primarily water, the LOD technique gives a good measure of
moisture content. These analyzers incorporate an electronic balance with a sample tray and surrounding heating
element. Under microprocessor control the sample can be heated rapidly and a result computed prior to the
completion of the process, based on the loss rate, known as a drying curve [5].

PROCESS DESCRIPTION:

API ( Active Pharmaceutical Ingredient) is a substance used in a finished pharmaceutical product (FPP), intended to
furnish pharmacological activity or to otherwise have direct effect in the diagnosis, cure, mitigation, treatment or
prevention of disease, or to have direct effect in restoring, correcting or modifying physiological functions in human
beings. The API raw material undergoes the following sequence of operations:
Milling Granulation Fluidization& Drying Tippling Sifting Blending
All the operations are carried out in a controlled processed area known as module. The raw material that is received
from the dispensary is initially milled in a multi mill and is then granulated in a Rapid Mixer Granulator (RMG).
The sample was collected from RMG and its initial moisture content was measured. Then the material was fed into
the Fluidized Bed Dryer (FBD) and at regular interval of two minutes its moisture content is analyzed using Halogen
moisture analyzer.

RESULTS AND DISCUSSION:

Before making the tablets, it is necessary to add the water to the API drug to mix the additives to the drug and later
the moisture from the drug has to be removed. It can be done using drying method. To find the drying
characteristics, the drying operation was carried under semi batch mode. Dry air at a temperature of 90 oC was
continuously fed to the FBD. The raw material of 274 kg was initially mixed with water (say 5.18%) that is the toal
mass is the sum of solid material and the amount of water added (289 kg’s). The %moisture content was measured
at a regular interval of 2 min. using Halogen moisture analyzer. Results are shown in Table 1. The result shows that
the % moisture content decreases with time.

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 Table 1: Values of Moisture content, Air temperatures and Drying Rates

Temperature (0C) % moisture Weight (kg) Loss on Drying rate (N)

Time
(X) in 289 kg moisture removed Drying (kg/min. m2)
(min) Inlet Outlet
of Material from 289 kg (LOD) kg
0 89 38 5.18 14.97 0 10.56
2 90 36 4.5 13.00 1.97 10.6
4 91 33 3.78 10.92 4.05 10.06
6 90 29 3.33 9.62 5.35 5.78
8 89 28 2.90 8.38 6.59 4.0
10 89 27 2.37 6.84 8.13 3.8
12 89 27 2.11 6.09 8.88 3.78
14 89 28 1.81 5.23 9.74 3.76
16 89 27 1.48 4.27 10.7 3.54
18 89 30 1.25 3.61 11.36 3.52
20 89 33 1.16 3.35 11.62 3.41

Weight of dry solid (Ss) = 274 Kg

Weight of wet solid = 289 Kg
Amount of moisture present = (289-274= 14.97 Kg)
Moisture removed from 289 Kg of wet solid is 14.97-3.35 = 11.62 Kg.

Plot between %moisture content and drying time is drawn and we find the slope at every time value in Figure 1. The
obtained value of the slope is dX/dt. After calculating the drying rate values at every point, we obtain a plot between
drying rate (N) and %moisture content is shown in Figure 2. The “critical moisture content” (Xcr) is obtained from
the plot at the point B.

The drying rate is calculated using the following formula: Drying rate (N) = - ((Ss/A) dX/dt) where
Ss = weight of dry solid, A = drying area, dX/dt = slope calculated from the plot between %moisture content and
time.

Figure 2 shows the variation of drying rate with %moisture content. Initially as the moisture content decreases, the
drying rate increases. The drying rate starts declining with the decrease in moisture content and attains a constant
value for a set of moisture retained values (constant rate period). The point where the constant rate period end and
the falling rate period start is called the “critical moisture point” (X cr). At this point there is insufficient water on the
surface to maintain a continuous film of water. The entire surface is no longer wetted and the wetted area
continuously decreases. After the critical moisture point, a sharp fall in the drying rate is observed. This is called the
“falling rate period”. The amount of moisture removed in this period may be relatively small but time required is
long. The “critical moisture content” (Xcr) is obtained from the plot and it appears to be 1.68 at the point B.

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 Figure 1: Plot between drying time and Figure 2: Plot between %moisture
%moisture content content and Drying rate (N)

MODEL DEVELOPMENT:

A mathematical model is developed based on the fundamentals of multiple regression analysis using Minitab
statistical software to predict the time required for drying based on the input parameters like Inlet temperature ( Ti),
outlet temperature (To) and %moisture content (%X) [6, 7].

Calculated Drying time, tcal (min.) = -2028 + (45.6613*Ti) + (0.1766*To) - (-5.9283*%X) - (-0.2538*Ti*Ti) +
(0.0113*To*To) + (0.6832*%X*%X) - (-0.0047*Ti*To) + (-0.1027*To*%X).

Plot between calculated drying time and experimental drying time is drawn in Figure 3 and it’s found to be a linear
relation with R2 value of 0.99. The developed model is valid for this particular drug only.

Figure 3: Plot between Experimental and Calculated drying time

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 CONCLUSION:

The Drying rate curves have been generated for the studied product and the critical moisture points have been
identified for the corresponding batch of material.We have seen from the study that as the time increases, the
moisture content decreases gradually. From the observed data a regression model is developed to know the drying
time for this particular granular material. The developed model is well suited to find the drying time.

REFERENCES:

[1]. Camelia Gavrila, Adrian Gabriel Ghiaus, Ion Gruia, Heat and Mass Transfer in Convective Drying
Processes, Excerpt from the Proceedings of the COMSOL Conference 2008 Hannover.
[2]. J. Duran, Sands, Powders, and Grains:An Introduction to the Physics of GranularMaterials (Springer, New
York, 1997).
[3]. Daizo Kunii & Octave Levenspiel (1991) Fluidization Engineering, 2nd ed., John Wiley & Sons: New
York, NY
[4]. J Mendham, R C Denney, J.D.Barnes, M.J.K. Thomas Vogels Textbook of Quantitative Chemical
Analysis, (6th Ed, pp122, 241.
[5]. S.F. Edwards, in Granular Matter: An Interdisciplinary Approach (Springer, New York,1994), pp. 121–
140.
[6]. S. Tsivilis and G. Parissakis, A mathematical model for the prediction of cement strength, Cement and
Concrete Research, Vol. 25, No. 1, pp. 9-14.1995.
[7]. Sedat Akkurta, Gokmen Tayfurb, Sever Can, Fuzzy logic model for the prediction of cement compressive
strength, Cement and Concrete Research 34 (2004) 1429–1433.

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