1.

0 Abstract

The objectives of this experiment was to study the operation of a packed bed distillation column
by verifying the Rayleigh Equation. Another objective is to obtain the T-x data under total reflux
condition at steady state and compare it with the theoretical value. Being able to operate the
column under total reflux condition and to calculate the minimum number of theoretical stages
using Fenskes equation is also one of the objectives to be fulfilled when conducting this
experiment. Being able to operate the column under any desired reflux condition and calculating
the theoretical number of stages using Mc-Cabe Thieles method is an objective to be achieved in
the experiment. The final objective in conducting this experiment is to calculate the height
equivalent to theoretical plate (HETP) for known packed height. The experiment first began with
plotting a graph of RI vs x, by preparing different concentration of methanol by diluting it with
distilled water. The x values ranges from 0 to 1, where at x=0.1 , the volume of water is 9 ml and
the volume of methanol is 1 ml. After collecting the experimental values of the refractive indices
based on the experimental value of the methanol solution, the packed bed distillation column was
switched on. It started with the total reflux condition with the cyclic timer set 999 seconds, then
the experiment was continued with desired reflux condition with the cyclic timer set at 5
seconds. The temperatures were set at 85C, 90C, and 95C. The feed and the distillate sample
was collected at these temperatures. After these samples were cooled down to room temperature,
the refractive indices were measured. For total desired reflux: 85C with RI F = 1.331 and RID =
1.3290; 90C with RIF = 1.334 and RID =1.3295, and 95C with RIF =1.333 and RID = 1.3250.
For desired reflux condition: 85C with RIF = 1.3285 and RID = 1.3340; 90C with RIF = 1.33 and
RID =1.334, and 95C with RIF =1.330 and RID = 1.3290.

1
2.0 Introduction

In chemical processing, a packed bed is a hollow tube, pipe, or other vessel that is filled with a
packing material. The packing can be randomly filled with small objects like Raschig rings or
else it can be a specifically designed structured packing. Packed beds may also contain catalyst
particles or adsorbents such as zeolite pellets, granular activated carbon.

The purpose of a packed bed is typically to improve contact between two phases in a chemical or
similar process. Packed beds can be used in a chemical reactor, a distillation process, or a
scrubber, but packed beds have also been used to store heat in chemical plants. In this case, hot
gases are allowed to escape through a vessel that is packed with a refractory material until the
packing is hot. Air or other cool gas is then fed back to the plant through the hot bed, thereby
pre-heating the air or gas feed.

Packed column are often used for distillation when the separation is relatively easy and the
required column diameter is not very large. The column height is generally based on the number
of theoretical plates and the height equivalent to theoretical plate (HETP).
For the calculation of height equivalent to theoretical plate (HETP):

Where Z and Nt are packed height and number of theoretical plates respectively. For simple
batch distillation process, initially the still is filled with F moles of feed with xF as the mole
fraction of the more volatile component. Let at any moment the number of moles of liquid in the
still be B having a mole fraction x of the more volatile component (i.e A) and let the moles of
accumulated condensate be D. Concentration of the equilibrium vapor is y*. Over a small time,
the change in the amount of liquid in the still is dB and the amount of vapor withdrawn is dD.
The following differential mass balance equations may be written:

2
3
The above equation is more convenient form of Rayleigh equation. Batch distillation with
only a single still does not give a good separation unless the relative volatility is very high.
To obtain product with a narrow composition range, a rectifying batch still is used that
consist of a reboiler, a rectifying column, a condenser, some means of splitting of a portion
of condensed vapor or distillate as reflux and the receiver. The operation of a batch still and
column can be analyzed using the same operating line equation as for the rectifying section
of the continuous distillation:

4
Since the slope of the operating line is R / (R+1), the slope increases as the reflux increases,
until when reflux is infinite. Under total reflux slope is 1. The operating line then coincides
with the diagonal. The number of plate is minimum at total reflux. Minimum number of
plates required can be calculated from the terminal concentration of xB and xD based on the
relative volatility of the components , which is defined in terms of equilibrium
concentrations:
Minimum number of theoretical plates required:

The above equation is known as Fenskes eqn. The final ratio does not change much over the
range of temperature encountered in a typical column, so the relative volatility is taken as
constant.

Application of Packed Bead Column in the Industry

Packed column bed distillation is used to enhance contact between vapor and liquid instead
of trays packing. It is more preferable to use packed bed column over tray packing when the
most cost-efficient distillation column when the diameter of the column is less than 0.6 m.
Packed bed column also has the advantage of a smaller pressure drop and is, therefore,
useful in vacuum fractionation. Not only that, packed bed column is the best option when
handling corrosive chemicals because packing can be made from inert materials, cheap
ceramic packing material, or other chemicals resistant packing element . Moreover, it is
good to be used to separate thermally sensitive liquids. For foaming liquid, the handling
of foaming liquid in packed column is more appropriate because of the relatively low degree
of agitation by the gas. However, if solid particles are present in the liquid, the cleaning of a
packing section is much too complicated and expensive compared with the plate discharge.

5
The packed bed column is not suitable for working under stressed conditions of temperature
variations and pressure because the packing elements are easily breakable. For operation of
too low liquid flow, contact efficiencies are decreased because the wetting of packing
material may not be adequate. For too high liquid flow rate, it is not economical.
Packed bed column is often used to recover solvents. In petrochemical industry, the example
of processes involve with distillation from hydro-carbon mixtures are splitting of gas
condensate into naphtha and low Sulphur gas oil, splitting off spec low flash petroleum
products into gasoline component and gasoil component, producing clean gasoil from dark
gasoil, splitting pipeline interfaces into gasoline component and gas oil component. Packed
bed column is also used in a pilot plant. A pilot plant is a small industrial system which is
operated to generate information about the behavior of the system for use in design of larger
facilities. The pilot plant can be used for training personnel for a full-scale plant. Pilot plants
are used to reduce the risk associated with construction of large process plants. (Naik et al.,
20

Advantages and Disadvantages of Packed Bed Distillation

The most cost-efficient distillation column when the diameter of the column is when the
diameter of the column is less than 0.6 m. Another advantage is that, because packing can be
made from inert materials, packed beds are able to handle corrosive materials. Furthermore,
there is lower pressure drop compared to than in plate columns preventing column flooding.
Packed bed distillation is good for thermally sensitive liquids. The packed bed is also
suitable for low pressure operations.
As for the disadvantages pertaining to packed bed distillation column, the packing can break
during installation, or due to thermal expansion. The packed bed is also not cost efficient for
high liquid flow. Another disadvantage is that the contact efficiencies are decreased when
the liquid flow rate is too low.

6
3.0 Procedure

In order to carry out the experiment, the following procedure was carried out:

3.1 The standard curve of x vs RI at methanol-water ratio from 0 1 was prepared.

3.2 The volume of water and methanol was noted down.

3.3 Valves V1 V6 was closed.

3.4 The switches on the panel were ensured to be at OFF position.

3.5 Water was filled in the cold water tank.

3.6 The reboiler was filled with methanol-water solution by opening the valve V1 and air vent
valve V2.

3.7 Valves V1 and V2 were closed.

3.8 The electric supply was connected to the set up.

3.9 The process temperature for the process range was set at 85- 95 C.

3.10 The heater and cooling water pump were started.

3.11 The cold water flow rate was adjusted by valve V3 to a moderate value.

3.12 The cyclic timer was set at total reflux.

3.13 Steady state was achieved after a waiting period of 20 -30 minutes.

3.14 The samples from the bottom and distillate stream was taken out by closing the timer for a
short while.

3.15 The samples collected were cooled down to room temperature and the refractive indices
were measured.

3.16 Samples at different temperatures were taken and the refractive indices were measured.

3.17 The temperature and the refractive indices were noted down.

7
3.18 The cyclic timer was then adjusted to a desired reflux ration for 3 5 mins.

3.19 The samples from both distillate and bottom product were taken out.

3.20 The samples were cooled down to room temperature and the refractive indices was
measured.

3.21 The samples were taken at different temperatures and the refractive indices was measured.

3.22 The temperature and the refractive indices were noted down.

3.23 The experiment was repeated for different set point temperatures and reflux ratios.

3.24 The water supply was stopped at the end of the experiment.

3.25 The pump, heater and the main power supply was switched OFF.

3.26 The column, reflux drum and receiving tank was drained.

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The following shows the calculations of formulas used in order to fulfill the objective of the
experiment:

(a) For total reflux condition

The x values are from the standard curve of RI vs x, which can be viewed in the Results and
Discussion section of this report:

XF , the value is corresponding to the RIF value.

XB, , the value is corresponding to the RIB value.

XD , the value is corresponding the RID value.

To calculate the property of methanol () at temperature TF (oC) from data book by interpolating.

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(b) For desired reflux condition

The x values are from the standard curve of RI vs x, which can be viewed in the Results and
Discussion section of this report:

XF , the value is corresponding to the RIF value.

XD , the value is corresponding the RID value.

The y value is then calculated for its respective temperature conditions.

x
y=
1+ ( 1 ) x

To calculate the property of methanol (CPM ,M ) and water (CPW ,W ) at temperature TB (oC)
from data book by interpolation.

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11
The following shows the nomenclature pertaining to this experiment.

12
4.0 Results and Discussion

13
 Table 1: Readings of Refractive Indices (RI) obtained for different mole fractions (x).
x Volume of H2O(ml) Volume of CH3OH (ml) RI
0.0 10 0 1.3310
0.1 9 1 1.3310
0.2 8 2 1.3325
0.3 7 3 1.3340
0.4 6 4 1.3360
0.5 5 5 1.3370
0.6 4 6 1.3370
0.7 3 7 1.3350
0.8 2 8 1.3330
0.9 1 9 1.3305
1.0 0 10 1.3275

Table 2: Observation table for total reflux condition and desired reflux condition when
temperature is 95 oC.
Total reflux condition Desired reflux condition

Table 3: Readings obtained experimentally under different temperature conditions for total
and desired reflux conditions.

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 Total Reflux Desired Reflux
o
T ( C) RIF xF RID xD RIF xF RID xD
85 1.3310 0.0 1.3290 0.96 1.3285 0.96 1.3340 0.30
90 1.3340 0.3 1.3295 0.92 1.3300 0.92 1.3340 0.30
95 1.3330 0.8 1.3250 - 1.3300 0.92 1.3290 0.96

1.34

1.34

1.33

1.33

1.33
RI

1.33

1.33

1.32

1.32
0 0.2 0.4 0.6 0.8 1 1.2

Figure 1: Graph of refractive index versus the mole fraction of methanol

As shown in results collected from Table 1 to Table 3, the objective of the experiment is fulfilled.
At the beginning of the experiment, a graph of RI vs x is drawn. Where x is the mole fraction of
methanol, and R1 is the refractive index of the methanol. The different mole fractions of
methanol was prepared by diluting a specific volume of methanol with a specific volume of
distilled water. The volumes of water and distilled water to be mixed can be seen in table 1. After
the solution of water-methanol is prepared, the refractive index is then measured. The results
obtained can be seen on the graph below.

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The graph shows the refractive indices collected experimentally. As the mole fraction of
methanol increases from 0 to 0.5, the refractive indices also increases from 1.3310 to 1.3370.
After the peak at x=0.5 to x=1.0, it starts declining from a value of 1.3370 to 1.3275.

The feed mixture contains components of different volatilities, and enters the column
approximately at the middle. The liquid flows downward through the packing, and the vapor
flows upward through the column. Differences in concentration cause the less-volatile
components to transfer from the vapor phase to the liquid phase. The packing increases the time
of contact, which increases the separation efficiency. The exiting vapor contains the most volatile
components, while the liquid product stream contains the least volatile components.

Figure 2: Packed Bed Distillation Column

After the feed mixture enters the column, the liquid flows down the column through the packing
counter currently and contacts the rising vapor stream. The liquid at the bottom, enters the
reboiler (heater). Two streams exit the reboiler, a vapor stream which returns to the column, and
a liquid product stream. The vapor stream flows upwards through the packing, picks up the more
volatile components, exits the column, and enters a condenser. After the vapor condenses, the
stream enters the reflux drum, where it is split into an overhead product stream, known as the
distillate, and the reflux stream that is recycled back to the column. In this experiment, to reflux
conditions was carried out which is total reflux condition and desired reflux condition. Under

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total reflux condition, the cyclic timer was set to infinity which was 999 seconds. Whereas, in the
case of desired reflux condition the cyclic timer was set at 5 seconds. When at 999 seconds, it
shows that for every 999 seconds the distillate will be secreted and some of the distillate will
return back (reflux stream) to the steam generator. In the case of desired reflux condition, it takes
every 5 seconds.

For total reflux condition, at temperature 85 oC, the distillate and the feed was collected with the
cyclic timer switched off momentarily. The refractive indices of this products were measured,
RIF (feed) and RID (distillate). The RIF value at 85 oC is 1.331, while RID was measured to be
1.3290. At 90 oC, RIF = 1.334 and RID = 1.3295. At 95 oC, RIF = 1.333 and RID = 1.325. After
much analyzation of the results obtained from table 2, as the temperature increases from 85 to 90
o
C the RIF value increases. It then decreases when set at temperature of 95 oC. The similar trend
also can be seen for the refractive index of the distillate sample (RI D). First increasing to 1.3295
from 1.3290, then decreasing to 1.3250 at temperature 95 oC. Its obvious here also that the
distillate sample has a higher refractive index compared to the feed sample. With the results
obtained experimentally, the two liquids were able to have more contact surface area. The packed
bed distillation column actually provides a higher contact surface are for the two phases to
encounter each other. Hence, making ideal for distillation to occur. Larger the contact surface
area, improving the contact between the fluids and therefore, improving distillation conditions in
the packed bed.

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5.0 Conclusion and Recommendations

From the results obtained it is obvious that the objective of the experiment was achieved. For
total desired reflux: 85C with RI F = 1.331 and RID = 1.3290; 90C with RIF = 1.334 and RID
=1.3295, and 95C with RIF =1.333 and RID = 1.3250. For desired reflux condition: 85C with
RIF = 1.3285 and RID = 1.3340; 90C with RIF = 1.33 and RID =1.334, and 95C with RIF =1.330
and RID = 1.3290. The objectives of this experiment was to study the operation of a packed bed
distillation column by verifying the Rayleigh Equation. Another objective is to obtain the T-x
data under total reflux condition at steady state and compare it with the theoretical value. Being
able to operate the column under total reflux condition and to calculate the minimum number of
theoretical stages using Fenskes equation is also one of the objectives to be fulfilled when
conducting this experiment. Being able to operate the column under any desired reflux condition
and calculating the theoretical number of stages using Mc-Cabe Thieles method is an objective
to be achieved in the experiment. The final objective in conducting this experiment is to calculate
the height equivalent to theoretical plate (HETP) for known packed height.

Although the results were obtained, they were not ideal. While conducting the experiment, there
were a few non-ideal conditions when preparing the methanol-water solutions for the
experimental data. While measuring the volume of water and methanol needed for the respective
solutions for the respective methanol mole fraction, there were air bubbles found in the syringe.
Hence, making difficult to obtain an ideal graph of RI vs x for the experimental data.

7.0 References

1. Warren L. McCabe, Julian C. Smith and Peter Harriott, Unit Operations of Chemical
Engineering, McGraw-Hill, 2005

2. Geankoplis, C.J., Transport Processes and Unit Operations, 3 rd ed., Prentice-Hall

International Inc., 1978

3. J. V. S. Nascimento,2009. Experimental Study of a Rotating Packed Bed Distillation

Column.

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4. Coulson, J.M. and Richardson, J.F., Chemical Engineering, Vol. II (Particle Technology and
Separation Processes), Pergamon, 1991.

5. Retrieved from, http://encyclopedia.che.engin.umich.edu/

19
7.0 Appendix

These are the data given in order to calculate the values:

Relative volatility 3.32

Molecular weight of methanol MM 32 g/mole
Molecular weight of Water MW 18 g/mole
Enthalpy of feed HF 0 kJ/kmole
Packed height Z 0.90 m

Property of methanol ( ) at temperature (TF). The calculations below shows the interpolation

for temperature of 95 oC.

Temperature (oC) Density, (kg/m3)

90 724
95 ?
110 704

Let T= x, and =y.

( xx 1)( y 2 y 1)
y = y2 + (x 2x 1 )

(9590)(704724)
y = 704 + (11090)

y = 699 kg/m3, the density ( = 699 kg/m3

V (699)(2)
F= M M 1000 = (1000)(32) = 0.045 kmol

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 x Fx D 0.81.0
B= F= 0.045= 0.09 kmol
x Bx D 0.91.0

F xF (0.045)(0.8)
ln
BxB = ln ( 0.09 ) (0.9) = -0.811

1 x
1 x
0.9(10.1)
B ( B)=3.32 ln =0
0.1(10.9)
( F )
F

ln

1x
1x
B ( B)=0.8110=0.811
E= ( F)
F
F xF
ln ln
B xB

1x
1x
( B) 0.9 ( 10.1 )
ln
Nm = x ( D) 0.1 (10.9 )
xD B 1= 1=2.66 3
ln a ln 3.32
ln

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