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Mass transfer and distillation column
1.1 Introduction
The term diffusion (mass transfer) is used to denote the transference of a
component in a mixture from a region where its concentration is high to a region
where the concentration is lower. Diffusion process can take place in a gas or
vapour or in a liquid, and it can result from the random velocities of the molecules
(molecular diffusion) or from the circulating or eddy currents present in a
turbulent fluid (eddy diffusion).
Diffusion is the movement of an individual component
through a mixture. (the influence of a physical stimulus)
Driving force is a concentration gradient of the diffusing
component.
A concentration gradient tends to move the component in the
direction to equalize concentrations and destroy the gradient.
Diffusion is the characteristic of many mass transfer
operations.
Diffusion can be causes by an activity gradient such as by a
pressure gradient, by a temperature gradient, or by the
application of an external force field.
Role of diffusion in mass transfer.
o Distillation
o Leaching
o Crystallization
o Humidification
o Membrane separation
Differences between heat transfer and mass transfer
Heat transfer is an energy transition but diffusion is the
physical flow of material.
Heat transfer in a given direction is based on one temperature
gradient and the average thermal conductivity.
Mass transfer, there are different concentration gradients for
each component and often different diffusivities.
Where:
JA: is the molecular diffusion flux of A, (moles per unit area per unit time)
kmol/m2.s.
CA: is the concentration of A (moles of A per unit volume) kmol/m3.
DAB: is known as the diffusivity or diffusion coefficient for A in B (unit area per
unit time) m2s
Z: is distance in the direction of transfer (m).
Diffusion depends on:
1. Driving force (ΔC), moles per unit volume (kmol/m3).
2. The distance in the direction of transfer (Δz), meter (m).
3. Diffusivity coefficient, unit area per unit time (m2/s).
The Fick’s law is similar to Fourier’s law of heat conduction and Newton’s
equation for shear-stress-strain relationship.
Total diffusion equation in the form of partial pressure (normally used for gases)
Total diffusion equation in the form of mole fraction (used for gases and liquids)
2. Counter diffusion:
i. Equimolecular counter diffusion:
When the mass transfer rates of the two components are equal and opposite the
process is said to be one of equimolecular counter diffusion. Such a process
occurs in the case of the box with a movable partition. It occurs also in a
distillation column when the molar latent heats of the two components are the
same (λA = λB). At any point in the column a falling stream of liquid is brought
into contact with a rising stream of vapour with which it is not in equilibrium.
The less volatile component is transferred from the vapour to the liquid and the
more volatile component is transferred in the opposite direction. If the molar
latent heats of the components are equal, the condensation of a given amount of
less volatile component releases exactly the amount of latent heat required to
volatilize the same molar quantity of the more volatile component. Thus at the
interface, and consequently throughout the liquid and vapour phases,
equimolecular counter diffusion is taking place (NB = - NA).
The most important things is to calculate the mass transfer rate for the sphere
surface where the surface area is constant (𝟒𝛑 𝐫𝟎𝟐):
When the mass transfer from surface to a large distance compare to the sphere
surface (𝐫𝟎):
𝐫 𝟏→ ∞ and 𝐂𝐀𝟐=0
For the case of diffusion radially through a cylinder wall inner radius r1 and
outer r2 and length L.
The two-film theory of Whitman (1923) was the first serious attempt to represent
conditions occurring when material is transferred in a steady state process from
one fluid stream to another. In this approach, it is assumed that a laminar layer
exists in each of the two fluids. Outside the laminar layer, turbulent eddies
supplement the action caused by the random movement of the molecules, and the
resistance to transfer becomes progressively smaller as shown in Figure below.
The thicknesses of the two films are z1 and z2. Equilibrium is assumed to exist
at the interface and therefore the relative positions of the points C and D are
determined by the equilibrium relation between the phases.
The rate of mass transfer per unit area in terms of the two-film theory for
equimolecular counter diffusion is given for the first phase as:
The rate of mass transfer per unit area from the liquid film:
The relation between the partial pressure (PA) and concentration (CA):
𝐲𝐀=𝐊 𝐗𝐀
Henry's law:
𝐏𝐀=𝐇 𝐂𝐀
Where: H is the Henry's constant.
The work of Higbie laid the basis of the penetration theory in which it is assumed
that the eddies in the fluid bring an element of fluid to the interface where it is
exposed to the second phase for a definite interval of time, after which the surface
element is mixed with the bulk again. Thus, fluid whose initial composition
corresponds with that of the bulk fluid remote from the interface is suddenly
exposed to the second phase. It is assumed that equilibrium is immediately
attained by the surface layers, that a process of unsteady state molecular diffusion
then occurs and that the element is remixed after a fixed interval of time. In the
calculation, the depth of the liquid element is assumed to be infinite and this is
justifiable if the time of exposure is sufficiently short for penetration to be
confined to the surface layers. Throughout, the existence of velocity gradients
within the fluids is ignored and the fluid at all depths is assumed to be moving at
the same rate as the interface.
The diffusion of solute A away from the interface (y-direction) is thus given by:
The mass transfer rate per unit area of surface is then given by:
The rate of mass transfer per unit area from the gas film:
The rate of mass transfer per unit area from the liquid film:
Where:
(𝐃𝐀𝐁)𝐠= (𝐃𝐀𝐁)𝐋 𝐍𝐀𝐠=𝐍𝐀𝐋
Since the film thickness 𝐙𝐠 and 𝐙𝐋 are difficult to define or estimate, then we
rewrite the above equations as follow:
But: 𝐏𝐀𝐢 and 𝐂𝐀𝐢 are difficult to measure, therefore we define the overall mass
transfer coefficient:
Where:
𝐤𝐋 is the individual liquid film mass transfer coefficient.
𝐤𝐠 is the individual gas film mass transfer coefficient.
𝐊𝐎𝐋 is the overall mass transfer coefficient based on liquid phase.
𝐊𝐎𝐆 is the overall mass transfer coefficient based on gas phase.
𝐏𝐀𝐢 is the partial pressure of the gas (A) at the interface.
𝐂𝐀𝐢 is the concentration of the liquid (A) at the interface.
𝐏𝐀∗ is the partial pressure of the gas phase which is in equilibrium with the liquid
phase 𝐂𝐀.
𝐂𝐀∗ is the concentration of the liquid phase which is in equilibrium with the gas
phase 𝐏𝐀.
2.1 Introduction
Distillation is a method used to separate the components of liquid solution,
which depends upon the distribution of these various components between
a vapor and a liquid phase.
The vapor phase is created from the liquid phase by vaporization at the
boiling point.
Distillation is concerned with solution where all components are
appreciably volatile such as in ammonia-water or ethanol-water solutions,
where both components will be in the vapor phase.
2.2 Vapor-Liquid Equilibrium Relations
Raoult’s Law
An ideal law, Rault’s law, can be defined for vapor-liquid phases in
equilibrium (only ideal solution e.g. benzene-toluene, hexane-heptane etc
pA PA xA
Where
PA is the partial pressure of component A in the vapor in Pa (atm)
PA is the vapor pressure of pure A in Pa (atm)
XA is the mole fraction of A in the liquid.
Composition in liquid: 1 x A xB
Composition in vapor: 1 y A yB
Boiling-Point Diagrams and xy Plots
Boiling-point diagram for system benzene (A)-toluene (B) at a total pressure of
101.32 kPa.
Where
pA, pB are the partial pressure of component A and B in the vapor in Pa (atm)
PA , PB are the vapor pressure of pure A and pure B in Pa (atm)
P is total pressure in Pa (atm)
xA is the mole fraction of A in the liquid.
The boiling point diagram can be calculated from the pure vapor-pressure data
in the table below and the following equations:
Example A mixture of 50% mole normal heptane and 50% normal octane at 30ºC
is continuously flash distilled at 1 standard atmosphere so that 60 mol% of the
feed is vaporized. What will be the composition of the vapor and liquid products?
The theoretical stages for the stripping section are determined by starting at x w,
going up to yW, and then across to the operating line, etc
In given below the figure, the q line is plotted for various feed conditions. The
slope of the q line is q/ (q-1).
q = 0 (saturated vapor)
q = 1 (saturated liquid)
q > 1(subcooled liquid)
q < 0 (superheated vapor)
0 < q < 1 (mix of liquid and
vapor)
3) Plot the operating lines. The intercept of the rectifying lie on the y axis is,
XD/(R+1) = 0.974/ (3.5+1) = 0.216. From the intersection of the rectifying
operating line and the feed line, the stripping line is drawn.
4) Draw the rectangular steps between the two operating lines and the
equilibrium curve. The stripping line is at the seventh step. By counting
steps it is found that, besides the reboiler, 11 ideal plates are needed and
feed should be introduced on the seventh plate from the top.
2) Fouling potential,
3) Liquid to vapor density ratio,
4) Liquid loading, and
5) Most importantly the life cycle cost.
Trays can be divided into many categories, such as baffle trays, dual flow trays,
conventional trays, high capacity trays, multiple down comer trays and system
limit trays. According to some rules of thumb, trays should be selected if:
1) The compounds contain solids or foulants
2) There are many internal transitions
3) Liquid loads are high
4) There is a lack of experience in the service
5) Vessel wall needs periodic inspection
6) There are multiple liquid phases
On the other hand, packing divisions include grid packing, random packing,
conventional structured packing, and high capacity structured packing. The rules
of thumb for selecting packing are:
1) The compounds are temperature sensitive
2) Pressure drop is important (vacuum service)
3) Liquid loads are low
4) Towers are small in diameter
5) Highly corrosive service (use plastic or carbon)
6) The system is foaming
7) The ratio of tower diameter to random packing is greater than 10
Some design guidelines should be considered when designing a tray tower, such
as follows:
1) Tray spacing should be from 18 to 24 inches, with accessibility in mind
(Generally, for a tower diameter of 4 feet and above, the most common tray
spacing is 24 inches to allow easy access for maintenance. However, for a
tower diameter below 4 feet, a tray spacing of 18 inches is adequate as the
column wall can be reached from the man way.)
2) Peak tray efficiencies usually occur at linear vapor velocities of 2 ft/s (0.6 m/s)
at moderate pressures, or 6 ft/s (1.8 m/s) under vacuum conditions.
3) A typical pressure drop per tray is 0.1 psi (0.007 bar)
4) Tray efficiencies for aqueous solutions are usually in the range of 60-90%
while gas absorption and stripping typically have efficiencies closer to 10-
20%
5) Sieve tray holes are 0.25 to 0.50 in. diameter with the total whole area being
about 10% of the total active tray area. Maximum efficiency is 0.5 in and 8%.
6) Valve trays typically have 1.5 in. diameter holes each with a lifting cap. 12-14
caps/square foot of tray is a good benchmark.
7) the most common weir heights are 2 and 3 in and the weir length is typically
75% of the tray diameter.
The packed tower design concepts are listed below:
1) Packed towers almost always have lower pressure drop compared to tray
towers.
2) Packing is often retrofitted into existing tray towers to increase capacity or
separation.
3) For gas flow rates of 500 ft3/min (14.2 m3/min), use 1 in (2.5 cm) packing,
for gas flows of 2000 ft3/min (56.6 m3/min) or more, use 2 in (5 cm) packing.
4) Ratio of tower diameter to packing diameter should usually be at least 15
5) Due to the possibility of deformation, plastic packing should be limited to an
unsupported depth of 10-15 ft (3-4 m) while metal packing can withstand 20-25
ft (6-7.6 m).
6) Liquid distributor should be placed every 5-10 tower diameters (along the
length) for pall rings and every 20 ft (6.5 m) for other types of random
packing.
7) For redistribution, there should be 8-12 streams per sq. foot of tower area for
towers larger than three feet in diameter. They should be even more numerous
in smaller towers.
8) Packed columns should operate near 70% flooding.
9) Height Equivalent to Theoretical Stage (HETS) for vapor-liquid contacting is
1.3- 1.8 ft (0.4-0.56 m) for 1 in pall rings and 2.5-3.0 ft (0.76-0.90 m) for 2 in
pall rings.
10) Design pressure drops should be as follows:
Distillation Definition
3.1 Definition:
A process in which a liquid or vapour mixture of two or more substances is
separated into its component fractions of desired purity, by the application and
removal of heat.
3.2 Distillation Process Types
Batch
Continuous
Batch Process
In batch operation, the feed to the column is introduced batch-wise. That is,
the column is charged with a 'batch' and then the distillation process is carried
out. When the desired task is achieved, a next batch of feed is introduced.
Continuous Columns
In contrast, continuous columns process a continuous feed stream. No
interruptions occur unless there is a problem with the column or surrounding
process units. They are capable of handling high throughputs and are the more
common of the two types. We shall concentrate only on this class of columns.
3.3 Distillation Types
Continuous columns can be further classified according to:
The nature of the feed that they are processing,
Binary column -feed contains only two components
multi-component column -feed contains more than two components
The number of product streams they have
multi-product column -column has more than two product streams
Where the extra feed exits when it is used to help with the separation,
extractive distillation -where the extra feed appears in the bottom
product stream
azeotropic distillation -where the extra feed appears at the top product
stream
The type of column internals
Tray column -where trays of various designs are used to hold up the
liquid to provide better contact between vapor and liquid, hence better
separation
packed column -where instead of trays, 'packings' are used to enhance
contact between vapor and liquid .
3.4 Distillation Equipment
A typical distillation contains several major components:
a vertical shell where the separation of liquid components is carried out
Column internals such as trays/plates and/or packings which are used to
enhance component Sep.
a reboiler to provide the necessary vaporization for the distillation process
a condenser to cool and condense the vapour leaving the top of the column
a reflux drum to hold the condensed vapour from the top of the column so
that liquid (reflux) can be recycled back to the column
Open structure for low resistance to vapour flow, hence low pressure
drops
Promote uniform liquid distribution on surface
Promote uniform gas flow across column cross-section
3.8.1 Packing Types
Shaped packing/ random packing
Structured packing
Various random shaped packing including:
Rasching Rings: simple hollow ring, oldest, cheapest, most widely used,
less effective, not necessarily most economic. Can be made in various
material and ceramic and carbon.
Lessing Rings: Rasching Rings with partitions across its Centre, increased
surface area and strength. Ceramic and metals
Pall Rings: superior performance, highly effective give better wetting and
distillation. Liquid smaller pressure drop than Rasching under same
conditions, available in metals, ceramics and plastics.
Berl saddles: less free gas space better aerodynamic shape, ceramic or
plastic
Kinds of Reflux
A. Cold Reflux
Cold reflux is defined as reflux that is supplied at temperature a little below that
at the top of the tower. Each pound of this reflux removes a quantity of heat equal
to the sum of its latent and sensible heat required to raise its temperature from
reflux drum temperature to the temperature at the top of the tower.
B. Hot Reflux
It is the reflux that is admitted to the tower at the same temperature as that
maintained at the top of the tower. It is capable of removing the latent heat
because no difference in temperature is involved.
C. Internal Reflux
It is the reflux or the overflow from one plate to another in the tower, and may be
called hot reflux because it is always substantially at its boiling point. It is also
capable of removing the latent heat only because no difference in temperature is
involved.
D. Circulating Reflux
It is also able to remove only the sensible heat which is represented by its change
in temperature as it circulates. The reflux is withdrawn and is returned to the
tower after having been cooled.
E. Side Reflux
This type of reflux (circulating reflux) may conveniently be used to remove heat
at points below the top of the tower. If used in this manner, it tends to decrease
the volume of vapor the tower handles.
F. Total Reflux
Total reflux is the conclusion when all the condensate is returned to the tower as
reflux, no product is taken off and there is no feed.
3.12 Column Problems
Foaming
Refers to the expansion of liquid due to passage of vapor or gas, caused by
high vapor flow rates.
Although it provides high interfacial liquid-vapor contact, excessive
foaming often leads to liquid buildup on trays. In some cases, foaming may
be so bad that the foam mixes with liquid on the tray above.