1. What is the effect of pressure on distillation?
Which condition is preferred- low pressure or
high pressure?
At high pressures, the distance between the diagonal line (y=x) and the equilibrium curve becomes
shorter and the corresponding boiling temperatures also become higher.
Illustrated in this graph is an equilibrium curve at different pressures, the red color is an equilibrium
curve at pressure p1 and the curve in green color is the equilibrium curve at pressure p2. (P2>P1).
The distance between the equilibrium curve at p2 and the diagonal line is closer to the diagonal line,
for a given liquid of mole fraction x of more volatile component, as the vapor composition will be
larger for pressure p1 than for p2 as shown.
The separability becomes less easy at higher pressures. For the same separation, larger column
dimensions (/a greater number of theoretical stages) are operated at high pressures.
This figure illustrates the effect of pressure on the reflux versus number of theoretical stages. It can
be seen from the curve that lower pressure leads to lower reflex requirements. Alternatively
speaking for a given reflex ratio low pressure requires less number of theoretical stages.
2. Question number two what is the difference between theoretical stage and actual stage?
An equilibrium stage is one in which the two phases: liquid and vapor, are contacted thoroughly and
phases leave at equilibrium.
Practical operating considerations impose a limitation on how close equilibrium is approached.
Therefore, tray efficiency is used to express the deviation from equilibrium in actual tray.
The actual stage represents an actual tray in the column
3. What is the effect of reflux ratio for given separation of components of feed mixture in a
distillation column. How does it affect the number of theoretical stages required for
separation.
As the reflex ratio R is increased, the slope of the operating line for the rectification section moves
away from the equilibrium line towards maximum value of 1. When overlapped product, D=0, R
becomes infinity and the slope reaches a value of 1.
this figure illustrates how the increase or decrease of reflux ratio moves the operating line from the
original position. It is obvious from this graph that increasing of r moves the operating line closer to
the diagonal line and decrease of or moves operating line of the rectification section closer to the
equilibrium curve.
As noted in the above figure when the dislike product rate is zero the operating line merges with the
diagonal line, we call this total reflux condition. (The entire overhead vapour is condensed and
returned as reflux to the column and no product is withdrawn.) What this means is that more and
more liquid that is rich in the more volatile component is being recycled back into the column under
this condition, thus, separation becomes better and the product becomes purer, thus fewer trays are
needed to achieve same degree of separation.
On the other hand, as reflux is decreased, the operating line for the rectification system moves
toward the equilibrium line. The ‘pinch’ between operating and equilibrium lines becomes more
pronounced and more trays required. The limiting condition occurs at minimum reflux ratio when
infinite number of trays will be required to effect the separation. This occurs at a point where the
rectification operating line intersects the equilibrium line. The normal design practice is to strike a
balance and operate the column at an optimum reflux ratio.
Higher reflux will result in higher boil up and hence higher rebuilder duty that means higher
operating cost. Most columns are designed to operate between 1.2 to 1.5 times the minimum flip
flux ratio because this is approximate region of minimum operating costs.
4. Where does the light non-key appears, in a multi component distillation column?
The light non-key in a multi-component distillation appears in the overhead product. The light non
key is lighter than the light key component hence it goes to the distillate.
5. What is the effect of relative volatility on the distillation process?
Relative volatility significantly impacts the separation of a given feed mixture in terms of:
the number of trays required to achieve a given degree of separation.
Assume alpha is 1, then according to the above equation y=x, what means is that the vapor leaving
the tray has the same concentration as a liquid leaving the tray. Thus, the tray will not achieve any
separation. This mixture cannot be separated by simple distillation process.
Now let us consider a binary mixture having alpha=1.2, so when x is 0.5 this mixture will have
equilibrium y=0.5454. The vapor is richer in the more volatile component (MVC) than the liquid by
9%. Hence separation by distillation is possible for this mixture.
As the value of alpha increases, the vapor enrichment increases, this means is that the number of
trays required to effect a given separation decreases as the relative volatility of the liquid mixture
increases.
Thus, the relative volatility alpha, is the main variable influencing the column design.
6. What is an azeotrope?
Azeotrope is a liquid mixture, that produces a vapor having the same composition as that of the
liquid. The VLE curve crosses the diagonal line (y=x).
7. What is bubble point and dew point? What is their usefulness in distillation process
analysis?
For a given mixture, the bubble point is defined as the temperature at which the first bubble of vapor
forms, at a given pressure.
At this temperature that is bubble point, vapor and liquid phases are in equilibrium.
At bubble point, liquid phase composition is known.
For a mixture, the dew point is defined as the temperature at which the first drop of liquid forms at a
given pressure.
At this temperature both liquid and vapours are in equilibrium.
At dew point the vapor phase composition is known.
Bubble point and Dew point are used in the analysis of multi-component distillation:
1. Dew point enables you to estimate the distillation column top temperature at the given
column pressure.
2. Bubble point enables you to determine the distillation column bottom temperature, at a
given column pressure.
The top and bottom temperatures of the column are required to determine the relative volatilities, at
the top and bottom.
Relative volatility of a multi-common system is a function of both temperature and pressure.
8. For which application vacuum distillation is preferred?
Vacuum distillation is usually preferred: (low pressure/ vacuum pressure operation so bp also
decreases)
1. when the products are thermally sensitive &
2. the components to be separated has close boiling point difference hence low relative
volatility.
9. What is boil up ratio?
Boil up ratio is defined as a ratio of amount of vapor generated in the reboiler per mole of bottom
product.
10. What is weeping? what action is needed by the engineer when weeping occurs?
Weeping is a process in which the liquid is falling through the tray holes. Weeping point is defined as
a vapor flow at which the first falling of liquid through the holes becomes noticeable. It affects the
separation process and its efficiency.
To avoid weeping, take action to increase the vapor flow rate, by increasing the reboiler load and also
the feed rate to the column.
Lecture 2
11. You are given a liquid mixture whose components have close boiling point, that is low
relative volatility how will you separate them?
Even with the low relative volatility of alpha > 1.05, you can separate the mixture by distillation.
Hence option one is conventional distillation, preferably vacuum distillation provided alpha=1.05
(minimum).
As relative volatility decreases, the separation becomes less easy by this method. You need large
number of stages and high reflux ratios, which will involve high capital cost and operating expenses.
One alternative for separation of low relative volatility feed or close boiling feed is to use extractive
distillation with an entrainer. The entrainer interacts differently with the components to be separated
and causes changes in the relative volatility thereby making separation task easier.
This figure illustrates a typical extractive distillation unit designed for separation of close boiling
components.
In a feed in the column c1, the feed entrainer interacts with the heavy component and leaves to the
bottom of the column with component b. The relative volatility of the component a is greater than b
which is greater than the entrainer e. Hence a is withdrawn as displayed from c1.
The bottom stream of the column c1 is fed to the column c2 where the entrainer is separated from
the component b. b being more volatile is removed as distillate from column 2. The entrainer is
removed from the bottom of c2 and recycled to column c1.
Another important closed boiling mixture in the petrochemical production process, is xylene isomers
which have close boiling points.
The separation by conventional distillation is not possible because of the close boiling points
Paraxyline is separated from other isomers by selective absorption on a molecular sieve with the use
of a desorbent followed by distillation. The selective absorption on molecular sieve with a desorbent
produces two streams: 1. EXTRACT: p-xylene diluted with desorbent
2.RAFFINATE: o, m-xylene diluted with desorbent.
The raffinate and extract streams are sent to 2 separate distillation columns for separation of xylenes
from the desorbent.
Another alternative in the separation of close boiling mixtures is hybrid processes. Hybrid process is a
combination of liquid liquid extraction with an entrainer followed by distillation. This is a more
economical alternative. Membrane separation with distillation hybrid process is emerging as another
alternative candidate for low relative relativity application.
Another alternative is heterogeneous azeotropic distillation. Availability of good and cheap solvent is
the key requirement.
You must evaluate the alternative processes including distillation and make an economic analysis to
decide on the final choice.
12. What is the difference between total condenser and the partial condenser in your
distillation system?
Total condenser a condenser in which the entire overhead vapor from a distillation column is
condensed and liquid is the only product. In general, conventional distillation column uses total
condenser. In total condenser the vapor and liquid phase composition is the same.
Part of the condensed product is returned to the column as reflux under flow control. The balance
liquid is withdrawn as distillate product under level control.
A partial condenser is one in which part of the vapor is condensed and returned to the column as
reflux and the balanced vapor quantity is withdrawn as vapor product.
A partial condenser acts as an equilibrium stage.
A partial condenser is commonly employed when there are light components in the column
overhead that would require high column pressure or low temperature refrigerant to condense. It
will eliminate the need for costly refrigerant in condensers. Several examples of partial condenser
can be seen in refineries and petrochemical plants. De-ethaniser is one such example in olefin
production process.
total condenser: in the scheme the entire vapor is going through the cooling water condenser and
condensed.
partial condenser: only the vapor equivalent to the amount of reflux required is condensed. The
balance vapor is separated in the reflux drum and withdrawn as a vapor distillate product.
13. A plant is designing a distillation column for separating a binary mixture. The plant wants the
entrainment to be minimum on the tray. You are given a choice to select a tray between sieve tray
and rectangular fixed valve tray. Which tray you will recommend?
You should recommend a rectangular sieve tray.
This figure illustrates the entrainment in % versus the vapor load on the tray for the two given types
of trays.
The entrainment for valve tray is lower compared to sieve tray for a constant load.
14. What is entrainment or jet flooding? What is the effect of entrainment on column
performance?
The column reaches its maximum capacity when the flooding commences. Flooding is excessive
accumulation of liquid on the tray.
When the flow rates of liquid and vapor are increased, liquid level on the tray increases due to
accumulation. Flooding occurs when the upward velocity is high enough, that creates a drag force
sufficient to suspend liquid droplets. The vapor liquid disengagement does not take place as desired
by design and the droplets begin to get entrained. The liquid entrained by the gas is transported to
the tray above. This causes some of the already separated liquid which has more of a less volatile
component than the tray above to mix with the liquid in the tray above. It counteracts the mass
transfer process and reduces the tray efficiency.
This graph illustrates the tray efficiencies versus column throughput and also the impact of flooding
on the efficiency.
Entertainment flooding can be classified into spray entertainment flooding and Froth entrainment
flooding.
i. Spray entertainment flooding is far more common (vap vel>>liq vel: liq drops in gas bed).
ii. Froth entrainment flooding (liq vel>>gas vel: gas bubbles in liq) is only encountered when
tray spacing is small and at high liquid loads.
15. What is point tray efficiency?
The point efficiency is defined as approach to equilibrium at some point on the tray.
The concentration of the vapor leaving the froth of the tray is considered to be in equilibrium with
the liquid composition at the specific point on the tray.
As a consequence, the point efficiency can vary across the length of the tray ie the flow path, if there
is a variation of liquid composition across the tray.
Lecture 3
16. What is the difference between a single pass tray and a multi-pass tray?
A single pass tray has one inlet down comer and one outlet down comer. The liquid entering the tray
from the inlet downcomer flows across the tray and overflows to the outlet downcomer to enter the
next tray below. We call it one pass for the liquid.
A multi-pass tray has more than two downcomers, hence they have two passes or more for the
liquid. As the liquid loading on the tray is increased, the liquid froth level on the tray increases. Under
higher liquid loading on the tray, column operation with a single downcomer faces instability.
Multi-downcomers are used:
i. To limit the liquid level on the tray
ii. to have stable hydraulics
Number of passes will depend on the: liquid loading and hence the number of downcomers.
17. You are given a sketch of a distillation column as shown below explain how will you measure the
pressure drop across the corner?
The pressure drop is measured as shown in
the sketch.
The imbalances of column pressures at the
bottom and top of the column is
individually tapped as shown in the figure
and fed to your differential pressure
transmitter which gives the output as a
column differential pressure.
It is not possible to measure the pressure
drop across the tray that is the reason why the column total pressure drop is measured. The column
total pressure drop = (individual tray pressure drop * the number of trays)
It is a reboiler that generates and drives a vapor up through the column for vapor liquid contact and
mass-transfer. The energy for the vapor flow is provided by the reboiler hence the pressure is highest
at the bottom. Fluid flows through the process equipment be it piping or heat exchanger or mass
transfer equipment etc always faces resistance to flow. This causes the pressure of the flowing fluid
to decrease hence the pressure of the fluid decreases in the direction of flow.
So, in distillation column a vapor flows from the reboiler to the bottom of the column and then to the
top through the trays. So, p2 the pressure at the bottom > p1, the pressure at the top.
Pressure drop is one of the important hydraulic parameters in analyzing sieve tray performance.
Pressure drop measurement for indication and control purpose is integral part of process design
development.
18. What are the factors that contribute to the tray pressure drop?
Tray is a vapor liquid contact element. It generates vapor bubbles thereby creates in the transfer area
for mass transfer.
The resistance to vapor flow arises from 2 sources: i. the tray holes ii. the liquid hold-up on the tray
Thus, the pressure drop across the tray
consists of 2 contributors: dry hole
pressure drop (hdh) and the pressure
drop due to the liquid inventory on the
tray (hydraulic pressure drop, hl).
Ht = (hdh + hl + hst)
Hst = residual pressure drop due to
surface tension (usually negligible)
Each hole can be treated as an orifice. Hence
the pressure drop occurs through a hole is
similar to the one that occurs when fluid flows
through an orifice. We can use a similar orifice
formula to calculate the dry phase pressure
drop.
Then when there is a liquid level on the tray, it
consists of: (clear liquid height close to the tray
surface + a froth height over the clear liquid (liq
+ vap mixture). This is the head which the
vapor has to overcome to flow up.
Pressure drop is an important operating parameter. High pressure drops results in high operating
temperatures at the bottom. When a tray column is used for heat sensitive products which gets
degraded at higher temperatures, the pressure drop becomes an important design parameter. Eg:
VDU.
The typical values of pressure drop across the tray in a distillation column:
i. for a conventional tray= 8 millibar
ii. for low pressure drop tray= 3 millibar
19. What is the difference between rectification, stripping and fractionation?
Rectification system remove heavy material from light product.
Stripping system removes light material from heavy product.
Fractionation system removes heavy material from light product and light material from heavy
product at the same time. A complex fractionation involves making of multiple products from either
a single turbo or a multiple or complex of towers with the recycle stream between them.
A good example of multiple product tower is a refinery crew
distillation column which produces naptha, kerosene and
diesel from the same tower.
20. what is k factor? What are the operating parameters
that influences the value of k?
K factor is a ratio of mole fraction of a component in the
vapor phase to that in the liquid phase in equilibrium. In a multi-component mixture, ki = (yi/xi). k
value is also known as equilibrium value. k factor is used in the analysis of multi-component
distillation process. k = function (temperature, pressure). Hence variation of pressure and
temperatures causes the value to change.
In your distillation column the pressure is always fixed. The temperature of each stage varies
depending on the tray
product composition.
Hence at a given pressure
the k value changes from
stage to stage. This graph is
a k-value profile for
propylene propane mixture
at 17 bar across the stages
obtained by simulation.
Lecture 4
21. For separation of a given liquid feed into respective components, the number of theoretical
stages is 50. What will be the approximate number of actual stages for the same degree of
separation?
You need overall column efficiency to determine the actual number of stages. The overall efficiency,
Eo = (number of theoretical stages in the column /number of actual stages in the column).
Overall efficiency is most commonly used efficiency term in the design of distillation column. The
overall column efficiency is approximately taken as 50% for preliminary design so the number of
actual stages= 50/ (50/100) =100.
22. What is HETP?
HETP is the height equivalent to a theoretical plate. This term is used as a measure of efficiency of a
given packed bed. HETP is the height of the packing in a distillation column to achieve a given
separation as would be achieved on one theoretical stage.
Higher HETP indicates lower efficiency. HETP values are complex functions of temperature, pressure,
composition, density, viscosity, diffusivity, pressure drop, vapor &/ liquid flow rates and packing
characteristics, etc.
23. Two pack towers are designed for the same mass velocity of the gas. The first tower has a
liquid and gas flow rate of 30 kg/second and 1.2 kg/second respectively. 2 nd tower has a liquid and
gas flow rates of 67.7 kg/second and 1.8 kg/second respectively. What is the ratio of the design
diameter of the wider tower to the narrower tower?
It is given that the two towers have been designed for the same mass velocity of gas, G.
The gas mass velocity of the first tower= GT1
The gas mass velocity of the second tower= GT2
Superficial velocity of gas = Us
Gas/Vapor density = RhoG
The wider tower thus has (wide-narrow/narrow) = 22.5 % larger diameter.
The increase in area takes care of the higher liquid loading of 67.7 kg per second while maintaining
the same superficial velocity as the narrow tower.
24. You are given two types of packing, packing a and packing b. Packing a has HETP=0.5 meter and
packing b has HETP = 0.3 meter. Which packing you will select for a heat sensitive product?
The HETP of packing A (=0.5 meter) > packing B (=0.3 m). Hence packing B is more efficient.
For a given feed and separation
objective, the packed column with
packing A will have higher packing
height than with packing B.
Accordingly packed column with
packing A will have higher pressure
drop than the column with packing B.
Higher pressure drop means higher
pressure at the bottom of the column
and higher pressure makes a liquid
boil at higher temperature. But at
higher temperature heat sensitive
products get degraded or decomposed. This affects the quality of the product produced. Since
column B will have a lower pressure drop, the packing b is preferred for heat sensitive product.
25. A binary mixture with two components (A&B) is to be separated in your distillation column to
get 95 mole% A as the top product. The relative volatility for the binary mixture is 2. The column
feed is a saturated liquid containing 50 mole% A. What is the minimum reflux ratio required for
separation?
The limiting condition occurs at minimum reflux ratio (R=0), when an infinite number of trays will be
required to effect separation. This occurs at a point where the rectification operating line intersects
the equilibrium line.
At minimal reflux, both operating lines touch the equilibrium line at pinch point (x’, y’).
Given that the feed is a saturated liquid, q=1. At minimum reflux the q line and the enrichment line
both intersect the equilibrium line at the same point.
Illustrated in this figure is the Mc-Cabe Thiele diagram developed for designing the distillation
column for the given separation.
Mole fraction of A in the feed (xF) is 0.5 and mole
fraction of A in the distillate (xd) is 0.95.
If you draw the rectification line such that the line
interacts with the equilibrium line at p which is (x’,y’),
the slope of the rectification line = Rm/(Rm+1)
At minimum reflux, the slope of the operating
line for rectification is obtained from the graph:
Since the feed is a saturated liquid, q=1 and x’=xf,
substituting this at the minimum reflux, the slope of the
rectification line becomes:
Now let us write the relationship between the
equilibrium concentration and relative volatility for ideal
solution using Raoult’s law:
Substituting the values of alpha =2, x’=xf=0.5, we get
y’=0.666. Using the previous equation, slope of the rectification line at minimum reflux: R m= 1.614
Lecture 5
26. What do you mean by quality of feed? What are the different qualities of feed usually and
considered in designing distillation column in the industries? If the feed to the distillation column
is 20 mole% vapor, what is the value of q?
The quality of feed means the fraction of feed that is liquid. The quality of feed is denoted by the
term q. When the feed is saturated liquid q=1. When the feed is saturated vapor q=0.
Distillation column can be designed to take feed that may fall under the following categories:
1. Sub cool liquid, q>1
2. Bubble point liquid, q=1
3. Partially vaporized, 0<q>1
4. Dew point vapor, q=0
5. Superheated vapor, q<1
Out of these 5 types of feed described above, Superheated vapor is not normally encountered in the
industrial applications. So, we consider only four categories of feed under 1 to 4 for distillation
column design and analysis.
Vapor % of the feed is 20 mole% hence q=1-0.2= 0.8, that is 80% liquid.
27. a. What is the significance of weir height on a tray in your distribution column? B. You have two
tray columns one operating at above atmospheric pressure and another operating under vacuum.
Which one of these two columns will have lower weir height?
The weir height is the plate parameter that has the most significant effect on the plate efficiency, as
the weir height is increased the plate efficiency increases, but the improvement in efficiency is
achieved at the expense of higher pressure drop and entrainment.
The tray column working under vacuum will have lower weir height as compared to column
operating above atmospheric pressure. The weir height in columns operating in atmospheric
pressure and above is usually in the range of 40 to 100 mm with 50 mm being the most common. In
vacuum distillation column, for keeping the tray pressure drop low, the weir height may be as low as
6 to 10 mm.
This is precisely the reason why VDU have lower plate efficiency.
28. What is turn down? What is the single most important factor that limits the turn down?
Turn down is the minimum flow rate at which the column begins to lose mass transfer efficiency
significantly. All tray types, have reasonably good turn down, 2:1.
In most cases, the turn down is limited with the loss of efficiency, which has different causes for
different devices. In all cases, the basic problem is inadequate liquid-vapor contact.
Sieve trays- The excessive weeping liquid falls through the column without flowing across the trays.
Valve trays- At low flow rates the valve remains closed, at large part of the tray. Significant quantity of
liquid flows across the trays without contacting the vapor stream.
Packing- At low flow rates, liquid distributors can no longer achieve uniform distribution because the
liquid level in the distributor is too low, that the liquid issuing from the holes get swayed by the gas.
In general, packing have better turn-down than trays, generally 10:1 for wetting liquids.
Valve trays have better turn down than Sieve trees generally at least 3:1.
29. How is the operating pressure controlled in a distillation column? Explain with your sketch.
In distillation column the pressure is maintained by the condenser. It is the condensation of the
overhead vapors that causes the pressure to decrease.
The amount of vapor generated in the column depends on the quantity of feed and the boil up ratio.
For the column pressure to remain constant, the amount of vapor generated should be equal to the
vapor condensed. Otherwise, pressure will vary.
This is done by manipulating the flowrate of cooling medium to the condenser. For example, if it's a
water-cooled condenser then the water flow rate has to be adjusted through a pressure control
valve.
The feed and steam fed in a reboiler generates vapor. The vapor moves up the column and comes
into contact with the liquid on the trays and the mass transfer takes place.
The light product upon enrichment leaves the column as overhead vapor and then condenses by
exchanging heat with cooling water in the condenser. So, it is condensation that removes the vapor
produced by the boiler. Now assume that the overhead vapor quantity is M and the amount
condensed in the condenser is m. The pressure will maintain if M=m, otherwise the pressure will
increase or decrease depending on whether M>m or M<m.
This figure illustrates a typical pressure control system in your distillation column.
Note the cooling water flow rate to the condenser is used to regulate the amount of condensation
and thereby to maintain the pressure in the column.
30. What is an azeotrope? How many types of azeotropes are there? How do you separate an
azeotrope?
Azeotropes are binary mixtures having the same composition in liquid and vapor phase and boil at
constant temperature. So, it is not possible to separate the components by fractional distillation
Azeotropic mixtures are formed by non-ideal solutions. They are of two types:
1. Maximum boiling azeotropes: They have bp either greater than
both the components. The components of this solution show
large negative deviation from Raoult’s law at a specific
composition. Eg: Nitric acid and water (concentration of 68%
HNO3 + 32% water by mass)
2. Minimum boiling azeotrope: bp less than both the
components. The components of this azeotropic solution show
large positive deviation from Raoult’s law at specific
composition. Eg: Ethanol-Water (concentration of 95%
ethanol)
Both components have bp greater than a minimum boiling azeotrope
To separate an azeotrope :
1. Azeotropic distillation: Azeotropic distillation is one in which a solvent is added that will
increase the volatility between the light and the heavy component. The interaction of a
solvent called agent with one of the components changes the volatility of the solvent and the
component to which it is attached. The azeotropic solvent should have volatility near the
major component desired in the overhead product. A good example of azeotropic distillation
is water and ethanol mixture (95% ethanol). Cyclohexane is one of the solvents used for
production of anhydrous ethanol. It is used as an entrainer. The ternary mixture forms a
ternary azeotrope with a different ethanol concentration, which allows ethanol to
concentrate in the bottom stream. This azeotropic mixture leaving the overhead is separated
to recover the entrainer and the ethanol.
30. (b) Shown below is the equilibrium diagram of a minimum boiling azeotrope. Identify the
azeotropic composition in the graph, the region where the equilibrium value k<1, and the region
where the value of k > 1.
The point ‘m’ where the diagonal line and the
equilibrium line intersects each other is the azeotropic
composition of the liquid mixture.
The part of the curve on the left of the point m, is a region where k<1, that is B is richer in the vapor
phase.
The part of the curve on the right of the point m, is a region where k>1, that means the vapor is
richer in component a.
