Distillation 2

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Design of Distillation Column

Design of Distillation Colum

Table of Contents

Introduction 3

Flowsheet 4

Limitations 5

Applicability 6

Theory 7

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Design of Distillation Colum

Introduction

This report describes the design of distillation process. This will enable the reader to
understand the necessary components along with distillation calculations. Distillation is a process
that separates two or more components into an overhead distillate and bottoms. The bottoms
product is almost exclusively liquid, while the distillate may be liquid or a vapor or both.

The separation process requires three things. First, a second phase must be formed so that both
liquid and vapor phases are present and can contact each other on each stage within a separation
column. Secondly, the components have different volatilities so that they will partition between
the two phases to different extent. Lastly, the two phases can be separated by gravity or other
mechanical means. Distillation differs from absorption and stripping in that the second phase is
created by thermal means.

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Design of Distillation Colum

Flowsheet

The distillation column contains one feed stream and two product streams. The feed
contains a mole percent of the light component, ZF. The product stream exiting the top
has a composition of XD of the light component. The product stream leaving the bottom
contains a composition of Xb of the light component. The column is broken in two
sections. The top section is referred to as the rectifying section. The bottom section is
known as the stripping section.

The top product stream passes through a total condenser. This effectively condenses all of
the vapor distillate to liquid. The bottom product stream uses a partial reboiler. This
allows for the input of energy into our column.
Limitations

Azeotropes: An azeotrope is a liquid mixture which when vaporized produces the same
composition as the liquid. If the mixture is azeotropic, then more advanced types of
separation must be considered. More information on azeotropes maybe found in Douglas,
Section 7.3.

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Design of Distillation Colum

Solids: If the material to be separated is high in solids, or contains tars or resins that could
plug or foul a continuous unit, then a batch separation should be considered (Perrys,
1997).

Optimum Pressure:
1. Vacuum operation: Use of a vacuum should be considered for heatsensitive compounds or
polymerizable materials. Vacuum is usually not used unless required, e.g., a low bottoms
temperature is needed to avoid thermal decomposition.
2. Distillation column is above atmospheric pressure: Column shell should be thicker to
withstand pressure of the column.
3. If the column pressure required to accomplish overhead condensation with cooling water
is less than 250 lb/in2, then the column pressure should give an average temperature
driving force of 5-15*C in the overhead condenser.
4. If the column pressure required accomplishing overhead condensation with cooling water
is greater than 250 lb/in2, then consider an alternative of using a refrigerant on the
overhead and running the column at a lower pressure.
Optimum Temperature Differences in Reboilers and Condensers:
1. Reboiler temperatures should be kept low enough to avoid bottoms degradation and/or
fouling.
2. Common temperature differences used for heat exchange across reboilers and condensers
are shown in the following table:

Temp, K
Condenser:
Refrigeration 3-10
Cooling Water 6-20
Pressurized Fluid 10-20
Boiling Water 20-40
Air 20-50
Reboiler:
Process Fluid 10-20
Steam 10-60
Hot Oil 20-60
Applicability

Distillation is the least expensive means of separating mixtures of liquids.

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Design of Distillation Colum

If relative volatilities of components is less than 1.1, distillation becomes very expensive
and extraction or reactive distillation should be considered.
Theory

Section 1. Graphical Determination of a Distillation Column Design

Step 1. Determine Process Operation Variables

Assumed feed rate, composition, purity of distillate and bottoms, and the quality of the
feed are known.
Perform overall material and component balances to determine the compositions of the
distillate and bottoms.

F*ZF=XD*D+XB*B (1)
F=D+B (2)
where
F Feed rate of input stream
ZF Composition of light component in feed
XD *Mole Fraction of light in distillate
XB *Mole Fraction of light in Bottom
D Total distillate amount
B Total bottom amount
*If more than two components, these values are the light-key and heavy-key component.

Step 2. Determine the Minimum Reflux Ratio

This graphical approach is determined using the McCabe-Thiele Method for binary
mixtures. The ratio of reflux flow to distillate flow is called the reflux ratio.
Assumptions

The following assumptions are implied when using this method (McCabe, 1993):
a. Constant Molal Overflow. The molar flow rates of the vapor and liquid are nearly
constant in each section of the column. This also ensures the operating lines are straight
lines.

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Design of Distillation Colum

b. Heat Effects are negligible. For example, heat losses to and from the column are small
and neglected.
c. For every mole of vapor condensed, another mole of liquid is vaporized.
d. The liquid and vapor leaving the tray is in equilibrium with the vapor and liquid entering
the tray.

Procedure

If an equilibrium curve is not given, draw a y-x diagram (y representing the vapor phase
and x the liquid). The equilibrium curve can be obtained by relating the relative volatility
to the composition of the liquid:
y = a*x/(1+x(a-1)) (4)
This shows the bubble-point and dew point of a binary mixture at constant pressure. An
equilibrium line describes the compositions of the liquid and vapor in equilibrium at a
fixed pressure. The equilibrium line crossing the forty-five degree line is an indication of
an azeotropic mixture. An azeotrope is a liquid mixture which when vaporized produces
the same composition as the liquid. If the mixture is azeotropic, then more advanced types
of separation must be considered.

Forty Five Degree Line

1. Draw the diagonal line connecting the points (0.0,0.0) to (1.0,1.0).


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Design of Distillation Colum

This is your forty-five degree line.

Feed Line (q-Line)

1. The feed line can be constructed by locating the point on the fortyfive degree line that
corresponds to the feed composition. This point can be extended with a slope of q/(q-1)
where q is the feed quality. The feed line can be directly plotted through the following
equation:

y=q/(q-1)X - ZF/(q-1) (5)

Upper Operating Line

3. Draw the operating line for the enriching section. First find the desired top product
composition (on the x-axis) and locate the corresponding point on the forty-five degree
line. Connect this point to the point where the equilibrium cure and the feed line intersect.
This is the upper operating line. The y intercept of this line is equal to XD/(R+1). The
following equation can be used to determine the minimum reflux:

Rmin=(XD/yintercept ) 1 (6)

Lower Operating Line

4. Draw the operating line for the stripping section. First find the desired bottom product
composition (on the x-axis) and locate the corresponding point on the forty-five degree
line. Draw a line from this point to the intersection of the equilibrium curve and the feed
line. This is your lower operating line. The slope of this line is equal to
(Vbmin+1)/Vbmin where Vb is the boilup ratio. The boilup ratio is the fractional amount
of liquid that is boiled back into the column to the amount of liquid leaving.

Step 3. Choose Actual Reflux Ratio:

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Design of Distillation Colum

As the reflux ratio increases, the number of trays and thus the capital cost of the column
decreases. However, as a trade-off, an increase in reflux ratio will also increase the vapor
rate within the tower, thus increasing expenses such as condensers and reboilers (4). Most
columns are designed to operate between 1.2 and 1.5 times the minimum reflux ratio
because this is approximately the region of minimum operating cost. Therefore, based on
first estimates, the operating reflux ratio is equated so that (Douglas, 1988):
Ractual =Rmin* 1.2 (7)

Step 4. Determine the Minimum Number of Trays

Upper/Lower Operating Line at Actual Reflux

1. Redraw the upper and lower operating line using the actual reflux ratio. Plot the point XD/
(R+1) and draw a line to the XD. The equation of the upper operating line is:
y=(R/R+1)*X+XD/(R+1) (8)
The equation for the lower operating line can be drawn by connecting the XB to the
intersection of the feed line and the upper operating line. The equation of the lower
operating line is:
y=((VB+1)/VB)*X+XB/VB (9)

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Design of Distillation Colum

Determine Number of Trays

2. Starting from composition of the distillate, a horizontal line is drawn to the equilibrium
curve. This line demonstrates the first tray.
3. From the previous intersection, drop vertically until the upper operating line is obtained.
Follow step two to determine next tray.
4. Continue stepping until the liquid composition ends equals the desired bottom
composition.
5. The total number of steps is equal to the theoretical number of trays.

6. When high conversions are desired, the stepping method may cause difficulties. In
these cases the Kremser equation should be used.


1 m V * ((yin ye,out ))+ m m V
V

N = ln L yout ye,out ln L

L
(10)

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Design of Distillation Colum

where
N Number of trays in unreadable region
m Slope of the line in unreadable region
V/L R/(R+1)
yin Conveniently chosen point below unreadable region
yout XD for rectifying section
ye,out m*XD+b (where b is the y intercept of new equil. line)

Step 5. Determine Actual Number of Trays

This is determined by taking the quotient of the number of theoretical trays to the tray
efficiency. Typical values for tray efficiency range from 0.5 to 0.7 (Douglas, 1988). These
values depend on the type of trays being used, as well as the internal liquid and vapor flow
rates.

Nactual = Ntheory /e (11)

Step 6. Principal Dimensions of the Column (Diameter/Height):

A design guideline that should be used is that the height of the column should not be
higher than 175 feet.
Height-to-diameter ratio should be less than 20 to 30.
Packed towers are used when the column has a small diameter (1.5 ft or less) or area (1.77
ft2 or less) rather than plate towers.

Either plate or packed towers may be used when the column diameter is between 1.5-4.5
ft (or area, 1.77- 15.9 ft2).

If the tower is higher than 190 ft, then a design with smaller tray spacing should be
considered (Douglas, 1988).

The tower height can be related to the number of trays in the column. The following
formula assumes that a spacing of two feet between trays will be sufficient including
additional five to ten feet at both ends of the tower. This includes a fifteen percent excess
allowance of space (Douglas, 1988).
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Design of Distillation Colum

Htower = 2.3 Nactual (12)

Before we can determine the tower diameter, we need to determine the vapor velocity. The
vapor velocity can be derived from the flooding velocity. To limit our column from
flooding, we choose a velocity 50-80 percent of flooding velocity (Douglas, 1988):

V = 1.2 G
(13)
where
V Vapor Velocity
G Density of the mixture

The diameter of the tower is relatively insensitive to changes in operating temperature or


pressure. The main determinant of the diameter is the vapor velocity. The desired vapor
velocity is dependent on the limitations of undesired column flooding.

M
Where
DT Diameter of tower

V Vapor velocity
MG Molecular weight of gas
m Molar density

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Design of Distillation Colum

Section 2. Analytically Determining the Specifications for a Distillation Column

Step 1. Determine Process Operation Variables

Assumed feed rate, composition, purity of distillate and bottoms, and the quality of the
feed are known.
Perform overall material and component balances to determine the compositions of the
distillate and bottoms.

Step 2. Determine the Minimum Reflux Ratio

Underwood Equation

The Underwood equation approximates the minimum reflux ratio (Douglas, 1988). The
following equation can be used for multi-component systems with constant relative
volatility. Relating mass balances and VLE equations, the following equation was derived
for which can be calculated.

F*(1-q)= ((a i * zi)/ (a i -f )) (15)

where
F Feed
q Feed quality
i Relative Volatility

zi Composition of component (i) in Feed

Through the previous expression, can be obtained in a polynomial expression. This


expression can be used to solve for . Only the that falls between the relative
volatilities of the components should be considered. The can be used to obtain the
minimum amount of vapor (Vmin):

Vmin = (a i * Dxi)/ (a i -f )) (16)

From a mass balance and the definition of reflux:

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Design of Distillation Colum

Lmin = Vmin D

Rmin = Vmin / D (17)

Step 3. Choose Theoretical Reflux Ratio

As the reflux ratio increases, the number of trays and thus the capital cost of the column
decreases. However, as a trade-off, an increase in reflux ratio will also increase the vapor
rate within the tower, thus increasing expenses such as condensers and reboilers (Douglas,
1988). Most columns are designed to operate between 1.2 and 1.5 times the minimum
reflux ratio because this is approximately the region of minimum operating cost.
Therefore, based on first estimates, the operating reflux ratio for the analytically method is
equated so that (Douglas, 1988):
RTheor = 1.2 *Rmin (18)

Step 4. Determine Theoretical Number of Trays

Modification of the Fenske Equation

A simplified approximate equation can be used to determine the number of trays


(Douglas, 1988). This is an expression for the minimum number of trays, assuming total
reflux and constant relative volatility. This equation takes into account the reflux ratio.

N= ln SF
ln

1 +1R * ZF

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Design of Distillation Colum

(19)

where

SF = *
(20)

Fractional recovery of light in the distillate Fractional recovery of light in the


bottom Relative volatility
R Reflux ratio
ZF Mole ratio of light component in feed
Step 5. Determine Actual Number of Trays:

This is determined by taking the quotient of the number of theoretical trays to the tray
efficiency. Typical values for tray efficiency range from 0.5 to 0.7 (Douglas, 1988). These
values depend on the type of trays being used, as well as the internal liquid and vapor flow
rates.
Nactual = N/e (21)

Step 6. Principal Dimensions of the Column (Diameter/Height):

A design guideline that should be used is that the height of the column should not be
higher than 175 feet.
Height-to-diameter ratio should be less than 20 to 30.
Packed towers are used when the column has a small diameter (1.5 ft or less) or area (1.77
ft2 or less) rather than plate towers.

Either plate or packed towers may be used when the column diameter is between 1.5-4.5
ft (or area, 1.77-15.9 ft2).
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Design of Distillation Colum

If the tower is higher than 190 ft, then a design with smaller tray spacing should be
considered (Douglas, 1988).
Height of Column

The tower height can be related to the number of trays in the column. The following
formula assumes that a spacing of two feet between trays will be sufficient including
additional five to ten feet at both ends of the tower. This includes a fifteen percent excess
allowance of space (Douglas, 1988).

Htower = 2.3 Nactual [ft] (22)

Vapor Velocity

Before we can determine the tower diameter, we need to determine the vapor velocity. The
vapor velocity can be derived from the flooding velocity. To limit our column from
flooding, we chose a velocity 60 percent of flooding velocity (Douglas, 1988). This is
assumed in the following equation:

1.2
V=
G
(23)
where
V Vapor Velocity G Density of the Gas

Diameter of Tower

The diameter of a tower is relatively insensitive to changes in operating temperature or


pressure. The main determinant of the diameter is the vapor velocity. The desired vapor
velocity is dependent on the limitations of undesired column flooding. This equation
allows for a twelve percent surplus in area (Douglas, 1998).

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Design of Distillation Colum

DT = .0164 (V) * (MG/ r m )^.25 (24)


where

V Vapor Velocity
MG
m Molar density
Section 3. Determining the Cost of Column and Components
All cost estimates formulas were taken from (Douglas, 1988).

Step 1. Cost of Column


Capital Cost
The following approximates installed cost and purchased cost for the shell and trays. This
cost relates the diameter, height, and design variables of the column. The design variable
is a correction used to allow specificity of the column pressure and material.

C c = M & S * 120 D T * H 0 .8 * (218 + Fc )


280

(25)
where
Cc Cost of shell and trays
Fc Design considerations for the column
DT Diameter of column
H Height of column
Step 2. Cost of the Reboiler
Capital Cost
The installed cost of the reboiler heat exchanger is:
C r =
M & S * 328 * H v 0.65 * V 0.65
280 11250
(26)
where
Cr Cost of reboiler
Hv Heat of vaporization of bottoms

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Design of Distillation Colum

V Rate of Boilup
Operating Cost
If we use steam to supply the heat for the reboiler, the temperature driving force must be
constrained to less than 30-45 F to prevent film boiling. We are also assuming a high
value of heat transfer coefficient because the heat transfer between a condensing vapor
and boiling liquid is high. The steam required is:

Ws = HHvs * V

(27)

Cs = 8.74*10 3 *(SteamCost)* HV * V
(28)
where
Ws Amount of steam needed
Cs Cost of steam
Hv Heat of vaporization
Hs Heat of saturation
V Mass flow rate
Step 3. Cost of Condenser
Capital Cost

If we assume the cooling water is available at 90 F and a heat transfer coefficient of 100,
the heat transfer area of the condenser heat exchanger is:

Ac=((DHv/3000) ln (Tb-90/Tb-120)) V (29)


where
Ac Area of condenser heat exchanger
Hv Heat of vaporization
Tb Bubble point of distillate V Mass flow rate

The installed cost of the heat exchanger for condensing:

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Design of Distillation Colum

Cc=(M&S/280)*101.3*(2.29+Fc)*Ac0.65 (30)
where
Cc Cost of condenser Fc Design considerations correction factor

Operating Cost

If we assume the cooling water is available at 90 F and a heat transfer coefficient of 100,
the amount of cooling water needed for the condenser and the associated cost is:

Wc=(DHv/30)V (31)

Cc=3.26 10-4*(Cooling water cost)(DHv)(V) (32) where

Wc Amount of cold water to condenser


Cc Cost of condenser
Hv Heat of vaporization
V Mass flow rate
Step 4. Total Cost of Column

The total annualized cost is the sum of capital cost divided by the payback period plus the
yearly operating cost.

TAC = Capital Cost / Payback Period + Operating Cost (33)

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Design of Distillation Colum
References

1. Seader, J. and Henley, E. Separation Process Principles. John Wiley & Sons, 1998, Chapters 7 and 8.
2. McCabe, Warren. Unit Operations of Chemical Engineering, Fifth Edition.
McGraw-Hill, Inc, 1993, Chapters 18 and 19.
3. Distillation Column Design. Copyright 1997. http://lorien.ncl.ac.uk/ming/distil/distil0.htm
4. Douglas, James. Conceptual Design of Chemical Processes. McGraw-Hill, Inc., 1988, Section A.3.
5. King, C. Judson. Separation Processes, Second Edition. McGraw-Hill, Inc., 1980, Chapters 4-6.

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