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Column schematic diagram

CFO Bobbert
10464842

L/D =
1.3
100kmol/h Feed at stage
27

Enriching Section
(Total condenser)
50.04kmol/h Distillate:
99.9% methyl acetate
0.01% isopropyl

Quality q = 1.235 sub


cooled liquid
50% methyl acetate

Stripping Section (Partial


reboiler)
49.96kmol/h Bottoms (stage
55):

V*/B =
2.775

0.02% methyl acetate

Column Summary
Design Constraints
Stage 1 Temperature
Distillate fractional recovery
Stage 55 Temperature
Bottoms fractional recovery
Average Column temperature
Column Dimensions
Diameter
Height
Tray thickness
Plate Details
Hole diameter
Tray type
Tray spacing
Tray Packing
Supports
External structure
Internal structure (column
frame)
Internal structure (tray)
Materials
Shell
Insulation
Pipes
Entries and exits
Join type
Heat Exchangers
Condenser
Condenser volume flow rate
Reboiler
Reboiler volume flow rate

330.24 K
0.999
361.66 K
0.999
345 K
1.3m
35.53m
1.3cm
1.27cm
Equilateral triangular sieve
4.83cm
No packing
Cylindrical cone skirt frame
Vertical beams bound with
rings
Straight diameter bar under
tray
Stainless Steel
Fibreglass
Stainless Steel
Welded
Baffle shell side condenser
0.657m3/s
Thermosiphon
3
6.74* 10
m3/s

Contents
i Column schematic diagram
ii Column summary
1 Methods for design
1.1 McCabe-Thiele Analysis
1.1.1External Mass Balance
1.1.2Feed Line Calculation
1.1.3Top Operating Line
1.1.4Bottom Operating Line
1.2 Gilliland Correlation for Number of Stages
2 Aspen simulation
2.1 Efficiency Calculation
2.1.1Average temperature
2.1.2Average temperature at feed composition
3 Mechanical design of the column
3.1 Column diameter calculation
3.2 Column height calculation
3.3 Sieve tray design
3.4 Tray Hydraulics
3.5 Materials for construction
3.6 Heat exchanger design

1. Methods for design


1.1 McCabe-Thiele Analysis
The McCabe-Thiele analysis is a method of approximating the
amount of stages required by means of a graphical analysis
with the use of some boundary operating equations. To obtain
these equations the following assumptions are made from
(Wankat, 2012:106), otherwise known as the Constant Molal
Overflow (CMO) assumptions:
The column is adiabatic
The specific heat changes are negligible compared to the
latent heat changes
|Hj+1 Hj| << and |hj+1 hj| <<
Latent heat of vaporization, v, is constant and is
concentration independent
These conditions can be summed up by having parallel
saturated liquid and vapour lines on the enthalpyconcentration graph
These assumptions result in constant mass flow rates in the
column. The flow rates in the enriching section and stripping
section will be different due to the feed stream.
1.1.1External Mass Balance
To evaluate the mass balance we take a system envelope
intersection only the feed (F), bottoms (B) and distillate (D)
streams. This results in the overall mass balance
F=B+D
And the most volatile component balance
Fz1 = BxB + DxD
Solving for these simultaneously with the given conditions
results in
D = 50.04kmol/h
4

B = 49.96kmol/h

1.1.2Feed Line Calculation


To find the feed line gradient we need to calculate the quality,
q, of the feed stream. Wankat defines the quality as
q (H hf)/(H h)
Where H is the feed tray vapour enthalpy, hf, is the feed
enthalpy and h is the liquid enthalpy on the feed tray. With the
following data (Yaws, 2009):

H|l,1 = 6060.07 kJ/kmol


H|l,2 = 8690.80 kJ/kmol
1 = 32.23 kJ/mol
2 = 30.61 kJ/mol

Calculate the mole average of the feed stream:


H|l,avg = 7375.44 kJ/kmol
avg = 31420 kJ/kmol
This results in q = 1.235. Now the slope of the feed line can be
calculated as
Slope = q/(q 1)
= 5.26
And the y intercept can be calculated by
y intercept = 1/(q 1)
= -2.13
The feed line can now be given by the function
y = 5.26x -2.13

Equilibrium Data for MeOAc(1) and IPAC(2) system at


101.3 kPa.
1
0.9
0.8
0.7
0.6
Y

0.5

y=x

Feed Line

L/Vmin

0.4
0.3
0.2
0.1
0
0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

Figure 1 VLE curve with Feed line and L/V)min line (Li
Xiao, 2013)
1.1.3Top Operating Line
The minimum gradient for the top operating line can now be
determined from the above figure.
L/V)min = 0.464
Now L/D)min can be determined from
L/D)min = [L/V)min]/[1 - L/V)min]
=0.866

As per Wankat, a scaling factor is used to obtain a L/D)real, the


maximum value of 1.5 is chosen to affect a greater separation.
L/D)real =( factor) L/D)min
= 1.5*0.866 = 1.3
And so the operating gradient of the top operating line is
determined to be
L/V)real = 0.565
Solving for the intercept with the point of x D on the y = x line
yields
y = 0.565x + 0.435
1.1.4Bottom Operating Line
Before the bottom operating line can be calculated an internal
mass balance must be done to find the vapour and liquid flow
rates in the enriching section.
L = L/D)real*D = 65.05 kmol/h
V = V/L)real*L = 115.13 kmol/h
Now a mass balance around the feed stage can be done
V

V*
**

L*

Figure 2 Feed stage stream balance


V* = (V + L*) (F + L)
= 138.63 kmol/h
7

And
L* = 188.55 kmol/h
Now the gradient, L*/V*)real can be determined. With the
intercept of the top operating line with the feed line and the
gradient of the bottom operating line, the function for the
bottom operating line can be calculated as
y = 1.36x 0.00003
Operating Lines for the system MeOAc(1) and IPAC(2) system at
101.3 kPa.
1
0.9
0.8
0.7

0.6

y=x

0.5

Feed Line

0.4

BOL

TOL

0.3
0.2
0.1
0
0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

Figure 3 VLE data with the feed line and the top and
bottom operating lines
From the above Figure 3, with the reflux ratio as 1.3, when the
stages were stepped off by hand there were 31 stages including
the partial reboiler with the optimum feed stage at 19.
1.2 Gilliland Correlation for Number of Stages
8

Gilliland (1940) developed and empirical correlation between


the number of stages to the finite L/D ratio. This correlation
was later modified by Liddle (1968). The first equation used is
the Fenske equation from (Wankat, 2012:240) for the minimum
number of stages, Nmin,
ln (
N min =

( FR A ) dist( FRB ) bot


)
(1( FR A ) dist )( 1( FR B ) bot )
ln( AB )

Where ( FR A ) dist

is the fractional recovery of methyl acetate

in the distillate while ( FRB ) bot

is the fractional recovery of

isopropyl acetate in the bottoms. These values were


calculated as follows
(FRA)dist =

x D D 0.999(50.04)
=
=
F zA
100(0.5)

(FRB)bot =

(1x B )( B) ( 0.9998 )(49.96)


=
=0.999
F zB
(100)(0.5)

0.999

The relative volatility, AB , was calculated to be 2.9. Using


these values in the Fenske equation gives
Nmin = 12.97 13 stages
The Abscissa, which corresponds to the x-value on Figure 4,
is equivalent to

Abscissa =

D
L/

min
(L/ D)

Abscissa = x = 0.18

Figure 4 Liddle (1968) modified Gilliland Correlation

Using the solid line and the x-value, a y-value is read off to be
0.42.
y=

NN min
N +1

N = 23 stages
Although this value is low, it is not unexpected because the
maximum L/D was chosen for the column which increases
column efficiency. Also this method assumes 100% efficiency
and is therefore only a guide for further simulation.

10

2. Aspen Simulation
Using the results from the McCabe-Thiele method and the
Gilliland correlation, the estimated number of stages should be
in the range of 25 to 35 stages. The downfall of these methods
is that they do not take efficiency into account.
2.1 Efficiency Calculation
The overall efficiency of the column can be calculated from the
figure and the following equation (Wankat, 2012:366)
E0 = 0.52782 0.27511log10() + 0.044923[log10()]27

11

Figure 5 OConnell correlation for plate efficiency


The relative volatility, , and the average viscosity, , need to
be determined at the columns average operating conditions.
The average temperature can be calculated via two methods
(Wankat, 2012:368):
2.1.1Average temperature Tavg = 0.5*(Ttop + Tbot)
Tbot = 361.66 K
Ttop = 330.24 K
Tavg = 345.95 K
From the aspen Txy diagram
@345.95K
x1 = 0.399
y1 = 0.658
1 = (y/x)/[(1-y)/(1-x)] (Wankat,2012:368):
1 = 2.898
2.1.2 Average T at feed composition x 1 = 0.5
12

T @ x1 = 0.5 = 341 K
y1 = 0.74
2 = 2.846
avg = (1 + 2)/2 = 2.872
Now the viscosity of the feed, , is calculated by using the
following equation
(Wankat, 2012:368)
lnmix = x1ln1 + x2ln2
Pure component viscosities at the feed stage temperature of
341K are
1 = 0.364 cP
2 = 0.515 cP
mix = 0.433 cP
E0 = 0.502
Using the () value of 1.24, the graph reads an efficiency of
about 45%. Enough data has been determined to do the Aspen
simulation. The results are as follows

Number of Feed
stages
stage
45
23
24
25
46
23
25
47
24
25
26
48
23

Distillate
fractional
recovery
0.9974
0.9974
0.997
0.9977
0.9976
0.998
0.998
0.9978
0.998
13

24
0.9981
25
0.9982
50
24
0.9984
25
0.9985
26
0.9985
52
25
0.9987
26
0.99875
27
0.99876
54
25
0.9988
26
0.9988
27
0.99894
55
27
0.99902
28
0.9989
Table 2 Aspen simulation of stages and distillate
fractional recovery
From the above table it is seen that the number of stages
required will be 55 with the optimum feed stage at stage 27.
The maximum reflux ratio is kept because the column is
expected to be very tall as it will increase the efficiency more
cost effectively than having a taller column.

3 Mechanical Design of the


column
3.1 Column Diameter Calculation
Before we can calculate the column diameter we need to
calculate the velocity of the vapour streams between the
stages that will cause flooding of the column due to
entrainment (Wankat, 2012:369):
14

uflood = Csb,f(/20)0.2[(l v)/v)


Where is the surface tension in dynes/cm and Csb,f is the
capacity factor which is a function of the flow parameter and is
given in (Wankat, 2012:370)
log10Csb,f = 0.94506 0.70234log10Flv 0.22618(log10Flv)2
This equation is for the chosen 24 inch tray spacing to allow for
workmen to service the column. The flow parameter is a
function of the densities, l and v, as well as the mass flow
rates, Wl and Wv, of the liquid and vapour. Flow rates in lb/h
while densities are in lb/ft3. (Wankat, 2012:369)
Flv = FP = (Wl/Wv)(v/l)
From these equations and making the assumption that we have
pure methyl acetate on the top stage and pure isopropyl
acetate on the last stage, we can find the flooding velocity of
these stages.
Paramete
r

Top Stage (methyl


acetate )

Bottom Stage (isopropyl


acetate)

T (K)

330.24

361.66

l (lb/ft3)

55.23

49.47

v (lb/ft3)

0.225

0.169

(dyne/cm
)

20.5

15

Wl (lb/h)

10623.76

42453.12

Wv (lb/h)

18802.66

31213.35

Table 1 Data summary for enriching and stripping


sections
Top stage calculation
15

Flv = 0.036063
Csb,f = 0.39578
uflood = 6.22ft/s
Bottom stage calculations
Flv = 0.079495
Csb,f = 0.35790
uflood = 5.77ft/s
Now that the flooding velocities have been determined we can
calculate the operation velocity, uop, which must be a fraction of
the flooding velocity and can be determined by (Wankat,
2012:370):
Uop = (fraction)*uflood
The value of 0.75 as suggested by Jones and Mellbom (1982)
(Wankat,
2012:370)
Top uop = 4.665 ft/s
Bottom uop = 4.328 ft/s
The column diameter is then determined from the equation
(Wankat, 2012:371):
D = [4VMv/(vuop*3600)]
Where V (lbmol/h) is the molar flow rate, Mv is the vapour molar
mass (lb/lbmol) and is the fraction of the cross sectional area
for vapour flow above the tray. From the literature (Wankat
2012), is usually between 0.85 and 0.95. The value of was
chosen to be 0.9

16

Top D = 2.65ft = 0.808m


Bottom D = 4.09ft = 1.247m
The bottom diameter is prevalent here and so a rounded up
value of 1.3m will be chosen for a safe design.
3.2 Column Height Calculation
The column height is estimated by the amount of trays
multiplied by the tray spacing and an extra two metres for any
extra features that are required.
Height 55stages x 0.6096m tray spacing + 2m
= 35.53m
3.3 Sieve Tray Design
To design the sieve tray holes and their spacing in the column
the source Wankat (2012:377) was used. Assuming that the
system is non-fouling, a half inch (1.27cm) diameter hole is
suggested as a first guess. Since the system components are
of the same functional group and the column operates above
the fusion temperatures of the components, this diameter is
chosen. The spacing between the holes is recommended to be
3.8d0 (4.83cm). The spacing between the holes and the inlet
downcomer as well as the column shell is recommended to be
two to three inches, so the average of 2.5 inches (6.35cm) is
chosen. Also the spacing between the holes and the
downcomer weir needs to be further to allow for vapour-liquid
disengagement; therefore a spacing of four inches (10.16cm) is
chosen.
Equilateral triangular punching patterns were selected because
it is the cheapest of the sieve designs and there is no
information indicating that another pattern is required. The
minimum tray thickness must be equal to the hole diameter of
0.5 in (1.27m). To keep the design simple, a straight
segmented downcomer with a cross flow stacking is chosen.
17

To calculate the number of holes per tray and the area of the
downcomer, the procedure in Wankat (2012:377-378) is
followed.
The total area of each tray can be calculated by
Atot = 0.25D2
= 1.327m2
The expression for the active area is given by
Aactive Atot(2 1)
= 1.062m2
The area covered by the holes can be calculated with the
average value of = 0.1.
Aholes = Aactive
Aholes = 0.106m2 = 1.141ft2
Now the number of holes can be calculated
Number of holes = Aholes/(0.25d02)
= 837 holes
And the downcomer area
Ad = (1 )Atot
= 0.133m2
With this information it is possible to determine the velocity of
the vapour through the holes. The maximum vapour velocity in
the column is below the feed stage at 305.63lbmol/h. This is
used so that the maximum value is determined.
uholes,v = VMv/(3600vAholes)
= 44.965ft/s
18

3.4 Tray Hydraulics


To determine the length and angle of the wier we need to use
the data in Wankat (2012:378) to get a correlation for the weir
length with respect to . For the chosen value of = 0.9 which
corresponds to 0.726 for the lweir/D from table 10.1 in Wankat
(2012:378)
lweir = 0.726*D
= 0.944m = 3.1ft
Now we can get the angle projected from the middle of the tray
to the edges of the downcomers with the equation (Wankat,
2012:379):
Ad = 0.5r2( sin)
Solving for yields
= 1.6755 rad = 96
The downcomers need to be design in such a way that the
liquid can flow down with enough ease so that there will not be
excessive pooling of liquids that can cause flooding of the
column. Once again the stripping section is used to calculate
the hydraulics in the column due to the high flow rates.
The method for analysis in Wankat (2012:378-381), allows
approximation of the entrainment mechanics within the stages
of the column. Below is a representation of the pressure heads
on sieve trays.

19

Figure 6 Stage hydraulic head schematic


The head of clear liquid in the downcomer, hdc, can be
determined from the sum of the other heads present on the
stage and by the equation:
hdc = hp,dry + hweir + hcrest + hgrad + hdu
The first term is the head of liquid that is required to overcome
the pressure drop of the vapour on a dry tray is approximated
by
hp,dry = 0.003vo2v(water/l)(1 2)/C02
where vo is the previously calculated velocity of the vapour
through the holes in ft/s, while the orifice coefficient, C o, can be
determined from the Hughmark and OConnell (1957)
correlation. do/ttray is taken as its minimum as one.
Co = 0.85032 0.04231(do/ttray) + 0.0017954(do/ttray)2
= 0.8098
hp,dry = 1.95 in = 4.95 cm
The next term for weir height is specified Wankat (2012:379) to
be at least 0.5 inch but usually between 2 and 4 inches,
whatever term is chosen the condition is that it is high enough
that the opposite downcomer always retains liquid. Just to be

20

safe the maximum value of 4 inches is chosen due to the lack


of contradictory information. Therefore
hweir = 4 in = 10.16cm
The height of the liquid crest over the weir, hweir, can be
calculated by the Francis weir equation (Wankat, 2012:379)
hcrest = 0.092Fweir(Lg/lweir)2/3
where Lg is the total liquid flow rate and is equivalent to the
previously calculated liquid flow rate, L, and the entrainment, e,
and can be determined from the equation for fractional
entrainment as follows
= e/(L + e)
in conjunction with the figure below

Figure 7 Entrainment correlation from Fair (1963)


(Wankat, 2012:373)
21

The flow parameter, Flv, has previously been calculated as


0.079495. (Wankat, 2012:372) recommends that a 75% flood
value should have negligible correction for entrainment. Using
these values, , is read off from Figure 7 to be 0.035.
= e/(L + e)
0.035 = e/(414.95 + e)
e = 15.05 lbmol/h
Lg = L + e = 430 lbmol/h = 111.92 gal/min
The other unknown, Fweir, is a modification factor to correct for
the curvature of the column wall in the downcomer and can be
found using the following figure

Figure 8 Weir correction factor, Fweir, for segmented


weirs from Bolles
(1946) (Wankat, 2012:380)
The two ratios required for interpretation for the figure are
lweir/D = 0.726
Lg/lweir = 36.1
Using these values a result for Fweir is approximately 1.22.
Substituting these results into the hcrest expression:

22

hcrest = 1.23 in = 3.12 cm


Typically on sieve trays the liquid gradient, h grad, is very small
and therefore neglected. The remaining term, hdu, is the
frictional loss due to flow in the downcomer and under the
downcomer onto the tray. The following empirical equation is
used (Wankat, 2012:372)
hdu = 0.56(Lg/449Adu)2
with
Adu = (gap)lweir = 0.26 ft2
Where Adu is the flow area under the downcomer apron and
there is typically a 1 inch gap above the tray.
hdu = 0.515 in = 1.31 cm
With these head calculations done, hdc can now be calculated as
hdc = 7.965 in 7.7 in = 3.03 cm
Due to operation of the column, the liquids are aerated and as
a result are less dense which results in the expected height
being higher than that of clear liquid. The expected height can
be estimated from the equation as follows Wankat (2012:380)
hdc,aerated = hdc/dc
with dc as the relative froth density. A value of 0.5 is assumed
to be adequate for normal operation Wankat (2012:380)
hdc,aerated = 15.4 in = 39.12 cm
It is recommended that the tray spacing must be greater than
hdc,aerated to avoid downcomer flooding. With the tray spacing at
24 inches, it is greater than hdc,aerated.
As per Wankat (2012:380), downcomers are designed for liquids
to have a minimum residence time of three to four seconds on
the tray. The residence time for a straight segmented
downcomer can be calculated by
23

tres = Adhdcl3600/(LgMM12)
= 11.1 sec
This is above the minimum residence time of 4 seconds.
Acceptable tray operation is bound by two limits, excessive
entrainment and excessive weeping. To ensure that operation
is above the weep point, an approximate analysis on the heads
balance at the hole is done. (Kessler and Wankat, 1987)
estimated that
hp,dry + h 0.10392 + 0.25119x 0.021675x2
The terms on the left represent the heads amounting to surface
tension, while x = hweir + hcrest + hgrad represents a function
depending on the liquid head. This equation holds for the
chosen value of 0.1. The surface tension head can we
estimated by Wankat (2012:380)
h = 0.04/(ld0)
=0.0243 in = 0.062 cm
And
x = 5.23
1.95 + 0.0243 0.10392 + 0.25119(5.23) 0.021675(5.23)2
1.9743 0.8248
There will be no weeping in the bottom section of the column.
3.5 Materials for construction
The inner and outer shell as well as the trays and piping will be
made from stainless steel because the system is non-corrosive
and stainless steel is a cheap and commonly used material
(Sinnot, 2005:296). Also the shell must be able to endure outside
conditions which stainless steel is suitable for. Fibreglass
sheets will be used to insulate the column because apart from
24

it being a good insulator, fibreglass is UV stable and resistant to


weathering
3.6 Heat Exchanger Design
For the partial reboiler, a thermosiphon design will be used
because this design is cheap and operates well at high
circulation rates. Also this design can be cleaned easily.
The total condenser will be a baffled shell side condenser and
this was chosen because it is the industry standard and has a
simple design.

References
Fiberglass Reinforced Plastic Composite Panels | Crane
Composites [ONLINE] Available at:
http://www.cranecomposites.com/_pdfs/6907_corp_lit.pdf.
Knovel, 2012. Knovel Solvents - Physical Properties, s.l.:
ChemTec Publishing.
Selection and Design of Condensers | Gerard Hawkins Academia.edu. 2014. Selection and Design of Condensers |
Gerard Hawkins - Academia.edu. [ONLINE] Available at:
http://www.academia.edu/3642011/Selection_and_Design_of_Co
ndensers
Selection of Reboilers for Distillation Columns | Gerard Hawkins
- Academia.edu. 2014. Selection of Reboilers for Distillation
Columns | Gerard Hawkins - Academia.edu. [ONLINE] Available
at:
http://www.academia.edu/3642019/Selection_of_Reboilers_for_
Distillation_Columns
25

Li Xiao, Q.-l. W. H.-x. W. T. Q., 2013. Isobaric vaporliquid


equilibrium data for the binary system methyl acetate +
isopropyl acetate and the quaternary system methyl acetate +
methanol + isopropanol + isopropyl acetate at 101.3 kPa. Fluid
Phase Equilibria, Issue 344, pp. 79-83.
Sinnott, R., 2005. Stainless steel. In: Coulson and Richardson's
Chemical Engineering Volume 6 - Chemical Engineering Design
(4th Edition). s.l.:Elsevier, p. 296.
Wankat, P. C., 2011. Chapter 10 . In: Seperation Process
Engineering. s.l.:Prentice Hall, p. 359-383.
Yaws, C. L., 2009. Yaws' Handbook of Thermodynamic
Properties for Hydrocarbons and Chemicals. s.l.:Knovel.

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