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A valve tray distillation column has a total condenser and a total reboiler. The column
operates at 200 kPa pressure and there is an estimated pressure drop of 10 kPa.
The column is fitted with valve trays. Comment on what would be the impact of
changing these to sieve type trays?
[4]
Chart for K value data, Gilliland correlation graph and a sheet of preliminary design
equations are supplied separately. Note that not all the equations are needed for the
present calculations.
K Value Chart
Fenske Equation:
x x d w
ln A B ln A B
x B D x A W w A dB
=
Or
Nmin = Nmin
ln α Ave, A,B ln α Ave,A,B
i =n i=n
α i,r x Fi α i,r x Di
∑ (α
i=1 i,r − q)
= (1 − q) R min + 1 = ∑ (α
i=1 i,r − θ)
Kirkbride’s Correlation
m W x ( x LK ) W
2
ln = 0.206 ln HK
p LK
D x F ( x HK )D
Gilliland Chart
Examination Solution
Heriot-Watt University, School of Engineering and Physical Sciences,
Chemical Engineering.
Subject : Lecturer/Author: Module Code:
Unit Operations A GW B40EA
Question Number: Exam Diet: Checked by: Co-ordinator:
1 Solution S2 GBT
Page 1 Of 3 Diagram Required: Other Data/ Special Stationery Required:
Gililand chart, No
equation sheet
a) Temperature in condenser
Molar compositions for distillate and bottoms product
Total condenser
Key components d b
LK N-HEXANE 0.548 0.014
HK N-HEPTANE 0.004 0.491
Minimum reflux is said to be 0.8. Use the standard multiplier (1.2x Rmin but
anything reasonable will be acceptable) R=0.96.
b) Outline what you consider is the reason that this column appears to have a
large number of stages, and a proportionally large reflux ratio. List in the
order of priority, recommendations you would to adjust these numbers.
Explain the background to your selection. [5]
where
K Value Table
Pressure 1 atm
Solution
Part a)
Using the liquid rate back to the column and the composition of that liquid we
get a mass balance round the 1st tray is then
Constant molar overflow would suggest internal liquid rate is 418, vapour rate
460.
SECOND TRAY
Temp 76
Rate mf Ki x=y/Ki
N-PENTANE 94 0.2025 3.2679 0.0620
BENZENE 285 0.6116 0.9079 0.6737
CYCLOHEXANE 48 0.1039 0.8859 0.1173
TOLUENE 38 0.0820 0.3714 0.2206
466 1.0736
Material balance
Vapour to
Distillate Liquid from 2nd tray next tray
N-PENTANE 19 26 45
BENZENE 18 282 300
CYCLOHEXANE 3 49 52
TOLUENE 1 92 93
490
Answer to Part i)
Temperature 67 76
X 0.151785714
(N-Nmin)/(N+1) 0.473589348
Nmin 41
Nactual 79
c) The large number of trays is due to the close volatility of benzene and
cyclohexane – there is not much of a difference across all temperature
ranges at this pressure. The difference in relative volatility should
become higher if the pressure were reduced. So in order to reduce the
number of stages, the 1st recommendation is to run the column under
vacuum conditions.
Examination Question
Heriot-Watt University, School of Engineering and Physical Sciences,
Chemical Engineering.
Subject : Lecturer/Author: Module Code:
Unit Operations GW B40EA
Question Number: Exam Diet: Checked by: Co-ordinator:
3 Robin Westacott
Page 1 of 2 Diagrams Required: Other Data/Special Stationery Required:
HYSYS output
The product stream from the drier and quench tower following an ethylene
cracker is to be separated into essentially pure components. Composition of
this mixture is given below.
a) Two options for separating the hydrogen are proposed; i) to distil the
mixture, ii) to use a series of 4 flash separation stages. Discuss the
relative merits of both process stages, mentioning the impact on
refrigeration duty needed. [4]
Examination Solution
Heriot-Watt University, School of Engineering and Physical Sciences,
Chemical Engineering.
Subject : Lecturer/Author: Module Code:
Unit Operations GW B40EA
Question Number: Exam Diet: Checked by: Co-ordinator:
3 Solution 2S2 2011-2012
Page 1 of 1 Diagrams Required: Other Data/Special Stationery Required:
a) The principle issue of distillation with the hydrogen feed is to reduce the temperature
of the column sufficiently low as to condense the methane and potentially the
hydrogen. But given that the hydrogen is the most volatile of all components, it will
not be possible to pull the temperature sufficiently low enough for any condenser. In
any case, to cool the mixture sufficiently low, a special refrigeration loop would be
needed.
The best option will be to use a series of flash separation stages to drive of the
majority of the hydrogen before it reaches the column. Even with this column, you
would need a refrigerant that can be pulled down low enough to condense methane.
(in practice you can expand high pressure hydrogen or high pressure methane to
drop its temperature which may provide the right level of temperature).
rd
Note: Students have encountered this type of distillation before in 3 year HYSYS
modelling class.
b) I) Heuristics would say that you separate the mixture based on
a. Flow rate – sepatate the components with the largest flow first – in this case
you would separate the ethylene methane from the rest of the mixture.
b. Components which are difficult to separate should be left in their own column
– in this case, separating the C2’s and C3’s and C4’s in their own columns
would be preferable
c. Separate those that are fouling – we have a relatively clean system here
operating at low temperatures. This is unlikely to cause issues due to fouling.
iii) Marginal vapour flowrates
Assume the sequence will be done at the mid range temperature of -100 deg
Step 1: Collect the flowrates and K values. Work out the relative volatility wrt the least
volatile component
Now work out the marginal flows for all possible key components
A B C D E F G H theta term
lk/hk
Now work out the marginal flow for the direct sequence
A B C D E F G H Marginal Flow
A/BCDEFGH 1.2136 0.1278 0.0140 0.0053 0.0002 0.0005 1.3613
B/CDEFGH 1.9799 0.2097 0.0791 0.0032 0.0070 2.2788
C/DEFGH 3.4462 1.2833 0.0500 0.1098 4.8893
D/EFGH 4.3454 0.1559 0.3413 4.8426
E/FGH 1.1660 2.4852 3.6512
F/GH 5.6531 5.6531
G/H 0.0000 0.0000
Total 22.6763
A B C D E F G H Marginal Flow
ABC/DEFGH 5.0115 10.3473 3.4462 1.2833 0.0500 0.1098 20.2481
AB/C 5.1853 5.1853
A/B 0.0000
E/FGH 1.1660 2.4852 3.6512
F/GH 5.6531 5.6531
G/H 0 0.0000
Total 34.7378
i) There is no information on the HYSYS printout which says the state of the feed.
This is deliberate. Students have to read through the column profile pages to
work out the details. The “Column Profile Flows” – which is in several places to
work out that show that the feed is 2055 kmols/hr, but the liquid flow to the next
tray is 2447, liquid from the top section is 518.7. This means that 2447-
518.7=1928 must come from the feed and must be liquid. Vapour from the bottom
section is 591.9 and through the top section is 718.7 which means 718.7-591.9 =
127 comes from the feed. So the feed is a two phase mixture. Feed enters on
plate 7 as indicated in the column profile summary
ii) The printout contains tables but no profile pots so the task here is to see if the
students realise that they can visualise the column profile from the given data set.
Analysing the tables however will give them sufficient information:
a. The overall liquid and gas rates don’t change very much from plate 9-15. This
is not surprising due to constant molar overflow. The temperatures however
remain very similar over the same range -57 on plate 9 and -57 on plate 14.
b. The composition profile (mapping the liquid/gas composition for each
component) shows that over this range there is little activity in the column
and hence no separation taking place, To further optimise this column, the
recommendation is to reduce the number of trays in this section.
a) Process interface unit: computer unit in distributed control system that does
most of the basic /regulatory control in a typical plant
b) Throughput manipulator: control system that sets that flow that control the
production rate of a plant
e) Selective control: control system in which the control system takes in and
compares data from various places but bases the controller output on a
selection.
Level 4
Business planning/logistics
Level 3
Advanced control
PI controller so use
∆t
∆m = K c en − en −1 + en
τI
t = 0:
e n-1 = 10
e n = 10
∆t
so ∆m = K c en − en −1 + en = 1(10 − 10 + 1 / 20 * 10) = 0.5
τI
m n = m n-1 +∆m= 50+1=50.5
t=1
e n-1 = 10oC=10%TO
e n = 9.8
∆t
so ∆m = K c en − en −1 + en = 1(9.8 − 10 + 1 / 20 * 9.8) = −0.2 + 0.49 = 0.29
τI
m n = m n-1 +∆m= 50.5+0.29=50.79
t=2
∆t
so ∆m = K c en − en −1 + en = 1(10 − 10 + 1 / 20 * 10) = 0.5
τI
m n = m n-1 +∆m= 50+1=50.5
t=1
e n-1 = 10oC=10%TO
e n = 9.8
∆t
so ∆m = K c en − en −1 + en = 1(9.8 − 10 + 1 / 20 * 9.8) = −0.2 + 0.49 = 0.29
τI
t=2
e n-1 = 9.8oC=9.8%TO
e n = 9.71
∆t
so ∆m = K c en − en −1 + en = 1(9.71 − 9.8 + 1 / 20 * 9.71) = −0.09 + 0.49 = 0.40
τI
m n = m n-1 +∆m=50.79 + 0.40=51.19
t=3
e n-1 = 9.71
e n = 9.65
∆t
so ∆m = K c en − en −1 + en = 1(9.65 − 9.71 + 1 / 20 * 9.71) = −0.06 + 0.48 = 0.42
τI
m n = m n-1 +∆m=51.19 + 0.42=51.61
t=4
e n-1 = 9.65
e n = 9.61
∆t
so ∆m = K c en − en −1 + en = 1(9.61 − 9.65 + 1 / 20 * 9.61) = −0.04 + 0.48 = 0.44
τI
m n = m n-1 +∆m= 51.61+0.44=52.05
t=5
e n-1 = 9.61
e n = 9.58
∆t
so ∆m = K c en − en −1 + en = 1(9.58 − 9.61 + 1 / 20 * 9.58) = −0.03 + 0.48 = 0.45
τI
m n = m n-1 +∆m= 52.05+0.45=52.50
50
40
%CO/%TO
Controller output
30
Humidity
20
10
0
0 250 500 750 1000 1250 1500 1750 2000
Time (seconds)
a) K=(50-25)/(20-15)=25/5=5%TO/%CO
b) ok is 250 sec-50sec=200 sec. 150-200 from Fit 3 is also ok (see part c))
c) Fit3: 0.283*25+25 = 32.1; t1= 350sec
0.632*25+25 = 40.8; t2=550 sec
Tau=3/2(550-350)= 300 sec
to=550-300=150.
d) Kc = 0.9/5*300/150=0.36; tauI=3.33*to=500.
RC
FA
FC
FB FC
V2
LC
PC
V1
FC
LC
V3
LC
AC
V1 V2
LC FC
FC
V1 V2
LC LC
AC
a) Determine the actual reflux ratio and actual number of stages in this column.
[5]
b) What would you expect to happen to the condenser and reboiler temperature
if the column pressure were to increase? As a consequence, what would you
expect to happen to the distribution of the heptane and the size of the
column? [5]
c) Determine the composition of the light and heavy key components in the
bottoms product. [15]
K values for the three components are shown graphically. Gilliland correlation graph
and a sheet of preliminary design equations are supplied separately. Note that not
all the equations are needed for the present calculations.
K Value Chart
Fenske Equation:
x x d w
ln A B ln A B
x B D x A W w A dB
=
Or
Nmin = Nmin
ln α Ave, A,B ln α Ave,A,B
i =n i=n
α i,r x Fi α i,r x Di
∑ (α
i=1 i,r − q)
= (1 − q) R min + 1 = ∑ (α
i=1 i,r − θ)
Kirkbride’s Correlation
m W x ( x LK ) W
2
ln = 0.206 ln HK
p
LK
D x F HK D
( x )
Gilliland Chart
Examination Solution
Heriot-Watt University, School of Engineering and Physical Sciences,
Chemical Engineering.
Subject : Lecturer/Author: Module Code:
Unit Operations A GW B40EA
Question Number: Exam Diet: Checked by: Co-ordinator:
1 Solution S2 GBT
Page 1 Of 3 Diagram Required: Other Data/ Special Stationery Required:
equation sheet No
st
1 Underwood equation says
i =n
α i,r x Fi
∑ (α
i=1 i,r − q)
= (1 − q)
Trial and error- guess theta which should lie between average alpha for LK and HK
Component Avg AlphaFeed CompGuess thetaGuess thetaGuess thetaGuess theta
1.15 1.3 1.164 1.170
N-HEXANE 1.38 0.400 2.361 6.551 2.515 2.576
CYCLOHEXANE 1.00 0.400 -2.667 -1.333 -2.435 -2.359
N-HEPTANE 0.61 0.200 -0.226 -0.177 -0.220 -0.218
Rmin+1= 5.824
Rmin 4.824
b) If the column pressure were increased, then the condenser and reboiler temperatures
would also have to increase to keep the same distribution of light and heavy keys. From the K
value graph, the relative volatility of the heptane would reduce and therefore there would be
no change in the distribution. The column may have to be larger though to accommodate the
cyclohexane that would be in the distillate.
x x
ln A B
x B D x A W
The fenske equation is Nmin =
ln α Ave, A,B
Since we know the minimum number of stages and the top and bottom temperatures. We
have
(Note - the answers will depend on the value for this exponential term)
eq1
and we have
Therefore
Hence
Hence
Therefore the key composition of the bottoms products are
Examination Question
Heriot-Watt University, School of Engineering and Physical Sciences,
Chemical Engineering.
Subject : Lecturer/Author: Module Code:
Unit Operations GW B40EA
Question Number: Exam Diet: Checked by: Co-ordinator:
2 S2
Page 1 of 2 Diagrams Required: Other Data/Special Stationery Required:
The HYSYS output, attached separately, shows details of a first attempt at a rigorous
column separating a mixture of propane, butane, pentane and hexane. Use this
information to answer the following:
a)
i) Determine the average liquid and vapour rates inside the column and hence
provide a sketch diagram of the column showing all the key flowrates. [4]
ii) Sketch a diagram of stages 9,10 and 11 and include the internal liquid and
vapour flowrates. [4]
iii) Verify the thermal state of each feed stream by calculating the q value. [4]
b) Assuming a combined feed that is saturated liquid, calculate what the minimum
reflux ratio should be for this column.
[5]
c) Calculate the minimum number of stages needed for this column [4]
d) Construct a temperature and key component ratio plot for this column and hence
outline what further changes could be done with the column [4]
Temperature Pressure Net Liq Net Vap Net Feed Net Draws
Stage
(C) (kPa) (kgmole/h) (kgmole/h) (kgmole/h) (kgmole/h)
Condenser 6.176 150 6.983 --- --- 40.2
1 7.842 150 6.87 47.18 --- ---
2 8.385 150 6.807 47.07 --- ---
3 8.648 150 6.776 47.01 --- ---
4 8.777 150 40.47 46.98 35 ---
5 13.85 150 40.54 45.67 --- ---
6 16.51 150 39.83 45.74 --- ---
7 20.11 150 38.66 45.03 --- ---
8 25.43 150 37.41 43.87 --- ---
9 31.87 150 36.05 42.61 --- ---
10 39.65 150 111.2 41.25 65 ---
11 42.23 150 111.5 51.38 --- ---
12 45.06 150 112 51.7 --- ---
13 47.72 150 112.7 52.23 --- ---
14 49.97 150 113.1 52.87 --- ---
15 52.07 150 113 53.35 --- ---
Reboiler 55.47 150 --- 53.2 --- 59.8
Feed Compositions
Propane n-Butane n-Pentane n-Hexane
Feed 1 0.2857 0.5714 0.1429 0.0000
Feed 2 0.0000 0.1538 0.5385 0.3077
The HYSYS output, attached separately, shows details of a first attempt at a rigorous
column separating a mixture of propane, butane, pentane and hexane. Use this
information to answer the following:
a)
i) Determine the average liquid and vapour rates inside the column and hence
provide a sketch diagram of the column showing all the key flowrates. [4]
ii) Sketch a diagram of stages 9,10 and 11 and include the internal liquid and
vapour flowrates. [4]
iii) Verify the thermal state of each feed stream by calculating the q value. [4]
65+35.05=100.05 which means that vapour has to have been condensed from tray
11. Therefore the feed at tray 10 is subcooled.
b) The rigorous column shows a reflux ratio of 0.174. Using appropriate methods,
calculate what the minimum reflux ratio should be for this column.
[5]
Short cut calculations deal with 1 feed to the column so work out the feed
composition from the HYSYS data provided
Distillate Bottoms
Propane 0.0653 0
Butane 0.8417 0.01 LK
Pentane 0.093 0.6555 HK
Hexane 0 0.3344
d) Construct a temperature and key component ratio plot for this column and
hence outline what further changes could be done with the column [4]
7
LK/HK Ratio
0
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17
Stage
Temperature Plot
60
50
40
Temperature
30
20
10
0
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17
Stage
The key component ratio plot for the top of the column looks as if that section is ok – the key
plot flattens out around the feed stage and steppes either side. The fact that key component
ratios are changing on either side of the feed tray indicates the column is working ok. Below
nd
the 2 feed stage however, the column is not really doing much.
The temperature profile shows 3 distinct sections which you would expect. The issue is that
the end points at the reboiler and condenser are not probably as steep as normal.
Since the split is around the inner two components – then its likely this column needs more
stages. Looking at the compositions of each feed stream, from that view point it seems that
Examination Question
Heriot-Watt University, School of Engineering and Physical Sciences,
Chemical Engineering.
Subject : Lecturer/Author: Module Code:
Unit Operations GW B40EA
Question Number: Exam Diet: Checked by: Co-ordinator:
3
Page 1 of 2 Diagrams Required: Other Data/Special Stationery Required:
HYSYS output
Recovery in
Feed Distillate
(kmol/hr)
Methane 40 99
Ethane 50 0.1
Propane 35 0
N-Butane 35 0
Table of K values
Examination Solution
Heriot-Watt University, School of Engineering and Physical Sciences,
Chemical Engineering.
Subject : Lecturer/Author: Module Code:
Unit Operations GW B40EA
Question Number: Exam Diet: Checked by: Co-ordinator:
3 Solution 2S2 2011-2012
Page 1 of 1 Diagrams Required: Other Data/Special Stationery Required:
b) Show that the reboiler utility temperature will be close to 40ºC [5]
Composition Distillate
xd Ki alpha
METHANE 0.999 1.0316 43.69 LK
ETHANE 0.001 0.0236 1.00 HK
PROPANE 0.000 0.0018 0.08
N-BUTANE 0.000 0.0002 0.01
Composition Bottoms
xb Ki alpha
METHANE 0.003 13.2355 6.52 LK
ETHANE 0.415 2.0295 1.00 HK
PROPANE 0.291 0.5099 0.25
N-BUTANE 0.291 0.1442 0.07
Key components d b
LK METHANE 0.999 0.003
HK ETHANE 0.001 0.415
d) If the minimum reflux ratio is 0.142, determine the actual number of stages in
this column. [4]
Set actual reflux = 1.2xRmin
Actual reflux ratio 0.173
(R-Rmin)/(R+1) 0.0246
(N-Nmin)/(N+1) 0.6
Check by correlation 0.673
Actual number of stages 14.5
CO2 would freeze in the methane column and therefore block internals. Its
normally removed to avoid this.
f) LNG feed would contain more than 4 components. Outline one method that
could be used to determine the sequence of columns to be used to separate
a typical LNG feed mixture. [3]
There are 2 potential methods to separate out a mixture of more than 2 components:
• Heuristics
• Minimum vapour flowrate
These would be used to select possible sequences for further investigation by rigorous
column simulation tools.
a) PID:
Steam
FC1 AT1
TT1
Reactor feed
Reactor
Products
Heat exchanger
Block diagram:
Pfeed
G2
Tfeed
G2
F1
Aset1 T1
A1
Km GAc1 GTC1 GFC1 Gv GHeat exchanger Greactor
HFT1
HTT1
HAT1
b)
Condensor
Cooling water
Separator
Condensate
LC
Steam PC
Evaporator
Feed Pump
AC
Product
c)
Cyclone
Feedwater
Solid feed
to sump
FC
Mill
AC
Water feed LC
Motor SC
Pump
d)
Steam doesn’t affect level so Y2 is level, X1 is flow. Steam and flow affect temperature. Y1 must be
temperature. X2 must be steam.
a)
2 o
GJ ( s ) = C / (kg/s)
2.5s + 1
0.6 o
GR (s) = C / oC
13s + 1
100%TO / 50 o C 2
H R (s) = = %TO / o C
s +1 s +1
b)
C(s)
HR(s)
C(s)
d) 1+OLTF=0
2 0.6 2
OLTF= G c G v G J G R H R so 1 + OLTF = 0 = 1 + Gc * 0.12 * * *
2.5s + 1 13s + 1 s + 1
e) i.
TT2 TC2
∞ Coolant
Product
ii
TRsp(s) TR(s)
Km Gc1 Gc2 0.12
f. Gc2=2
2 0.48
* 0.12 * 2
G= 2. 5 s + 1 = 2. 5 s + 1 =
0.48
=
0.48
2 0.48 2.5s + 1 + 0.48 2.5s + 1.48
1+ * 0.12 * 2 * 1 1 +
2.5s + 1 2.5s + 1
TRsp(s) TR(s)
Km Gc1
Characteristic equation:
i. T= Tu= (105-2)/6 =17.2; Kcu = 3.39. wu= 2pi/T = 0.366. Pretty close.
e. i. PID Ziegler Nichols Quarter decay based on autotune.
Proportional- K T T
integral-derivative, K c' = cu τ 'I = u τ 'D = u
1.7 2 8
PID*
Kc=3.35/1.7=1.97
Tu
τ 'I =
2
16.4/2=8.2 min
Tu
τ 'D =
8
=16.4/8=2.05
Ii Use Tyreus-Luyben
Tyreus-Luyben controller settings for a more conservative response
Kc τI τD
PI 0.31K cu 2.2T u -