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ChE511-Equipment Design
5ChE-B November 5, 2017
INTRODUCTION
Distillation is one the most common unit operations used in the industries. It is a
process wherein the desired component is separated from the initial mixture by selective
condensation or evaporation. This separation process could be in partial or complete
depending on the type of distillation use [1].
One of the types of distillation and is one of the main process in the propylene glycol
industry is the use of flash distillation, also known as equilibrium distillation. This happens
when a definite fraction of the liquid feed is vaporized and is in equilibrium with the
residual liquid. The process also involves reducing the pressure suddenly to lower the
boiling point of the component (hence, it is called flash distillation) [2].
Sieve tray distillation column are only used for continuous/ flash distillation
processes. Sieve trays are design to look like the usual sieves use in mechanical
separations. The sieve trays have metal plates with holes wherein the vapor passes
straight upward through the liquid on the plate. The effectiveness of the tray depends on
the number and size of the holes and the arrangement of it [3].
In the propylene glycol industry, a 99.6% final product purity of propylene glycol
from glycerol, which is harvested directly from biodiesel productions, will be the main
concerned. The crude glycerol that can be used as the feed, cannot be fed directly to the
reactor because it contains chloride and sulfate salts. If they were to enter the reactor,
these salts would cause corrosion. Therefore, removing these salts using a distillation
column is a necessity [5].
The distillation column is designed to process the feed from the heat exchanger
which contains 15,000 kg/hr crude glycerol, with a composition of 51.6% water and 1.7%
methanol (Usual composition of crude glycerol found in the market) at its dew point. The
objective of the equipment is to completely separate the methanol from the glycerol and
reduce the water content to 20% of the original (bottoms: glycerol-20% of the water from
the feed; distillate: methanol-80% of the water from the feed).
INPUT CONDITIONS
Crude glycerol is being processed in the column to recover pure glycerol in the
bottoms. In this process, the following assumptions were made:
1. Since methanol has a lower boiling point than that of water, the two mixtures could
be considered as one system. Once the water hits its boiling point, methanol had
already reached its boiling point, therefore, complete separation of methanol had
already occurred.
2. The efficiency was estimated using the OConnell Equation. (McCabe-Thiele
method cannot be use because of the distance of the equilibrium curve from the
diagonal)
3. The vapor feed enters at its dew point which is at 113.5oC.
4. The crude glycerol contains 46.7%(w/w) glycerol, 51.6%(w/w) water and
1.7%(w/w) methanol
5. 15-20% by weight of the original water content will be retained in the bottoms. This
is the optimal concentration to be used in the trickle bed reactor due to viscosity
concerns.
6. The vapor-liquid diagram with its data was obtained from www.vle-calc.com
[Appendix A].
TEMPERATURE x1 (water) y1 (water)
C mol/mol mol/mol
299.075 0 0
273.803 0.01 0.416587
254.717 0.02 0.690761
239.457 0.03 0.8304
226.967 0.04 0.900621
207.635 0.06 0.959137
193.233 0.08 0.979931
181.988 0.1 0.988869
162.088 0.15 0.996434
148.903 0.2 0.998467
139.501 0.25 0.999209
132.51 0.3 0.999537
127.188 0.35 0.999701
123.089 0.4 0.999791
119.93 0.45 0.999844
117.514 0.5 0.999877
115.699 0.55 0.999898
114.377 0.6 0.999911
113.456 0.65 0.99992
112.854 0.7 0.999924
114.498 0.75 0.99991
114.498 0.8 0.99991
114.498 0.85 0.99991
111.87 0.9 0.999923
111.713 0.92 0.999924
111.502 0.94 0.999927
111.221 0.96 0.999937
111.046 0.97 0.999945
110.842 0.98 0.999957
110.603 0.99 0.999974
109.593 1 1
Material Balances:
Overall Material Balance: F=D+B
Solute Balance: Fxf = DxD + BxB
Other balances: V=L+D
L = L + qF
V = V + (1-q)F
EQUIPMENT DESIGN THEORETICAL CALCULATIONS
Table 1 shows the composition of the feed at its dew point. This were the basis for
all calculations.
Table 1. Feed Composition
Molecular
Feed (kg/hr) Feed (mol/hr) % by mole
Weight
Glycerol 7,005 92 76.141 14.81
Water 7,740 18 430 83.64
Methanol 255 32 7.96875 1.55
The dew point of the feed was obtained using Figure 2 wherein the composition of
the water (0.8364) was used.
Table 2 shows the composition of the distillate and the bottoms. Take note that the
water in the bottoms satisfy the 15-20% by weight range.
Table 2. Distillate and Bottoms Composition
Distillate Distillate (% by Bottoms Bottoms (%
(mol/hr) mole) (mol/hr) by mole)
Glycerol 0 0 76.1413 46.96
Water 344 97.7 86 53.04
Methanol 7.96875 2.3 Trace Trace
TOTAL 351.96875 162.1413
The flowrates of L and V in the rectifying section was also computed. The values
obtained were 211.18125 mol/hr and 563.15 mol.hr, respectively. L and V was also
computed. The values obtained were 211.18125 mol/hr and 49.0452 mol/hr, respectively
(See Appendix B for the calculations of Table 2 and the flowrates).
The minimum number of stages was calculated using the Fenske-Underwood
Equation [4].
(1 )
log( )
( )
1
= log()
Equation 1
Where:
Substituting all values from Equation 1, the minimum number of stages calculated
was 0.999999 or 1 stage.
The minimum reflux ratio for the system was also calculated using Equation 2. This
equation is use when feed is at the dew point [4].
( + 1) = 1 Equation 2
Where:
The calculated minimum reflux ratio from the above equation was 0.5. As a rule of
thumb, economically optimum reflux ratio is about 1.2 times the minimum. Therefore, the
reflux ratio is 0.6.
In getting the theoretical number of stages, the Erbar and Madd graph was used
where [4]:
= +1 = 0.375; = +1 = 0.333
Figure 3 Plates reflux correlation of Erbar and Madd
Plotting the z and y-axis, a 0.45 value for the x-axis was obtained. Equating
this to = , the number of theoretical stages will be 2.22 or 3 stages.
For the tray efficiency, the OConnell correlation was used [6].
Where:
Substituting the values to Equation 3, the efficiency was 12.828%. Using the
efficiency, the actual number of trays can be calculated using the formula:
= Equation 4
All calculations for the equipment design is seen in Appendix D. The calculations
were based on Seader and Henley and Flooding considerations using the Handbook
assuming the column is a plate column.
Material of Construction
Operation: Continuous
Design Data:
Sapp, K., Lawson, J. (2007). Batch Distillation Theory. USA. University of Florida.
Retrieved September 22, 2017, from
http://www.che.ufl.edu/ren/course/4404L/BD/BD%20Theory%20Handout.pdf
[3] Process & Operation Engineer, Egypt. Follow. (2015, February 25). Types and design
of the towers trays. Retrieved November 03, 2017, from
https://www.slideshare.net/MohamedSalah69/types-and-design-of-the-towers-trays
[4] Brannan, C. (n.d.). Rule of Thumb for Chemical Engineers (3rd ed.). Gulf Professional
Publishing.
[5] Chatterjee, K., Hall, K., & Tell, S. (n.d.). Glycerol to Propylene Glycol
[Abstract]. University of Pennsylvania: Scholarly Commons. Retrieved November 3,
2017, from
http://repository.upenn.edu/cgi/viewcontent.cgi?article=1025&context=cbe_sdr
[6] SALUNKE, D. B. (2006). AN OCONNELL TYPE CORRELATION FOR PREDICTION
OF OVERALL EFFICIENCY OF VALVE TRAY COLUMNS (Unpublished master's
thesis). Pune University .
McCabeThiele method. (2017, September 03). Retrieved September 22, 2017,
from https://en.wikipedia.org/wiki/McCabe%E2%80%93Thiele_method
Kim, K., Diwekar, U. (2005, April 27). Chapter 5: Batch Distillation. USA. p.112-114.
What is the Difference Between Reflux & Distillation? (n.d.). Retrieved September
25, 2017, from http://sciencing.com/difference-between-reflux-distillation-
5953384.html
Albarede, F., Hofmann, A. W., & Condomines, M. (n.d.). The Rayleigh distillation
equation.Geochemistry,220-221. doi:10.1017/cbo9781139165006.017
Th: Define and use K values, relative volatility, and x-y diagrams. (n.d.). Retrieved
November 03, 2017, from
http://pillars.che.pitt.edu/student/slide.cgi?course_id=12&slide_id=72.0
APPENDIX B
Distillate composition:
1
77400.80 = 6192 =
18
1
255 = .
32
Bottoms composition:
1
77400.20 = 1548 =
18
1
7005 = .
92
=+
= 0.6 = L =211.18125mol/hr V= 563.15mol/hr
= = . mol/hr
=+ V = 49.0452mol/hr
APPENDIX C
(1 )
=
(1 )
Where:
Substituting the values given, the relative volatility of the mixture is 37.60896.
APPENDIX D
1. Tray Spacing: For reasons of accessibility, tray spacings are made 20-24in.
3. Tray Holes and Hole Area: Sieve tray holes 0.25-0.50 in. dia, hole area being
10% of the active cross section
4. Tray Thickness: In general, tray thickness is about gauge 10 (0.134 in; 3.40
mm) for carbon steel
5. Pressure Drop: Pressure drop per tray is of the order of 747 Pa (3 in. water) or
689.5 Pa (0.1 psi).
7. Weir Length: The chord length will normally be between 0.6 and 0.85 of the
column diameter.
8. Hole Pitch: Normal practice is to use a hole pitch to hole diameter ratio between
2.2 to 3.8.
Therefore:
MAWP = 5 + 25 psig
= 30psig
Design Temp. = 113.5oC + 10oC = 123.5oC
Other concerns: Pressure vessel head: Both are hemispherical, nozzles for feed,
bottoms and distillate product, and skirt thickness.
APPENDIX E
This section displays the detailed parts of a sieve tray distillation column with its
nomenclature and definition.