Separations

ChEN 4253 Design I

Chapter 19
Terry A. Ring
University of Utah
 Simple Separation Units
• Flash
– Quench
• Liquid-liquid decantation
– Liquid-liquid Flash
• Sublimation
– Solid/Vapor Flash
• Crystallization
• Filtration
Use of Separation Units
 Separation
Reaction
Hydrodealkylation of
Toluene

T+H2B+CH4
side reaction
2B Biphenyl+H2

Reactor Effluent
T=1,350F
P = 500 psia
 Reactor Effluent
Reaction Conditions
T=1,350F
P = 500 psia Component kmole/hr
Hydrogen 1292
Methane 1167
Benzene 280
Toluene 117
Biphenyl 3
Total 2859
After Flash to 100F @ 500 psia
Effluent Vapor Liquid
Component kmole/hr kmole/hr kmole/hr
Hydrogen 1292 1290 2
Methane 1167 1149 18
Benzene 280 16 264
Toluene 117 2 115
Biphenyl 3 0 3
Total 2859 2457 402

Recycled Reactants
 Separation
• Vapor Separation
– CH4 from H2
• Liquid Separation
 Further Separation
What separation units should be used?
• Liquid Separation
– Toluene, BP=110.6ºC
– Benzene, BP=80.1ºC

• What happens to the Methane (BP= -161.5ºC) and Biphenyl

(BP=255.9ºC) impurities?
• Gas Separation
– Hydrogen
– Methane

• what happens to the Toluene and Benzene impurities?

Direct Distillation Sequence
 Criteria for the Selection of a
Separation Method
• Energy Separation • Mass Separation
Agent (ESA) Agent (MSA)
– Phase condition of feed – Phase condition of feed
– Separation Factor – Choice of MSA
– Cost Additive
I – Separation Factor
C 1 – Regeneration of MSA
I
C – Cost
SF  II
2
C 1 Phases I and II,
II
C 2 Components 1 and 2 (light key and heavy key)
Distillation
Distillation
 Plate Types
• Bubble Cap Tray • Sieve Tray
 Packed Towers
• Random Packing

• Structured Packing

Note: Importance of
Distributor plate
 Distillation
α=KL/KH
• Relative Volatility

• Equilibrium Line
 Distillation
• Rectifying Section
– R= reflux ratio
– V=vapor flow rate
• Stripping Section
– VB= Boil-up ratio

• Feed Line
Minimum Reflux Ratio
McCabe-Thiele
Step Off Equilibrium Trays
 Marginal Vapor Rate
• Marginal Annualized Cost~ Marginal Vapor Rate
• Marginal Annualized Cost proportional to
– Reboiler Duty (Operating Cost)
– Condenser Duty (Operating Cost)
– Reboiler Area (Capital Cost)
– Condenser Area (Capital Cost)
– Column Diameter (Capital Cost)
• Vapor Rate is proportional to all of the above
 Short cut to Selecting a Column
Design
• Minimum Cost for Distillation Column will
occur when you have a
– Minimum of Total Vapor Flow Rate for column
– Occurs at
• R= 1.2 Rmin @ N/Nmin=2 or see Fig 19.1
– V=D (R+1)
• V= Vapor Flow Rate
• D= Distillate Flow Rate (=Production Rate)
• R=Reflux Ratio
Figure 19.1
 How To Determine the Column
Pressure given coolant
• Cooling Water Available at 90ºF
• Distillate Can be cooled to 120ºF min.
• Calculate the Bubble Pt. Pressure of Distillate
Composition at 120ºF
– equals Distillate Pressure
– Bottoms Pressure = Distillate Pressure +10 psia delta P
• Compute the Bubble Pt. Temp for an estimate of
the Bottoms Composition at Distillate Pressure
– Give Bottoms Temperature

• Not Near Critical Point for mixture

 Design Issues
• Packing vs Trays
• Column Diameter from flooding consideration
– Trays, DT=[(4G)/((f Uflood π(1-Adown/AT)ρG)]1/2 eq. 19.11
• Uflood= f(dimensionless density difference), f = 0.75-0.85 eq. 19.12
– Packed, DT =[(4G)/((f Uflood πρG)]1/2 eq. 19.14
• Uflood= f(flow ratio), f = 0.75-0.85 eq. 19.15
• Column Height
– Nmin=log[(dLK/bLK)(bHK/dHK)]/log[αLK,HK] Fenske eq.19.1
– N=Nmin/ε (or 2 Nmin/ ε)
• Column Height = N*Htray
• Tray Height = typically 1 ft (or larger), 2 inch weir height
• Packed Height = Neq*HETP (or 2 Neq*HETP)
– HETP(height equivalent of theoretical plate)
– HETPrandom = 1.5 ft/in*Dp Rule of thumb eq. 19.9
• Tray Efficiency, ε = f(viscosityliquid * αLK,HK) Fig 19.3
• Pressure Drop
• Tray, ΔP=ρLg hL-wier N
• Packed, ΔP=Packed bed (weeping)
 Tray Efficiency

19.3

μL * αLK,HK
Costing
 Column Costs
• Column – Material of Construction gives ρmetal
– Pressure Vessel Cp= FMCv(W)+CPlatform
– Height may include the reboiler accumulator tank
– Tray Cost = N*Ctray(DT)
– Packing Cost = VpackingCpacking + Cdistributors
• Reboiler CB α AreaHX
• Condenser CB α AreaHX
• Pumping Costs – feed, reflux, reboiler
– Work = Q*ΔP
• Tanks
– Surge tank before column, reboiler accumulator, condensate accumulator
– Pressure Vessel Cp= FMCv(W)+CPlatform
CPI
 Distillation Problems
• Multi-component Distillation
– Selection of Column Sequences
• Azeotropy
– Overcoming it to get pure products
• Heat Integration
– Decreasing the cost of separations
 Problem
• Methanol-Water Distillation
• Feed
– 10 gal/min
– 50/50 (mole) mixture
• Desired to get
– High Purity MeOH in D
– Pure Water in B
 Simulator Methods - Aspen
• Start with simple distillation method
– DSDTW or Distil
• Then go to more complicated one for sizing
purposes
– RadFrac
– Sizing in RadFrac
• Costing
 Simulation Methods- ProMax
• Start with 10 trays (you may need up to 100 for some difficult separations)
• set ΔP on column, reboiler, condenser and separator
• set ΔT on condenser
• Create a component recovery for HK in bottom with large ±
• Set Reflux ratio = 0.1 (increase to get simulation to run w/o errors).
• May need pump around loop estimate.
• Determine αLK,HK, viscosity
• (use Plots Tab to determine extra trays) determine Nmin and feed tray
• Use Fig. 19.1 to determine Rmin from R, N from Nmin
• Redo calc with tray efficiency defined see Figure 19.3 correlation.
• Recommendations for final design
– Use N/Nmin=2 (above and below feed tray)
– R/Rmin=1.2
Figure 19.1
Tray Efficiency

μL * αLK,HK