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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

Hydrogen Methane Benzene Toluene Biphenyl Total

kmole/hr 1292 1167 280 117 3 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 Agent (ESA) – Phase condition of feed – Separation Factor – Cost I 1

C SF 

C

I 2

C

II 2

II 1

C

• Mass Separation Agent (MSA) – Phase condition of feed – Choice of MSA Additive – Separation Factor – Regeneration of MSA – Cost

Phases I and II, 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

– Packed, DT =[(4G)/((f Uflood πρG)]1/2

eq. 19.14

• Uflood= f(dimensionless density difference), f = 0.75-0.85 eq. 19.12 • Uflood= f(flow ratio), f = 0.75-0.85

eq. 19.15

• Column Height

– Nmin=log[(dLK/bLK)(bHK/dHK)]/log[αLK,HK] – N=Nmin/ε (or 2 Nmin/ ε)

Fenske eq.19.1

• 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

• Tray Efficiency, ε = f(viscosityliquid * αLK,HK) • Pressure Drop • Tray, ΔP=ρLg hL-wier N • Packed, ΔP=Packed bed (weeping)

eq. 19.9

Fig 19.3

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