2019 Spring ChE338 - Homework #6 (Assigned 03/28)

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Problem 1.
One thousand kg/h of a 45 wt% acetone-in-water solution is to be extracted at 25°C in a continuous,
countercurrent system with pure 1,1,2-trichloroethane to obtain a Raffinate containing 10 wt%
acetone. Using the given equilibrium data.

The minimum flow rate of solvent is 233 kg/h. Determine the below with an equilateral-triangle
diagram:

1.1. The number of stages required for a solvent rate equal to 1.5 times minimum;

1 pt: Draw a ternary phase diagram with given tie-line info

1 pt: Draw the first (F-E1=P) and the last (RN-S=P) operating lines and find P (operating point)
1 pt: Find a tie-line that end E1 by interpolation and resultant R1
1 pt: Repeated staging until R merged to RN
1 pt: Determine how many stages
About 5 stages

1.2. The flow rate and composition of each stream leaving each stage

1 pt: Determine solute (A), carrier (C), and solvent (S) compositions in each equilibrium stage
Extract Raffinate
Solute Carrier Solvent Solute Carrier Solvent
Stage (A) (C) (S) (A) (C) (S)
1 0.5 0.04 0.46 0.4 0.57 0.03
2 0.43 0.03 0.54 0.34 0.64 0.02
3 0.35 0.02 0.63 0.29 0.7 0.01
4 0.28 0.02 0.72 0.2 0.79 0.01
5 0.18 0.01 0.81 0.1 0.89 0.01

1 pt: Determine solvent flow: S = Smin x 1.1 S=349.5 kg

1 pt: Determine the mixing point
1 pt: Determine E1 and R5 the same way in problem 1.2.
Total mass balance F + S = M = E1 + R5 1349.5 = E1 + R5
Solute mass balance F(XA)F + S(XA)S = M(XA)M = E1(XA)E + R5(XA)R
1000(0.45) + 350(0) = E1(0.5) + R5(0.1)
E1 = 787.62 kg, R5 = 561.88 kg

1 pt: Mass balance each stage

** Depending on this reading, the results can be significantly different. Possibly get unreasonable
values. If the approach is correct, full grade will be given.

Check attached solutions

Problem 2.
Isopropyl ether (E) is used to separate acetic acid (A) from water (W). The liquid–liquid equilibrium data at
25°C and 1 atm are below:

One hundred kilograms of a 30 wt% A–W solution is contacted with 120 kg of ether (E).

2.1. What are the compositions of the resulting Extract and Raffinate?

1 pt: Determine mixing point composition

1 pt: Ternary phase diagram with given tie-line info and find the mixing point.
1 pt: Find a tie-line that passes the mixing point (interpolation)
1 pt: Read Extraction and Raffinate points

2.2. What are the weights of the resulting Extract and Raffinate?

1 pt: Total mass balance F+S=M=E+R

220 = E + R
Solute mass balance F(XA)F + S(XA)S = M(XA)M = E(XA)E + R(XA)R
 100(0.3) + 120(0) = E(0.09) + R(0.21)
1 pt: Solve linear algebra
E = 133.2 kg, R = 86.6 kg

2.3. What would the concentration of acid in the (ether-rich) extract be if all ether were removed?

1 pt: Extraction phase when all solvent is removed.

9 / (9+3) x 100 = 75 wt%
Problem 3.
Why is liquid–liquid extraction preferred over distillation for the separation of a mixture of formic acid
and water?

At 1 atm, the boiling point of formic acid is 100.6°C, almost identical to the normal boiling point of
water. A maximum-boiling azeotrope is formed at 107.1 C with 43.4 mol% water. Thus, it is
impossible to separate formic acid from water at 1 atm by ordinary distillation. Liquid-liquid-extraction
overcomes azeotrope and requires less energy to separate formic acid from water better than
distillation.

1 pt: Identify close boiling points or azeotrope

1 pt: Discuss overcome azeotrope and less energy requirement

Problem 4.
Discuss similarities and differences between distillation and liquid-liquid-extraction processes.

1 pt: Discussion about thermodynamic phase equilibrium

1 pt: Discussion about mass transport
1 pt: Unique application: eg. Energy intensive, hydrocarbon separation (Distillation), Require
additional separation, biological material separation (Extraction)
1 pt: Operating parameters and limiting conditions (eg. Reflux and solvent flow)

Refer Table (attached)

 100(0.3) + 120(0) = E(0.09) + R(0.21)
1 pt: Solve linear algebra
E = 133.2 kg, R = 86.6 kg

2.3. What would the concentration of acid in the (ether-rich) extract be if all ether were removed?

1 pt: Extraction phase when all solvent is removed.

9 / (9+3) x 100 = 75 wt%
Problem 3.
Why is liquid–liquid extraction preferred over distillation for the separation of a mixture of formic acid
and water?

At 1 atm, the boiling point of formic acid is 100.6°C, almost identical to the normal boiling point of
water. A maximum-boiling azeotrope is formed at 107.1 C with 43.4 mol% water. Thus, it is
impossible to separate formic acid from water at 1 atm by ordinary distillation. Liquid-liquid-extraction
overcomes azeotrope and requires less energy to separate formic acid from water better than
distillation.

1 pt: Identify close boiling points or azeotrope

1 pt: Discuss overcome azeotrope and less energy requirement

Problem 4.
Discuss similarities and differences between distillation and liquid-liquid-extraction processes.

1 pt: Discussion about thermodynamic phase equilibrium

1 pt: Discussion about mass transport
1 pt: Unique application: eg. Energy intensive, hydrocarbon separation (Distillation), Require
additional separation, biological material separation (Extraction)
1 pt: Operating parameters and limiting conditions (eg. Reflux and solvent flow)

Refer Table (attached)

ChE338  Separation:  Distillation  vs.  Extraction    
 
  Distillation   Extraction  
General   Phase  creation     Phase  addition    
strategies   (require  ESA:  Energy  Separating  Agent)   (require  MSA:  Material  Separating  Agent)  

   
Representative  Table  7.1   Table  8.1  
examples   Thermodynamically  reversible  components   Temperature  irreversible  components  
e.g.  hydrocarbons,  crude  oils   e.g.  biological  molecules    
Thermodynamic   Vapor-­Liquid-­Equilibrium     Ternary  Phase  Diagram:  Solute-­Solvent-­Carrier    
phase   (Ideal  &  less  ideal:  Equation  Of  State  (EOS))   (Experimental  measurement)  
equilibrium   (Non-­idea:  Experimental  measurement,   (Additional  tie  lines  can  be  interpolated)  
Graphs)   Single  phase  vs  Binary  phase  regions  
   
  Tie-­line  indicates  an  equilibrium  
Each  point  in  V-­L-­E  indicates  an  equilibrium    
point  
 

 
 
   
 
Impractical   Azeotrope   Plait  point    
condition  to  
separate  

 
  alpha  phase:  Extract,  beta  phase:  Raffinate  
 
Quantitative   Relative  volatility   Relative  selectivity  
info  about  how  
a  target  
component  
distributed  
between  two  
phases  

 
 
Single  stage   Flash  drum    
process  

 
 
Operating  line:    Mass  balance  (Feed,  Vapor,    
Liquid),  Feed  composition  (zF)  &  condition  (q-­ Operating  line:  Mixing  point,  Tie-­line  passing  a  
line  slope)   mixing  point  
   
Comparison  process:  Separating  power   Comparison  process:  Extraction  factor  
Graphical      
integration    
equilibrium  and    
operation      
(Single  stage)    
 
 
 
 
 
 
 
 
Operation   Degree  of  freedom   Degree  of  freedom  
(change   :  Determine  how  many  parameters  and  how   :  Determine  how  many  parameters  and  how  much  
thermodynamic   much  adjusted  to  move  a  thermodynamic   adjusted  to  move  a  thermodynamic  state  to  a  
state)   state  to  a  desired  state   desired  state  
 
Cascade   General  process     General  process  
(Multi-­staging)    
   
 

 
 
For  both  distillation  and  extraction  
Overcome  single  stage  separation  that  is  mainly  
restricted  by  thermodynamic  equilibrium.  
(*Chemistry  and  analytical  separation)  
 
Achieve  higher  purity  products  
Continuous  process    
Scale-­up  process  
(*Unique  aspect  of  chemical  engineering  
 
  separation)  
Critical   Energy  balance:  Phase  creation  requires   Solvent:  Solvent  is  critical  consideration  to  
consideration  in   significant  amount  of  energy.  Energy   determine  thermodynamic  equilibrium,  economic  
separation   efficiency  is  critical  consideration.   aspect  (cheap),  safety  aspect  (stable),  and  down-­
process  design   stream  separation  (required  for  extraction)    
Mass  transport   Specific  density:  Vapor  (light-­move  up),   Specific  density:  different  density  between  carrier  
Liquid  (heavy-­move  down)   and  solvent  
Bubble  cap  to  facilitate  mass  transport   Agitation  /  Mixing:  Increase  interface  between  two  
  liquid  phases  
Mass  transport   Assume  enough  time  is  given  to  reach   Assume  enough  time  is  given  to  reach  equilibrium  at  
&  Equilibrium   equilibrium  at  each  stage.   each  stage  
 
Murphree  efficiency  (if  mass  transport  occurs  
before  reaching  an  equilibrium)  

 
Graphical   McCabe-­Thiele  graphical  equilibrium-­stage   Hunter-­Nash  graphical  equilibrium-­stage  
integration  
equilibrium  and  
operation    
(Multi-­stage)  
 
 

 
 

 
 
Partial  condenser  and  reboiler  requires  one  
additional  equilibrium  stage.  
 
Key  operating   Reflux  Ratio   Solvent  Flow  
parameter    
Limiting   Total  Reflux,  Minimum  Reflux,  Perfect   Feed  composition,  Minimum  and  Maximum  Solvent  
conditions   Separation   Flow  
(Graphical  meaning  !!!)   (Graphical  meaning  !!!)