Level 4: General structure of separation system

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1 Level 4: General structure of separation system Cheng-Ching Yu Dept of Chem. Eng. National Taiwan University

2 Separation Systems Typical reaction/separation structure Remark: Focus on reactor exit. 2

3 Remark: 1. Liquid separation system: column, extraction, azeotropic distillation etc. 2. Two phase: use reactor as a phase splitter or cool down to 35 C. 3

4 Heuristic: phase split is cheap. Steps: 1. Cool down to 35C 2. A. phase split exists == Step 3 B. no phase split (i) pressurize (ii) refrigerated partial condenser (iii) to vapor recovery system 3. Design vapor recovery system and liquid separation systems. 4

5 Gas recovery systems location: Location 1: If significant amount of valuable materials are being lost in the purge. Location 2: If materials are deleterious to the reactor operation. Location 3: Both factors are valid. None: Both factors do not exist. 5

6 Type: condensation absorption adsorption membrane reaction system (removing CO 2, H 2 S) Strategy: If vapor flow after the phase split is small, we can consider combining vapor/liquid recovery together. 6

7 Liquid separation system Light ends Method -drop the pressure for removal -partial condenser -pasteurization column -stabilizer column Destination -vent -flare -vapor recovery system 7

8 Azeotropes -recycle the azeotropes -split the azeotrope (need two columns for a binary azeotrope). Applicability of distillation Why -handle wide range of throughput -handle wide range of feed composition -ability to produce high purity product Cases not suited -relative volatility < 1.1 (column can become very expensive) -low molecular weight -high molecular weight heat sensitive materials 8

9 Basic principle of distillation Principle -use boiling point difference for separation -described by vapor liquid equilibrium (VLE) x LK =x HK y LK >y HK VLE- Txy Diagram - x1 and y1 in equilibrium 9

10 Effect of Pressure -keep the pressure low P2 > P1 10

11 Column Configuration remove heat at lower T input heat at higher T 11

12 Column Notation- EMO 12

13 Realistic View 13

14 Minimum Reflux Ratio Understand the effects of changing reflux rate or boilup rate. 14

15 Total Reflux Find minimum number of trays (N min ) 15

16 Capital cost vs operating cost (energy) RR= 1.1~1.2 RRmin 16

17 Typical Procedure to Set Column Pressure Remark: Prefer using cooling water as cooling media. 17

18 Column sequencing Definitions -single feed -two products -key components are adjacent in boiling pt. -column has a condenser and a reboiler 18

19 Direct vs Indirect (LOF vs HOF) 19

20 Two Alternatives for NC= 3 / 20

21 Six Alternatives for NC= 4 21

22 14 Alternatives for NC= 5 22

23 Summary -# of alternatives increases drastically - how do we screen for the best few sequences - what criteria should we use to choose between alternative sequences

24 Heuristics Ex. A 33% B 33% C 33% (8/2/1) Ex. A 15% B 15% C 70% (4/2/1) 24

25 25

26 Quantitative Measure Calculate vapor rates from short-cut method: 1. Underwood Eq. (RRmin) 2. RR=~1.1 RRmin 3. V=(1+RR)D 4. Repeat 1-3 for all columns 26

27 Ternary System- boundary when Q direct =Q indirect HK I D IK LK 27

28 Complete picture for HDA light ends (H2/CH4) 3.8% product (Benzene) 69.3% reactant (Toluene) 25.7% heavy ends (Diphenyl) 1.2% 28

29 Complex column LOF HOF SSR SSS PF SS 29

30 30

31 31

32 Azeotropic Systems Minimum-boiling repulsion 32

33 Azeotropic Systems-cont Maximum-boiling attraction 33

34 Activity Coefficient- Wilson, NRTL, UNIQUAC, UNIFAC repulsion vs attraction 34

35 Two-liquid phase Repulsion force is extremely large 35

36 Two-liquid phase (a) is a typical system 36

37 Two-liquid phase- effect of temperature Effects of temperature (for which case?) 37

38 Breaking Azeotrope We have to change something to overcome azeotrope 1. Change P- pressure swing 2. Change gamma- add entrainer 3. Change y- remove vapor across membrane (pervaporization) 38

39 Pressure Swing 39

40 Entrainer Addition Remark: 1. Must change gamma or the ratio of them. 2. Can possibly induce phase splitting. 3. Too many choices! 40

41 Design Procedure 41

42 Design Procedure- In practice -leave azeotropes until last -try pressure swing -try extractive distillation using entrainer while not causing phase-split (homogeneous azeotropic distillation) -try adding a (light) entrainer and induce phase-split (heterogeneous azeotropic distillation) 42

43 References Books 1. Doherty, M. F.; Malone, M. F. Conceptual Design of Distillation Systems, McGraw-Hill, an up-to-date book on distillation 2. Douglas, J. M. Conceptual Process Design, McGraw-Hill, a highly readable and useful book in process design 3. Luyben, W. L.; Wenzel, L. A. Chemical Process Analysis, Prentice-Hall, an introductory book on material & energy balances 4. Smith, R. Chemical Process Design, McGraw-Hill, philosophy is similar to the Douglas book with somewhat updated materials 5. Smith, R. Lecture Note on Advanced Distillation System Design, Taipei,

44 References Papers 1. Fien, G-J A.; Liu, Y. A. I&EC Res 1994, 33, a highly readable review paper on azeotropic distillation 2. Guttinger, T. E.; Morari, M. I&EC Res 1996, 35, look at stability of homogeneous azeotrpic distillation- typical Morari paper 3. Laroche. L.; Bekiaris, N.; Anderson, H. W.; Morari, M. I&EC Res 1992, 31, explore design aspect of homogeneous azeotropic distillation 4. Hauan, S.; Westerberg, A. W.; Lien, C. Chem. Eng. Sci. 2000,55,1053. first systematic paper investigate the effect of reaction on RCM 5. Venimadhavan, G.; Malone, M. F.; Doherty, M. F. AIChE J. 1999, 45, 546. also explore the effect of reaction on RCM 44

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