1. CHEN 4460 – Process Synthesis, Simulation and Optimization Dr. Mario Richard Eden Department of Chemical Engineering Auburn University Lecture No. 5 – Sequencing Ordinary Distillation Columns September 18, 2007 Contains Material Developed by Dr. Daniel R. Lewin, Technion, Israel Sequencing Distillation Columns

2. Lecture 5 – Objectives  Understand how distillation columns are sequenced and how to apply heuristics to narrow the search for a near- optimal sequence.  Be able to apply systematic methods to determine an optimal sequence of distillation-type separations.

3. Sequencing OD Columns Use a sequence of ordinary distillation (OD) columns to separate a multicomponent mixture provided:   in each column is > 1.05.  The reboiler duty is not excessive.  The tower pressure does not cause the mixture to approach the T C of the mixture.  Column pressure drop is tolerable, particularly if operation is under vacuum.  The overhead vapor can be at least partially condensed at the column pressure to provide reflux without excessive refrigeration requirements.  The bottoms temperature for the tower pressure is not so high that chemical decomposition occurs.  Azeotropes do not prevent the desired separation.

4. Pressure/Condenser Algorithm

5. Number of Sequences for OD Number of different sequences of P –1 ordinary distillation (OD) columns, N S, to produce P products: (7.9) P# of Separators Ns Ns 211 322 435 5414 6542 76132 87429

6. Example: 4 Components

8. Best Sequence using Heuristics The following guidelines are often used to reduce the number of OD sequences that need to be studied in detail:  Remove thermally unstable, corrosive, or chemically reactive components early in the sequence.  Remove final products one-by-one as distillates (the direct sequence).  Sequence separation points to remove, early in the sequence, those components of greatest molar percentage in the feed.  Sequence separation points in the order of decreasing relative volatility so that the most difficult splits are made in the absence of other components.  Sequence separation points to leave last those separations that give the highest purity products.  Sequence separation points that favor near equimolar amounts of distillate and bottoms in each column. The reboiler duty should not be excessive.

9. Class Exercise Design a sequence of ordinary distillation columns to meet the given specifications.

10. Exercise – Possible Solution Guided by Heuristic 4, the first column in position to separate the key components with the greatest SF.  Sequence separation points in the order of decreasing relative volatility so that the most difficult splits are made in the absence of other components.

11. Exercise – Possible Solution  = 3.6  = 2.8  = 1.5  = 1.35

12. Complex Columns In some cases, complex rather than simple distillation columns should be considered when developing a separation sequence. Ref: Tedder and Rudd (1978)

13. Regions of Optimality As shown below, optimal regions for the various configurations depend on the feed composition and the ease-of-separation index (ESI): ESI =  AB /  BC ESI  1.6 ESI  1.6

14. Sequencing V-L Separation When simple distillation is not practical for all separators in a multicomponent mixture separation system, other types of separators must be employed and the order of volatility or other separation index may be different for each type. If they are all two-product separators and if T equals the number of different types, then the number of possible sequences is now given by: For example, if P = 3, and ordinary distillation, extractive distillation with either solvent I or solvent II, and LL extraction with solvent III are to be considered, T = 4, and applying Eqns (7.9) and (A) gives 32 possible sequences (for ordinary distillation alone, N S = 2). (A)

15. Example: Butenes Recovery For T = 2 (OD and ED), and P = 4, N S = 40. However, since 1-Butene must also be separated (why?), P = 5, and N S = 224. Clearly, it would be helpful to reduce the number of sequences that need to be analyzed. Need to eliminate infeasible separations, and enforce OD for separations with acceptable volatilities. Propane Butane Butene Pentane 1-Butene and 2-Butene are structurally very different, whereas, the optical isomers are much closer related and are difficult to separate by distillation

16. Example: Butenes Recovery Splits A/B and E/F should be by OD only (   2.5) Split C/D is infeasible by OD (  = 1.03). Split B/C is feasible, but an alternative may be more attractive. Use of 96% furfural as a solvent for ED increases volatilities of paraffins to olefins, causing a reversal in volatility between 1-Butene and n-Butane, altering separation order to ACBDEF, and giving  C/B = 1.17. Also, split (C/D) II with  = 1.7, should be used instead of OD. Thus, splits to be considered, with all others forbidden, are: (A/B…) I, (…E/F) I, (…B/C…) I, (A/C…) I, (…C/B…) II, and (…C/D…) II Adjacent Binary Pair  ij at 65.5 o C Propane/1-Butene (A/B)2.45 1-Butene/n-Butane (B/C)1.18 n-Butane/trans-2-Butene (C/D)1.03 cis-2-Butene/n-Pentane (E/F)2.50

17. Estimating Annualized Cost For each separation, C A is estimated assuming 99 mol % recovery of light key in distillate and 99 mol % recovery of heavy key in bottoms. The following steps are followed:  Set distillate and bottoms column pressures using  Estimate number of stages and reflux ratio by WUG method (e.g., using Aspen Plus “DSTWU Column”)  Select tray spacing (typically 2 ft.) and calculate column height, H  Compute tower diameter, D (using Fair correlation for flooding velocity, or Aspen Plus Tray Sizing Utility)  Estimate installed cost of tower (e.g. Peters & Timmerhaus)  Size and cost ancillary equipment (condenser, reboiler, reflux drum). Sum total capital investment, C TCI  Compute annual cost of heating and cooling utilities (COS)  Compute C A assuming ROI (typically r = 0.2). C A = COS + r *C TCI

18. Butenes Recovery – 1 st Branch SequenceCost, $/yr 1-5-16-28900,200 1-5-17-29872,400 1-6-181,127,400 1-7-19-30878,000 1-7-201,095,600 Species PropaneA 1-ButeneB n-ButaneC trans-2-ButeneD cis-2-ButeneE n-PentaneF (A/B…) I, (…E/F) I, (…B/C…) I, (A/C…) I, (…C/B…) II, and (…C/D…) II

19. Butenes Recovery – 2 nd Branch Species PropaneA 1-ButeneB n-ButaneC trans-2-ButeneD cis-2-ButeneE n-PentaneF SequenceCost, $/yr 2-(8,9-21)888,200 2-(8,10-22)860,400 (A/B…) I, (…E/F) I, (…B/C…) I, (A/C…) I, (…C/B…) II, and (…C/D…) II

20. Butenes Recovery – 3 rd Branch Species PropaneA 1-ButeneB n-ButaneC trans-2-ButeneD cis-2-ButeneE n-PentaneF SequenceCost, $/yr 3-11-23-31878,200 3-11-241,095,700 3-12-(25,26)867,400 3-13-271,080,100 (A/B…) I, (…E/F) I, (…B/C…) I, (A/C…) I, (…C/B…) II, and (…C/D…) II

21. Butenes Recovery – 4 th Branch Species PropaneA 1-ButeneB n-ButaneC trans-2-ButeneD cis-2-ButeneE n-PentaneF SequenceCost, $/yr 4-14-151,115,200 (A/B…) I, (…E/F) I, (…B/C…) I, (A/C…) I, (…C/B…) II, and (…C/D…) II

22. Example: Butenes Recovery Lowest Cost Sequence SequenceCost, $/yr 2-(8,10-22)860,400

23. Example: Butenes Recovery

24. Summary – Sequencing  Understand how distillation columns are sequenced and how to apply heuristics to narrow the search for a near- optimal sequence.  Be able to apply systematic B&B methods to determine an optimal sequence of distillation-type separations. On completion of this part, you should:

25. Other Business Homework –SSL: 7.1, 7.2, 7.3 –Due Tuesday September 25 Next Lecture –Review of Non-Ideal Thermodynamics (SSL 258-271)