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4 - Separation Trains1 SEQUENCING OF SEPARATION TRAINS Ref: Seider, Seader and Lewin (2004), Chapter 7

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4 - Separation Trains2 Introduction Almost all chemical processes require the separation of chemical species (components), to: purify a reactor feed recover unreacted species for recycle to a reactor separate and purify the products from a reactor Frequently, the major investment and operating costs of a process will be those costs associated with the separation equipment For a binary mixture, it may be possible to select a separation method that can accomplish the separation task in just one piece of equipment. However, more commonly, the feed mixture involves more than two components, involving more complex separation systems

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4 - Separation Trains3 Instructional Objectives Be familiar with the more widely used industrial separation methods and their basis for separation. Understand the concept of the separation factor and be able to select appropriate separation methods for vapor and liquid mixtures. Understand how distillation columns are sequenced and how to apply heuristics to narrow the search for a near- optimal sequence. Be able to apply algorithmic methods to determine an optimal sequence of distillation-type separations. When you have finished studying this unit, you should:

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4 - Separation Trains4 Example 1. Specification for Butenes Recovery

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4 - Separation Trains5 Design for Butenes Recovery System 100-tray column C3 & 1-Butene in distillate Propane and 1-Butene recovery Pentane withdrawn as bottoms n-C4 and 2-C4=s cannot be separated by ordinary distillation ( =1.03), so 96% furfural is added as an extractive agent ( 1.17). n-C4 withdrawn as distillate. 2-C4=s withdrawn as distillate. Furfural is recovered as bottoms and recycled to C-4

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4 - Separation Trains6 Separation is Energy Intensive Unlike the spontaneous mixing of chemical species, the separation of a mixture of chemicals requires an expenditure of some form of energy Separation of a feed mixture into streams of differing chemical composition is achieved by forcing the different species into different spatial locations, by one or a combination of four common industrial techniques: ESA – energy separating agent the creation by heat transfer, shaft work, or pressure reduction of a second phase that is immiscible with the feed phase (ESA – energy separating agent) MSA – mass separating agent the introduction into the system of a second fluid phase (MSA – mass separating agent). This must be subsequently removed. solid phase MSA the addition of a solid phase upon which adsorption can occur (MSA) barrier (ESA) the placement of a membrane barrier (ESA)

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4 - Separation Trains7 Common Industrial Separation Methods Separation Method Phase of the feed Separating agent(s) Developed or added phase Separation principle FlashL and/or V Pressure reduction or heat transfer V or Ldifference in volatility Distillation (ordinary) L and/or V Heat transfer or shaft work V or Ldifference in volatility Gas absorption V Liquid absorbent Ldifference in volatility StrippingL Vapor stripping agent Vdifference in volatility Extractive distillation L and/or V Liquid solvent and heat transfer V and Ldifference in volatility Azeotropic distillation L and/or V Liquid entrainer and heat transfer V and Ldifference in volatility

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4 - Separation Trains8 Common Industrial Sep.Methods (Cont’d) Separation Method Phase of the feed Separation agent Developed or added phase Separation principle Liquid-liquid extraction LLiquid solvent Second liquid Difference in solubility Crystalli- zation LHeat transfer Solid Difference in solubility or m.p. Gas adsorption VSolid adsorbent Solid difference in adsorbabililty Liquid adsorption LSolid adsorbent Solid difference in adsorbabililty MembraneL or VMembrane difference in permeability and/or solubility

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4 - Separation Trains9 Common Industrial Sep.Methods (Cont’d) Separation Method Phase of the feed Separation agent Developed or added phase Separation principle Supercritical extraction L or V Supercritical solvent Supercritical fluid Difference in solubility LeachingSLiquid solvent LDifference in solubility DryingS and LHeat transfer VDifference in volatility DesublimationVHeat transfer SDifference in volatility

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4 - Separation Trains10 Selecting Separation Method (1) The development of a separation process requires the selection of: Separation methods ESAs and/or MSAs Separation equipment Optimal arrangement or sequencing of the equipment Optimal operating temperature and pressure for the equipment separation method Selection of separation method depends on feed condition : Vapor: partial condensation, cryogenic distillation, absorption, adsorption, gas permeation (membranes), desublimation Liquid: partial vaporization, distillation, stripping, extractive distillation, azeo-distillation, LL extraction, crystallization, adsorption, membrane separation (dialysis, reverse osmosis, ultrafiltration and pervaporation), supercritical extraction Solid: if slurry filtration, if wet drying, if dry leaching

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4 - Separation Trains11 Selecting Separation Method (2) separation factor single stage of contacting The separation factor, SF, defines the degree of separation achievable between two key components of he feed. This factor, for the separation of component 1 from component 2 between phases I and II, for a single stage of contacting, is defined as: (7.1) C = composition variable, I, II = phases rich in components 1 and 2. SF is generally limited by thermodynamic equilibrium. For example, in the case of distillation, using mole fractions as the composition variable and letting phase I be the vapor and phase II be the liquid, the limiting value of SF is given in terms of vapor-liquid equilibrium ratios (K-values) as: (7.2,3)

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4 - Separation Trains12 Selecting Separation Method (3) For vapor-liquid separation operations that use an MSA that causes the formation of a non-ideal liquid solution (e.g. extractive distillation): (7.5) In general, MSAs for extractive distillation and liquid-liquid extraction are selected according to their ease of recovery for recycle and to achieve relatively large values of SF. If the MSA is used to create two liquid phases, such as in liquid-liquid extraction, the SF is referred to as the relative selectivity, , where: (7.6)

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4 - Separation Trains13 Relative volatilities for equal cost separators Ref: Souders (1964)

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4 - Separation Trains14 Sequencing of Ordinary Distillation Columns in each column is > 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. Use a sequence of ordinary distillation (OD) columns to separate a multicomponent mixture provided:

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4 - Separation Trains15 Algorithm to Select Pressure and Condenser Type

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4 - Separation Trains16 Number of Sequences for Ordinary Distillation Equation for number of different sequences of P 1 ordinary distillation (OD) columns, N S, to produce P products: (7.9) P# of Separators Ns Ns

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4 - Separation Trains17 Example 2 – Sequences for 4-component separation

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4 - Separation Trains18 Example 2 – Sequences for 4-component separation

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4 - Separation Trains19 Identifying the Best Sequences using Heuristics 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 following guidelines are often used to reduce the number of OD sequences that need to be studied in detail:

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4 - Separation Trains20 Class Exercise Design a sequence of ordinary distillation columns to meet the given specifications.

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4 - Separation Trains21 Class Exercise – Possible Solution Guided by Heuristic 4, the first column in position to separate the key components with the greatest SF.

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4 - Separation Trains22 Complex Columns for Ternary Mixtures Ref: Tedder and Rudd (1978) In some cases, complex rather than simple distillation columns should be considered when developing a separation sequence.

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4 - Separation Trains23 Regions of Optimality ESI 1.6 ESI 1.6 As shown below, optimal regions for the various configurations depend on the feed composition and the ease-of-separation index: ESI = AB / BC

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4 - Separation Trains24 Sequencing of V-L Separation Systems 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. 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, then T = 4, and applying Eqns (7.9) and (7.10) gives 32 possible sequences (for ordinary distillation alone, N S = 2). (7.10) 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:

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4 - Separation Trains25 Example 3 (Example 1 Revisited) Speciesb.pt.( C)Tc ( C)Pc, (MPa) PropaneA ButeneB n-ButaneC trans-2-ButeneD cis-2-ButeneE n-PentaneF 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.

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4 - Separation Trains26 Example 3 (Example 1 Revisited) Adjacent Binary Pair ij at 65.5 o C Propane/1-Butene (A/B) 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 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 method 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 = 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

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4 - Separation Trains27 Estimating Annualized Cost, C A For each separation, C A is estimated assuming 99 mol % recovery of light key and heavy key in distillate and bottom, respectively. The following steps are followed: 2.Estimate number of stages, feed stage and initial guess of reflux ratio (R = 1.2 R min ) by using a short-cut distillation method (e.g., DSTWU in Aspen plus). 3.Select tray spacing (typically 2 ft.) and calculate column height, H (assume an overall efficiency equal to 75%). 4.Estimate reboiler duty, condenser duty and column diameter by a rigorous distillation method (e.g., RadFrac in Aspen plus) 5.Estimate installed cost of tower (see Chapter 16). 6.Size and cost ancillary equipment (condenser, reboiler, reflux drum). Sum total capital investment, C TCI. 7.Compute annual cost of heating and cooling utilities (C COS ). 8.Compute C A assuming ROI (typically r = 0.33). C A = C COS + r C TCI 1.Set distillate and bottoms column pressures using

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4 - Separation Trains28 SequenceCost, $/yr , , ,127, , ,095,600 1 st Branch of Sequences 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

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4 - Separation Trains29 SequenceCost, $/yr 2-(8,9-21)888,200 2-(8,10-22)860,400 2 nd Branch of Sequences 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

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4 - Separation Trains30 SequenceCost, $/yr , ,095, (25,26)867, ,080,100 3 rd Branch of Sequences 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

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4 - Separation Trains31 SequenceCost, $/yr ,115,200 4 th Branch of Sequences 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

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4 - Separation Trains32 Lowest Cost Sequence SequenceCost, $/yr 2-(8,10-22)860,400

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4 - Separation Trains33 Marginal Vapor Rate Method The difference in costs between the separation in the absence of nonkey components and the separation in the presence of nonkey components, defined as Marginal Annualized Cost (MAC). A good approximation of MAC is the MV, which is the corresponding difference in molar vapor rate passing up the column. The sequence with the minimum sum of column MVs is selected. Vapor rate is a good measure of cost because it is a major factor in determining column diameter, reboiler and condenser areas, and reboiler and condenser duties. When the number of products is more than four, using the annualized cost method is very difficult and time- consuming. One of the less rigorous method for OD that can produce good results is Marginal Vapor Rate (MV) that proposed by Modi and Westerberg (1992).

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4 - Separation Trains34 Estimating Marginal Vapor Rate, MV For each separation, MV is estimated assuming feed at bubble point and 99.9 mol % recovery of light key and heavy key in distillate and bottom, respectively. The following steps are followed: 1.Set distillate and bottoms column pressures using 2.Estimate distillate rate (D), by using a short-cut distillation method (e.g., DSTWU in Aspen plus with R=1.2 R min ). 3.Calculate the up column vapor rate as V=D(R+1). 4.Calculate the MV (The difference in vapor rate between the separation in the absence of nonkey components and the separation in the presence of nonkey components)

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4 - Separation Trains35 Example 4 Use the marginal vapor rate (MV) method to determine a sequence for the hydrocarbon specified in the figure, except: 1.Ignore the given temperature and pressure of the feed 2.Assume a recovery of 99.9% in each column

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4 - Separation Trains36 Example 4 A=isobutane, B= n-butane, C=isopentane, D= n-pentane

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4 - Separation Trains37 Separation Trains - Summary Be familiar with the more widely used industrial separation methods and their basis for separation. Understand the concept of the separation factor and be able to select appropriate separation methods for liquid mixtures. Understand how distillation columns are sequenced and how to apply heuristics to narrow the search for a near- optimal sequence. Be able to apply algorithmic methods to determine an optimal sequence of distillation-type separations. On completing this unit, you should: Next week: Azeotropic Distillation Next week: Azeotropic Distillation

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