1) Decide on the materials of construction and chose the appropriate standard (ASTM, API, BSI etc.) for pressure vessels. Choose the design pressure and the design temperature, which will be related to the operating pressure, condensing temperature and reboiler temperature.
2) The overall mass balance can be calculated from the required product compositions and the feed flow rate. The operating pressure can be specified from available cooling media temperatures, a suitable approach temperature and the phase of the overhead product. The temperature of the reboiler can be calculated from the composition of the bottom product and an assumed pressure drop across the column, which must be confirmed at a later stage.
3) A key step in the design of any distillation column is the selection of the reflux or boil-up ratio. In general these ratios are a function of the type of system (ideal hydrocarbon, non-ideal, associated, oxygenated organics etc.). For hydrocarbons, the reflux ratio will be approximately 20-50% above the minimum: this may also be a function of the operating temperature and can be as low as 10% above minimum for low temperature refrigerated columns. The stability of the feed quality and the requirements of the control system may modify the above criteria. For non-ideal systems, no such simple rule is generally applicable and each case must be considered on its own merits. The ratio finally chosen may be close to the minimum but the possibility of some trace component building up to substantial concentrations can invalidate any simple view. All of the above views can also be applied to the boil-up ratio but the use of reflux ratio is preferred. The final objective is to select a reflux/boil-up ratio that is economically justified.
4) The methods available for the determination of the minimum reflux ratio only really apply to thermodynamically ideal systems with constant molar overflow i.e. Fenske- Underwood-Gilliland-Kirkbride etc. Such methods must be applied with care and the designer should be ready to modify the value after taking account of large variations in component activity and/or molar latent heat.
5) Collect together all the physical and thermodynamic properties needed for your chosen design procedure as outlined below. ChemCad can be used as a data source; but it must be recognised that ChemCad may not always be wholly accurate especially for non- hydrocarbon systems.
6) The energy balances for the distillation column can now be established with the condenser and reboiler heat loads being calculated. The application of a ChemCad mass and energy balance is only reliable/justified when all deviations from ideality have been accurately modelled. Such deviations include liquid phase activity coefficients that vary
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appreciably over the composition range. This is certainly true for any columns containing physically associating components, such as HCN-H 2 O, EDC-H 2 O, HCl-EDC, H 2 O-H 2 S and CH 3 OH-H 2 O, TEG-H 2 O, MED/DEA/MDEA-H 2 O etc. Some non-ideal systems may be modelled using an appropriate liquid phase model, such as NRTL or a modified Cubic Equation of State model such as PSRK. Particular care is necessary with components which appear essentially at one end of the column and are only trace components at the other i.e. where the reboiler contains only a trace of a component that appears essentially in the distillate.
7) You will be required to do carry out a detailed plate-to-plate calculation for your column, using suitable methods. In some circumstances this can be done by hand but more commonly ChemCad can be used but this must be checked by appropriate hand calculations. In either case you are required to propose an economically optimised design based on the minimisation of a suitable combination of Capital and Operating costs.
8) Decide on and write down an overall design procedure including all the appropriate mass and energy balance equations and necessary equilibrium relationships to be used at the various stages of the calculation. Your procedure may include the use of an equation solver and/or suitable spreadsheet. At an appropriate time, discuss your equations and procedure with the course supervisor. Students are not encouraged to waste time on non-productive effort.
9) Evaluate the optimum number of theoretical stages required for the separation making suitable allowances for the pressure drop across each theoretical stage. A second pass through the calculation procedure may be necessary to match the pressures on each tray but this is more significant in low-pressure columns. It is however important to evaluate the correct reboiler pressure and hence boiling temperature when the reboiler is designed.
10) It is now necessary to determine the type of column internals necessary to bring about the required separation. It is not recommended to use trays in a column with a diameter less than about 1000 mm because it is difficult to get a worker into the column for cleaning, inspecting and changing trays. Hence columns with diameters less than this tend to be packed. It is therefore necessary to determine the approximate tower diameter before the type of internals is chosen. It should be noted that a change in diameter might occur across the feed tray and where side streams occur.
11) When using trays a choice must be made between the various types available i.e. sieve plates, bubble plates, valve trays etc. Design methods for the first two types are given explicitly in the literature and an approximation design for valve trays may be inferred. For a real design a tray vendor would have to confirm the tray design as a part of the procurement procedure. It is desirable to check the hydraulic design at the trays above and below the feed tray, the tray immediately above the reboiler and the reflux tray with other checks being done anywhere else that significant changes in internal flows occur. It should be noted that trays are often used because the design methods are better established than those for packed towers.
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12) The determination of tray efficiency is not well quantified but some guidance is available in the literature. The efficiency is largely a function of the liquid viscosity and relative volatility and does therefore vary between components. The actual number of trays can be calculated and the true pressure drop evaluated. This can be compared with the value assumed in the design procedure.
13) The selection of the type and size of packing to be used in small diameter columns is dependent on a number of factors. The D tower /D packiing ratio is always more than 10 but rarely greater than 40 and to minimise the packed height the smallest packing size within this range is usually selected. More detailed guidance is available in the literature such as given at the end of this note. The type of packing depends upon the characteristics required i.e. capacity and the Height Equivalent to a Theoretical Plate (HETP). The use of a suitable correlation will give the tower diameter as a function of the percentage of the predicted flooding point. The actual percentage of the flooding point used will normally be in the range 50% to 80% (60% recommended) and this will depend upon the nature of the system (note that 60% of flooding is typically 80% of the loading point according to G A Morris).
14) There are no reliable methods to predict the HETP. In practice measured data is used and guidance on typical values is available in the literature.
15) Liquid distribution in a packed bed is an important consideration. In general it requires an adequate number of distribution points which are placed some suitable height above the packed bed. Students should ensure that such requirements are met. Periodic redistribution of the liquid is necessary. It is usual to install additional sections of packing below each distributor or redistributor to act as a secondary distribution zone. It is vital with secondary distributors to mix the collected liquid before redistribution.
16) The following design aids are available 16.1 ChemCad a) Can be used to generate heat loads between selected process temperatures within the cooling/heating range of the column, b) Can be used to calculate K values for components if the selected K value option is appropriate, c) Can be used to predict the physical properties of the mixtures being encountered on the trays, d) Can be used identify the appropriate combination of the number of ideal stages, condenser and reboiler heat loads, feed plate position, tower pressure, tower diameter etc which minimise a suitable combination of Capital and Operating costs.
16.2 TK Solver a) Can be used to solve groups of simultaneous equations for calculations of local mass and energy balances and equilibrium relationships
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16.3 Excel a) Should be considered for general repetitive calculations.
17) References a) King - Separation Processes b) Van Winkle - Distillation c) Ludwig - Applied Process Design for Chemical and Petrochemical Plants d) Coulson and Richardson - Chemical Engineering e) Treybal - Mass Transfer Operations f) Perry - Chemical Engineers handbook g) Rose - Distillation Design in Practice h) Strigle, R.F., Random Packings and Packed Towers, Gulf Publishing Company 1987 i) Kent and Eisenberg - Better data for Amine Treating, Hydrocarbon Processing, Feb. 1976, page 87. j) Hirata M, Ohe S and Nagahama K, Computer Aided Data Book of Vapour-Liquid Equilibrium, Elsevier Scientific, 1975
18) It is strongly suggested that students check equations quoted in textbooks against the original references. A number of critical errors have been found in some of the more commonly used textbooks.
19) Specific design data is available from CAM/RBT on a) Activity coefficient HCl-EDC systems b) VLE data for EDC-H 2 O system c) HCN-NH 3 -H2O data
Students should note that the above references are given in shortened form. Full and specific references should be given in any report.