CHAPTER 11 Separation Columns (Distillation, …...design calculations. If a column is poorly insulated, changes in the internal reﬂux due to sudden changes in the external conditions,

CHAPTER 11

Separation Columns(Distillation, Absorption and Extraction)

11.1. INTRODUCTION

This chapter covers the design of separating columns. Though the emphasis is on distil-lation processes, the basic construction features, and many of the design methods, alsoapply to other multistage processes; such as stripping, absorption and extraction.

Distillation is probably the most widely used separation process in the chemical andallied industries; its applications ranging from the rectification of alcohol, which has beenpractised since antiquity, to the fractionation of crude oil.

Only a brief review of the fundamental principles that underlie the design procedureswill be given; a fuller discussion can be found in Volume 2, and in other text books; King(1980), Hengstebeck (1976), Kister (1992).

A good understanding of methods used for correlating vapour-liquid equilibrium datais essential to the understanding of distillation and other equilibrium-staged processes;this subject was covered in Chapter 8.

In recent years, most of the work done to develop reliable design methods for distillationequipment has been carried out by a commercial organisation, Fractionation ResearchInc., an organisation set up with the resources to carry out experimental work on full-size columns. Since their work is of a proprietary nature, it is not published in the openliterature and it has not been possible to refer to their methods in this book. Fraction-ation Research’s design manuals will, however, be available to design engineers whosecompanies are subscribing members of the organisation.

Distillation column design

The design of a distillation column can be divided into the following steps:

1. Specify the degree of separation required: set product specifications.2. Select the operating conditions: batch or continuous; operating pressure.3. Select the type of contacting device: plates or packing.4. Determine the stage and reflux requirements: the number of equilibrium stages.5. Size the column: diameter, number of real stages.6. Design the column internals: plates, distributors, packing supports.7. Mechanical design: vessel and internal fittings.

The principal step will be to determine the stage and reflux requirements. This isa relatively simple procedure when the feed is a binary mixture, but a complex

493

494 CHEMICAL ENGINEERING

and difficult task when the feed contains more than two components (multicomponentsystems).

11.2. CONTINUOUS DISTILLATION: PROCESS DESCRIPTION

The separation of liquid mixtures by distillation depends on differences in volatilitybetween the components. The greater the relative volatilities, the easier the separation.The basic equipment required for continuous distillation is shown in Figure 11.1. Vapourflows up the column and liquid counter-currently down the column. The vapour and liquidare brought into contact on plates, or packing. Part of the condensate from the condenseris returned to the top of the column to provide liquid flow above the feed point (reflux),and part of the liquid from the base of the column is vaporised in the reboiler and returnedto provide the vapour flow.

Feed

Reboiler

Bottomproduct

(a)

Reflux

Topproduct

Condenser

Multiplefeeds

Sidestreams

(b)

Figure 11.1. Distillation column (a) Basic column (b) Multiple feeds and side streams

In the section below the feed, the more volatile components are stripped from the liquidand this is known as the stripping section. Above the feed, the concentration of the morevolatile components is increased and this is called the enrichment, or more commonly, therectifying section. Figure 11.1a shows a column producing two product streams, referredto as tops and bottoms, from a single feed. Columns are occasionally used with morethan one feed, and with side streams withdrawn at points up the column, Figure 11.1b.This does not alter the basic operation, but complicates the analysis of the process, tosome extent.

SEPARATION COLUMNS (DISTILLATION, ABSORPTION AND EXTRACTION) 495

If the process requirement is to strip a volatile component from a relatively non-volatilesolvent, the rectifying section may be omitted, and the column would then be called astripping column.

In some operations, where the top product is required as a vapour, only sufficient liquidis condensed to provide the reflux flow to the column, and the condenser is referred toas a partial condenser. When the liquid is totally condensed, the liquid returned to thecolumn will have the same composition as the top product. In a partial condenser thereflux will be in equilibrium with the vapour leaving the condenser. Virtually pure topand bottom products can be obtained in a single column from a binary feed, but where thefeed contains more than two components, only a single “pure” product can be produced,either from the top or bottom of the column. Several columns will be needed to separatea multicomponent feed into its constituent parts.

11.2.1. Reflux considerations

The reflux ratio, R, is normally defined as:

R D flow returned as reflux

flow of top product taken off

The number of stages required for a given separation will be dependent on the reflux ratioused.

In an operating column the effective reflux ratio will be increased by vapour condensedwithin the column due to heat leakage through the walls. With a well-lagged column theheat loss will be small and no allowance is normally made for this increased flow indesign calculations. If a column is poorly insulated, changes in the internal reflux dueto sudden changes in the external conditions, such as a sudden rain storm, can have anoticeable effect on the column operation and control.

Total reflux

Total reflux is the condition when all the condensate is returned to the column as reflux:no product is taken off and there is no feed.

At total reflux the number of stages required for a given separation is the minimumat which it is theoretically possible to achieve the separation. Though not a practicaloperating condition, it is a useful guide to the likely number of stages that will beneeded.

Columns are often started up with no product take-off and operated at total reflux tillsteady conditions are attained. The testing of columns is also conveniently carried out attotal reflux.

Minimum reflux

As the reflux ratio is reduced a pinch point will occur at which the separation can only beachieved with an infinite number of stages. This sets the minimum possible reflux ratiofor the specified separation.


Methods for predicting the entrainment from sieve plates are given in Section 11.13.5,Figure 11.27; a similar method for bubble-cap plates is given by Bolles (1963).

11.11. APPROXIMATE COLUMN SIZINGAn approximate estimate of the overall column size can be made once the number ofreal stages required for the separation is known. This is often needed to make a roughestimate of the capital cost for project evaluation.

Plate spacing

The overall height of the column will depend on the plate spacing. Plate spacings from0.15 m (6 in.) to 1 m (36 in.) are normally used. The spacing chosen will depend onthe column diameter and operating conditions. Close spacing is used with small-diametercolumns, and where head room is restricted; as it will be when a column is installed in abuilding. For columns above 1 m diameter, plate spacings of 0.3 to 0.6 m will normallybe used, and 0.5 m (18 in.) can be taken as an initial estimate. This would be revised, asnecessary, when the detailed plate design is made.

A larger spacing will be needed between certain plates to accommodate feed and side-streams arrangements, and for manways.

Column diameter

The principal factor that determines the column diameter is the vapour flow-rate. Thevapour velocity must be below that which would cause excessive liquid entrainment or ahigh-pressure drop. The equation given below, which is based on the well-known Soudersand Brown equation, Lowenstein (1961), can be used to estimate the maximum allowablesuperficial vapour velocity, and hence the column area and diameter,

Ouv D ��0.171l2t C 0.27lt � 0.047�[��L � �v�

�v

]1/2

�11.79�

where Ouv D maximum allowable vapour velocity, based on the gross (total) columncross-sectional area, m/s,

lt D plate spacing, m, (range 0.5 1.5).

The column diameter, Dc, can then be calculated:

Dc D√

4 OVw�v Ouv

�11.80�

where OVw is the maximum vapour rate, kg/s.

This approximate estimate of the diameter would be revised when the detailed platedesign is undertaken.

11.12. PLATE CONTACTORSCross-flow plates are the most common type of plate contactor used in distillation andabsorption columns. In a cross-flow plate the liquid flows across the plate and the vapour


Figure 11.17. Typical cross-flow plate (sieve)

up through the plate. A typical layout is shown in Figure 11.17. The flowing liquid istransferred from plate to plate through vertical channels called “downcomers”. A pool ofliquid is retained on the plate by an outlet weir.

Other types of plate are used which have no downcomers (non-cross-flow plates), theliquid showering down the column through large openings in the plates (sometimes calledshower plates). These, and, other proprietary non-cross-flow plates, are used for specialpurposes, particularly when a low-pressure drop is required.

Three principal types of cross-flow tray are used, classified according to the methodused to contact the vapour and liquid.

1. Sieve plate (perforated plate) (Figure 11.18)

This is the simplest type of cross-flow plate. The vapour passes up through perforations inthe plate; and the liquid is retained on the plate by the vapour flow. There is no positivevapour liquid seal, and at low flow-rates liquid will “weep” through the holes, reducingthe plate efficiency. The perforations are usually small holes, but larger holes and slotsare used.

2. Bubble-cap plates (Figure 11.19)

In which the vapour passes up through short pipes, called risers, covered by a cap with aserrated edge, or slots. The bubble-cap plate is the traditional, oldest, type of cross-flowplate, and many different designs have been developed. Standard cap designs would nowbe specified for most applications.

The most significant feature of the bubble-cap plate is that the use of risers ensuresthat a level of liquid is maintained on the tray at all vapour flow-rates.


Figure 11.18. Sieve plate

Figure 11.19. Bubble-cap

3. Valve plates (floating cap plates) (Figure 11.20)Valve plates are proprietary designs. They are essentially sieve plates with large-diameterholes covered by movable flaps, which lift as the vapour flow increases.

As the area for vapour flow varies with the flow-rate, valve plates can operate efficientlyat lower flow-rates than sieve plates: the valves closing at low vapour rates.


Figure 11.20. Simple valve

Some very elaborate valve designs have been developed, but the simple type shown inFigure 11.20 is satisfactory for most applications.

Liquid flow pattern

Cross-flow trays are also classified according to the number of liquid passes on the plate.The design shown in Figure 11.21a is a single-pass plate. For low liquid flow rates reverseflow plates are used; Figure 11.21b. In this type the plate is divided by a low centralpartition, and inlet and outlet downcomers are on the same side of the plate. Multiple-pass plates, in which the liquid stream is sub-divided by using several downcomers, areused for high liquid flow-rates and large diameter columns. A double-pass plate is shownin Figure 11.21c.

11.12.1. Selection of plate type

The principal factors to consider when comparing the performance of bubble-cap, sieveand valve plates are: cost, capacity, operating range, efficiency and pressure drop.

Cost. Bubble-cap plates are appreciably more expensive than sieve or valve plates. Therelative cost will depend on the material of construction used; for mild steel the ratios,bubble-cap : valve : sieve, are approximately 3.0 : 1.5 : 1.0.

Capacity. There is little difference in the capacity rating of the three types (the diameterof the column required for a given flow-rate); the ranking is sieve, valve, bubble-cap.

Operating range. This is the most significant factor. By operating range is meant therange of vapour and liquid rates over which the plate will operate satisfactorily (the


(a)

(b)

(c)

Figure 11.21. Liquid flow patterns on cross-flow trays. (a) Single pass (b) Reverse flow (c) Double pass

stable operating range). Some flexibility will always be required in an operating plant toallow for changes in production rate, and to cover start-up and shut-down conditions. Theratio of the highest to the lowest flow rates is often referred to as the “turn-down” ratio.Bubble-cap plates have a positive liquid seal and can therefore operate efficiently at verylow vapour rates.

Sieve plates rely on the flow of vapour through the holes to hold the liquid on the plate,and cannot operate at very low vapour rates. But, with good design, sieve plates can bedesigned to give a satisfactory operating range; typically, from 50 per cent to 120 percent of design capacity.

Valve plates are intended to give greater flexibility than sieve plates at a lower costthan bubble-caps.

Efficiency. The Murphree efficiency of the three types of plate will be virtually thesame when operating over their design flow range, and no real distinction can be madebetween them; see Zuiderweg et al. (1960).

Pressure drop. The pressure drop over the plates can be an important design consid-eration, particularly for vacuum columns. The plate pressure drop will depend on thedetailed design of the plate but, in general, sieve plates give the lowest pressure drop,followed by valves, with bubble-caps giving the highest.

Summary. Sieve plates are the cheapest and are satisfactory for most applications.Valve plates should be considered if the specified turn-down ratio cannot be met withsieve plates. Bubble-caps should only be used where very low vapour (gas) rates have tobe handled and a positive liquid seal is essential at all flow-rates.

11.12.2. Plate construction

The mechanical design features of sieve plates are described in this section. The samegeneral construction is also used for bubble-cap and valve plates. Details of the various


types of bubble-cap used, and the preferred dimensions of standard cap designs, can befound in the books by Smith (1963) and Ludwig (1997). The manufacturers’ designmanuals should be consulted for details of valve plate design; Glitsch (1970) andKoch (1960).

Two basically different types of plate construction are used. Large-diameter plates arenormally constructed in sections, supported on beams. Small plates are installed in thecolumn as a stack of pre-assembled plates.

Sectional constructionA typical plate is shown in Figure 11.22. The plate sections are supported on a ring weldedround the vessel wall, and on beams. The beams and ring are about 50 mm wide, withthe beams set at around 0.6 m spacing. The beams are usually angle or channel sections,constructed from folded sheet. Special fasteners are used so the sections can be assembledfrom one side only. One section is designed to be removable to act as a manway. Thisreduces the number of manways needed on the vessel, which reduces the vessel cost.

Manway

Calming areaDowncomer and weir

Major beam

Major beamclamp, weldedto tower wall

Major beam

Minor beamsupport clamp

Subsupport plate ringused with angle ring

Minor beamsupport clamp

Subsupportangle ring

Peripheral ring clamps

Minor beam support clamp

Platesupportring

Figure 11.22. Typical sectional plate construction

Diagrams and photographs, of sectional plates, are given in Volume 2, Chapter 11.

Stacked plates (cartridge plates)The stacked type of construction is used where the column diameter is too small for aman to enter to assemble the plates, say less than 1.2 m (4 ft). Each plate is fabricated


complete with the downcomer, and joined to the plate above and below using screwed rods(spacers); see Figure 11.23. The plates are installed in the column shell as an assembly(stack) of ten, or so, plates. Tall columns have to be divided into flanged sections so thatplate assemblies can be easily installed and removed. The weir, and downcomer supports,are usually formed by turning up the edge of the plate.

Packagedfor installation

Downcomers

Spacer Topspacer

Hexagonalspacerbars

Screwed male/femalebar ends

Base spigotand bracket

Sta

ck o

f8

plat

es

Figure 11.23. Typical stacked-plate construction

The plates are not fixed to the vessel wall, as they are with sectional plates, so thereis no positive liquid seal at the edge of the plate, and a small amount of leakage willoccur. In some designs the plate edges are turned up round the circumference to makebetter contact at the wall. This can make it difficult to remove the plates for cleaning andmaintenance, without damage.

Downcomers

The segmental, or chord downcomer, shown in Figure 11.24a is the simplest and cheapestform of construction and is satisfactory for most purposes. The downcomer channel is


(a)

(b)

(c)

(d)

Figure 11.24. Segment (chord) downcomer designs. (a) Vertical apron (b) Inclined apron (c) Inlet weir(d) Recessed well

formed by a flat plate, called an apron, which extends down from the outlet weir. Theapron is usually vertical, but may be sloped (Figure 11.24b) to increase the plate areaavailable for perforation. If a more positive seal is required at the downcomer at the outlet,an inlet weir can be fitted (Figure 11.24c) or a recessed seal pan used (Figure 11.24d).Circular downcomers (pipes) are sometimes used for small liquid flow-rates.

Side-stream and feed points

Where a side-stream is withdrawn from the column the plate design must be modifiedto provide a liquid seal at the take-off pipe. A typical design is shown in Figure 11.25a.When the feed stream is liquid it will be normally introduced into the downcomer leadingto the feed plate, and the plate spacing increased at this point; Figure 11.25b.

Structural design

The plate structure must be designed to support the hydraulic loads on the plate duringoperation, and the loads imposed during construction and maintenance. Typical designvalues used for these loads are:

Hydraulic load: 600 N/m2 live load on the plate, plus 3000 N/m2 over thedowncomer seal area.

Erection and maintenance: 1500 N concentrated load on any structural member.

It is important to set close tolerances on the weir height, downcomer clearance, andplate flatness, to ensure an even flow of liquid across the plate. The tolerances specifiedwill depend on the dimensions of the plate but will typically be about 3 mm.


(a)

(b)

Figure 11.25. Feed and take-off nozzles

The plate deflection under load is also important, and will normally be specified asnot greater than 3 mm under the operating conditions for plates greater than 2.5 m, andproportionally less for smaller diameters.

The mechanical specification of bubble-cap, sieve and valve plates is covered in aseries of articles by Glitsch (1960), McClain (1960), Thrift (1960a, b) and Patton andPritchard (1960).

11.13. PLATE HYDRAULIC DESIGN

The basic requirements of a plate contacting stage are that it should:

Provide good vapour-liquid contact.Provide sufficient liquid hold-up for good mass transfer (high efficiency).Have sufficient area and spacing to keep the entrainment and pressure drop withinacceptable limits.Have sufficient downcomer area for the liquid to flow freely from plate to plate.

Plate design, like most engineering design, is a combination theory and practice. Thedesign methods use semi-empirical correlations derived from fundamental research workcombined with practical experience obtained from the operation of commercial columns.Proven layouts are used, and the plate dimensions are kept within the range of valuesknown to give satisfactory performance.


A short procedure for the hydraulic design of sieve plates is given in this section.Design methods for bubble-cap plates are given by Bolles (1963) and Ludwig (1997).Valve plates are proprietary designs and will be designed in consultation with the vendors.Design manuals are available from some vendors; Glistsch (1970) and Koch (1960).

A detailed discussion of the extensive literature on plate design and performance willnot be given in this volume. Chase (1967) and Zuiderweg (1982) give critical reviews ofthe literature on sieve plates.

Several design methods have been published for sieve plates: Kister (1992), Barnickiand Davies (1989), Koch and Kuzniar (1966), Fair (1963), and Huang and Hodson (1958);see also the book by Lockett (1986).

Operating range

Satisfactory operation will only be achieved over a limited range of vapour and liquidflow rates. A typical performance diagram for a sieve plate is shown in Figure 11.26.

Weeping

Dow

ncom

erba

ck-u

plim

itatio

nArea ofsatisfactoryoperationC

onin

g

Excessive

entrainment

Flooding

Liquid rate

Vap

our

rate

Figure 11.26. Sieve plate performance diagram

The upper limit to vapour flow is set by the condition of flooding. At flooding thereis a sharp drop in plate efficiency and increase in pressure drop. Flooding is caused byeither the excessive carry over of liquid to the next plate by entrainment, or by liquidbacking-up in the downcomers.

The lower limit of the vapour flow is set by the condition of weeping. Weeping occurswhen the vapour flow is insufficient to maintain a level of liquid on the plate. “Coning”occurs at low liquid rates, and is the term given to the condition where the vapour pushesthe liquid back from the holes and jets upward, with poor liquid contact.

In the following sections gas can be taken as synonymous with vapour when applyingthe method to the design of plates for absorption columns.


11.13.1. Plate-design procedure

A trial-and-error approach is necessary in plate design: starting with a rough plate layout,checking key performance factors and revising the design, as necessary, until a satisfactorydesign is achieved. A typical design procedure is set out below and discussed in thefollowing sections. The normal range of each design variable is given in the discussion,together with recommended values which can be used to start the design.

Procedure1. Calculate the maximum and minimum vapour and liquid flow-rates, for the turn

down ratio required.2. Collect, or estimate, the system physical properties.3. Select a trial plate spacing (Section 11.11).4. Estimate the column diameter, based on flooding considerations (Section 11.13.3).5. Decide the liquid flow arrangement (Section 11.13.4).6. Make a trial plate layout: downcomer area, active area, hole area, hole size, weir

height (Sections 11.13.8 to 11.13.10).7. Check the weeping rate (Section 11.13.6), if unsatisfactory return to step 6.8. Check the plate pressure drop (Section 11.13.14), if too high return to step 6.9. Check downcomer back-up, if too high return to step 6 or 3 (Section 11.13.15).

10. Decide plate layout details: calming zones, unperforated areas. Check hole pitch,if unsatisfactory return to step 6 (Section 11.13.11).

11. Recalculate the percentage flooding based on chosen column diameter.12. Check entrainment, if too high return to step 4 (Section 11.13.5).13. Optimise design: repeat steps 3 to 12 to find smallest diameter and plate spacing

acceptable (lowest cost).14. Finalise design: draw up the plate specification and sketch the layout.

This procedure is illustrated in Example 11.11.

11.13.2. Plate areas

The following areas terms are used in the plate design procedure:

Ac D total column cross-sectional area,Ad D cross-sectional area of downcomer,An D net area available for vapour-liquid disengagement, normally equal to Ac � Ad,

for a single pass plate,Aa D active, or bubbling, area, equal to Ac � 2Ad for single-pass plates,Ah D hole area, the total area of all the active holes,Ap D perforated area (including blanked areas),Aap D the clearance area under the downcomer apron.

11.13.3. Diameter

The flooding condition fixes the upper limit of vapour velocity. A high vapour velocityis needed for high plate efficiencies, and the velocity will normally be between 70 to


90 per cent of that which would cause flooding. For design, a value of 80 to 85 per centof the flooding velocity should be used.

The flooding velocity can be estimated from the correlation given by Fair (1961):

uf D K1

√�L � �v

�v

�11.81�

where uf D flooding vapour velocity, m/s, based on the net column cross-sectional areaAn (see Section 11.13.2),

K1 D a constant obtained from Figure 11.27.

Figure 11.27. Flooding velocity, sieve plates

The liquid-vapour flow factor FLV in Figure 11.27 is given by:

FLV D LwVw

√�v

�L�11.82�

where Lw D liquid mass flow-rate, kg/s,Vw D vapour mass flow-rate, kg/s.

The following restrictions apply to the use of Figure 11.27:

1. Hole size less than 6.5 mm. Entrainment may be greater with larger hole sizes.2. Weir height less than 15 per cent of the plate spacing.


3. Non-foaming systems.4. Hole: active area ratio greater than 0.10; for other ratios apply the following correc-

tions:hole: active area multiply K1 by

0.10 1.00.08 0.90.06 0.8

5. Liquid surface tension 0.02 N/m, for other surface tensions � multiply the value ofK1 by [�/0.02]0.2.

To calculate the column diameter an estimate of the net area An is required. As a firsttrial take the downcomer area as 12 per cent of the total, and assume that the hole activearea is 10 per cent.

Where the vapour and liquid flow-rates, or physical properties, vary significantlythroughout the column a plate design should be made for several points up the column.For distillation it will usually be sufficient to design for the conditions above and belowthe feed points. Changes in the vapour flow-rate will normally be accommodated byadjusting the hole area; often by blanking off some rows of holes. Different columndiameters would only be used where there is a considerable change in flow-rate. Changesin liquid rate can be allowed for by adjusting the liquid downcomer areas.

11.13.4. Liquid-flow arrangement

The choice of plate type (reverse, single pass or multiple pass) will depend on the liquidflow-rate and column diameter. An initial selection can be made using Figure 11.28,which has been adapted from a similar figure given by Huang and Hodson (1958).

Figure 11.28. Selection of liquid-flow arrangement


11.13.5. Entrainment

Entrainment can be estimated from the correlation given by Fair (1961), Figure 11.29,which gives the fractional entrainment (kg/kg gross liquid flow) as a function of theliquid-vapour factor FLV, with the percentage approach to flooding as a parameter.

The percentage flooding is given by:

percentage flooding D un actual velocity (based on net area)

uf (from equation 11.81)�11.83�

The effect of entrainment on plate efficiency can be estimated using equation 11.78.

Per cent flood

Fra

ctio

nal e

ntra

inm

ent,

100

10−1

30

35

40

45

50

60

70

80

90

95

FLV

10−2

10−3

10−2 10−1 100

Ψ

2 3 4 5 6 7 8 9 2 3 4 5 6 7 8 9

2

3

4

5

6

789

2

3

4

5

6789

2

3

4

5

6789

Figure 11.29. Entrainment correlation for sieve plates (Fair, 1961)


As a rough guide the upper limit of can be taken as 0.1; below this figure the effecton efficiency will be small. The optimum design value may be above this figure, seeFair (1963).

11.13.6. Weep point

The lower limit of the operating range occurs when liquid leakage through the plateholes becomes excessive. This is known as the weep point. The vapour velocity at theweep point is the minimum value for stable operation. The hole area must be chosenso that at the lowest operating rate the vapour flow velocity is still well above theweep point.

Several correlations have been proposed for predicting the vapour velocity at the weeppoint; see Chase (1967). That given by Eduljee (1959) is one of the simplest to use, andhas been shown to be reliable.

The minimum design vapour velocity is given by:

Luh D [K2 � 0.90�25.4 � dh�]

��v�1/2�11.84�

where Luh D minimum vapour velocity through the holes(based on the hole area), m/s,

dh D hole diameter, mm,

K2 D a constant, dependent on the depth of clear liquid on the plate, obtained

from Figure 11.30.

Figure 11.30. Weep-point correlation (Eduljee, 1959)


The clear liquid depth is equal to the height of the weir hw plus the depth of the crest ofliquid over the weir how; this is discussed in the next section.

11.13.7. Weir liquid crestThe height of the liquid crest over the weir can be estimated using the Francis weirformula (see Volume 1, Chapter 5). For a segmental downcomer this can be written as:

how D 750[Lw�Llw

]2/3

�11.85�

where lw D weir length, m,how D weir crest, mm liquid,Lw D liquid flow-rate, kg/s.

With segmental downcomers the column wall constricts the liquid flow, and the weir crestwill be higher than that predicted by the Francis formula for flow over an open weir. Theconstant in equation 11.85 has been increased to allow for this effect.

To ensure an even flow of liquid along the weir, the crest should be at least 10 mm atthe lowest liquid rate. Serrated weirs are sometimes used for very low liquid rates.

11.13.8. Weir dimensions

Weir heightThe height of the weir determines the volume of liquid on the plate and is an importantfactor in determining the plate efficiency (see Section 11.10.4). A high weir will increasethe plate efficiency but at the expense of a higher plate pressure drop. For columnsoperating above atmospheric pressure the weir heights will normally be between 40 mmto 90 mm (1.5 to 3.5 in.); 40 to 50 mm is recommended. For vacuum operation lower weirheights are used to reduce the pressure drop; 6 to 12 mm

( 14 to 1

2 in.)

is recommended.

Inlet weirsInlet weirs, or recessed pans, are sometimes used to improve the distribution of liquidacross the plate; but are seldom needed with segmental downcomers.

Weir lengthWith segmental downcomers the length of the weir fixes the area of the downcomer. Thechord length will normally be between 0.6 to 0.85 of the column diameter. A good initialvalue to use is 0.77, equivalent to a downcomer area of 12 per cent.

The relationship between weir length and downcomer area is given in Figure 11.31.For double-pass plates the width of the central downcomer is normally 200 250 mm

(8 10 in.).

11.13.9. Perforated area

The area available for perforation will be reduced by the obstruction caused by structuralmembers (the support rings and beams), and by the use of calming zones.


20

15

10

5

0.6 0.7 0.8 0.9

(Ad

/Ac)

x 10

0, p

er c

ent

l w / Dc

Figure 11.31. Relation between downcomer area and weir length

Calming zones are unperforated strips of plate at the inlet and outlet sides of the plate.The width of each zone is usually made the same; recommended values are: below 1.5 mdiameter, 75 mm; above, 100 mm.

The width of the support ring for sectional plates will normally be 50 to 75 mm: thesupport ring should not extend into the downcomer area. A strip of unperforated platewill be left round the edge of cartridge-type trays to stiffen the plate.

The unperforated area can be calculated from the plate geometry. The relationshipbetween the weir chord length, chord height and the angle subtended by the chord isgiven in Figure 11.32.

11.13.10. Hole size

The hole sizes used vary from 2.5 to 12 mm; 5 mm is the preferred size. Larger holesare occasionally used for fouling systems. The holes are drilled or punched. Punchingis cheaper, but the minimum size of hole that can be punched will depend on the platethickness. For carbon steel, hole sizes approximately equal to the plate thickness can bepunched, but for stainless steel the minimum hole size that can be punched is about twicethe plate thickness. Typical plate thicknesses used are: 5 mm (3/16 in.) for carbon steel,and 3 mm (12 gauge) for stainless steel.

When punched plates are used they should be installed with the direction of punchingupward. Punching forms a slight nozzle, and reversing the plate will increase thepressure drop.


0.4

θc l w Dc

0.3

lh

0.2L h

/Dc

Lw/Dc

0.1

0

130

110

90 θco

70

500.6 0.7 0.8 0.9

Figure 11.32. Relation between angle subtended by chord, chord height and chord length

11.13.11. Hole pitch

The hole pitch (distance between the hole centres) lp should not be less than 2.0 holediameters, and the normal range will be 2.5 to 4.0 diameters. Within this range thepitch can be selected to give the number of active holes required for the total hole areaspecified.

Square and equilateral triangular patterns are used; triangular is preferred. The totalhole area as a fraction of the perforated area Ap is given by the following expression, foran equilateral triangular pitch:

AhAp

D 0.9[dhlp

]2

�11.86�

This equation is plotted in Figure 11.33.

11.13.12. Hydraulic gradient

The hydraulic gradient is the difference in liquid level needed to drive the liquid flowacross the plate. On sieve plates, unlike bubble-cap plates, the resistance to liquid flowwill be small, and the hydraulic gradient is usually ignored in sieve-plate design. It can besignificant in vacuum operation, as with the low weir heights used the hydraulic gradientcan be a significant fraction of the total liquid depth. Methods for estimating the hydraulicgradient are given by Fair (1963).


2.0 2.5 3.0 3.5 4.0

0.05

0.10

0.15

0.2

IP / dh

Ah

/ Ap

Figure 11.33. Relation between hole area and pitch

11.13.13. Liquid throw

The liquid throw is the horizontal distance travelled by the liquid stream flowing overthe downcomer weir. It is only an important consideration in the design of multiple-passplates. Bolles (1963) gives a method for estimating the liquid throw.

11.13.14. Plate pressure drop

The pressure drop over the plates is an important design consideration. There are twomain sources of pressure loss: that due to vapour flow through the holes (an orifice loss),and that due to the static head of liquid on the plate.

A simple additive model is normally used to predict the total pressure drop. The totalis taken as the sum of the pressure drop calculated for the flow of vapour through thedry plate (the dry plate drop hd); the head of clear liquid on the plate (hw C how); anda term to account for other, minor, sources of pressure loss, the so-called residual losshr . The residual loss is the difference between the observed experimental pressure dropand the simple sum of the dry-plate drop and the clear-liquid height. It accounts for thetwo effects: the energy to form the vapour bubbles and the fact that on an operating platethe liquid head will not be clear liquid but a head of “aerated” liquid froth, and the frothdensity and height will be different from that of the clear liquid.

It is convenient to express the pressure drops in terms of millimetres of liquid. Inpressure units:

Pt D 9.81 ð 10�3ht�L �11.87�

where Pt D total plate pressure drop, Pa(N/m2),ht D total plate pressure drop, mm liquid.


Dry plate dropThe pressure drop through the dry plate can be estimated using expressions derived forflow through orifices.

hd D 51[uhC0

]2 �v

�L�11.88�

where the orifice coefficient C0 is a function of the plate thickness, hole diameter, andthe hole to perforated area ratio. C0 can be obtained from Figure 11.34; which has beenadapted from a similar figure by Liebson et al. (1957). uh is the velocity through theholes, m/s.

0 5 10 15 200.65

0.70

0.75

0.80

0.85

0.90

0.95

Plate thick

ness

Hole diameter

1.2

1.0

0.8

0.6

0.2

Orif

ice

coef

ficie

nt, C

0

Per cent perforated area, Ah / Ap x 100

Figure 11.34. Discharge coefficient, sieve plates (Liebson et al., 1957)


Residual headMethods have been proposed for estimating the residual head as a function of liquidsurface tension, froth density and froth height. However, as this correction term is smallthe use of an elaborate method for its estimation is not justified, and the simple equationproposed by Hunt et al. (1955) can be used:

hr D 12.5 ð 103

�L�11.89�

Equation 11.89 is equivalent to taking the residual drop as a fixed value of 12.5 mm ofwater � 1

2 in.�.

Total dropThe total plate drop is given by:

ht D hd C �hw C how�C hr �11.90�

If the hydraulic gradient is significant, half its value is added to the clear liquid height.

11.13.15. Downcomer design [back-up]

The downcomer area and plate spacing must be such that the level of the liquid and frothin the downcomer is well below the top of the outlet weir on the plate above. If the levelrises above the outlet weir the column will flood.

The back-up of liquid in the downcomer is caused by the pressure drop over the plate(the downcomer in effect forms one leg of a U-tube) and the resistance to flow in thedowncomer itself; see Figure 11.35.

Figure 11.35. Downcomer back-up


In terms of clear liquid the downcomer back-up is given by:

hb D �hw C how�C ht C hdc �11.91�

where hb D downcomer back-up, measured from plate surface, mm,hdc D head loss in the downcomer, mm.

The main resistance to flow will be caused by the constriction at the downcomer outlet,and the head loss in the downcomer can be estimated using the equation given by Cicaleseet al. (1947)

hdc D 166[Lwd�LAm

]2

�11.92�

where Lwd D liquid flow rate in downcomer, kg/s,Am D either the downcomer area Ad or the clearance area under the downcomer

Aap; whichever is the smaller, m2.

The clearance area under the downcomer is given by:

Aap D haplw �11.93�

where hap is height of the bottom edge of the apron above the plate. This height isnormally set at 5 to 10 mm

( 14 to 1

2 in.)

below the outlet weir height:

hap D hw � �5 to 10 mm�

Froth height

To predict the height of “aerated” liquid on the plate, and the height of froth in thedowncomer, some means of estimating the froth density is required. The density of the“aerated” liquid will normally be between 0.4 to 0.7 times that of the clear liquid. Anumber of correlations have been proposed for estimating froth density as a function ofthe vapour flow-rate and the liquid physical properties; see Chase (1967); however, noneis particularly reliable, and for design purposes it is usually satisfactory to assume anaverage value of 0.5 of the liquid density.

This value is also taken as the mean density of the fluid in the downcomer; which meansthat for safe design the clear liquid back-up, calculated from equation 11.91, should notexceed half the plate spacing lt, to avoid flooding.

Allowing for the weir height:

hb 6> 12 �lt C hw� �11.94�

This criterion is, if anything, oversafe, and where close plate spacing is desired a betterestimate of the froth density in the downcomer should be made. The method proposedby Thomas and Shah (1964) is recommended.

Downcomer residence time

Sufficient residence time must be allowed in the downcomer for the entrained vapour todisengage from the liquid stream; to prevent heavily “aerated” liquid being carried underthe downcomer.


A time of at least 3 seconds is recommended.The downcomer residence time is given by:

tr D Adhbc�LLwd

�11.95�

where tr D residence time, s,hbc D clear liquid back-up, m.

Example 11.11

Design the plates for the column specified in Example 11.2. Take the minimum feed rateas 70 per cent of the maximum (maximum feed 10,000 kg/h). Use sieve plates.

Solution

As the liquid and vapour flow-rates and compositions will vary up the column, platedesigns should be made above and below the feed point. Only the bottom plate will bedesigned in detail in this example.

From McCabe-Thiele diagram, Example 11.2:

Number of stages D 16Slope of the bottom operating line D 5.0Slope of top operating line D 0.57Top composition 94 per cent mol. 98 per cent w/w.Bottom composition essentially water.Reflux ratio D 1.35

Flow-rates

Mol. weight feed D 0.033 ð 58 C �1 � 0.033�18 D 19.32Feed D 13,000/19.32 D 672.9 kmol/hA mass balance on acetone gives:

Top product, D D 672.9 ð 0.033/0.94 D 23.6 kmol/hVapour rate, V D D�1 C R� D 23.6�1 C 1.35� D 55.5 kmol/h

An overall mass balance gives:Bottom product, B D 672.9 � 23.6 D 649.3 kmol/hSlope of the bottom operating line Lm0/Vm 0 D 5.0

and Vm 0 D Lm0 � B, from which:vapour flow below feed, Vm 0 D 162.3 kmol/hliquid flow below feed, Lm0 D 811.6 kmol/h

Physical propertiesEstimate base pressure, assume column efficiency of 60 per cent, take reboiler as equiv-alent to one stage.

Number of real stages D 16 � 1

0.6D 25


Assume 100 mm water, pressure drop per plate.

Column pressure drop D 100 ð 10�3 ð 1000 ð 9.81 ð 25 D 24,525 Pa

Top pressure, 1 atm (14.7 lb/in2) D 101.4 ð 103 Pa

Estimated bottom pressure D 101.4 ð 103 C 24,525

D 125,925 Pa D 1.26 bar

From steam tables, base temperature 106ŽC.

�v D 0.72 kg/m3

�L D 954 kg/m3

Surface tension 57 ð 10�3 N/m

Top, 98% w/w acetone, top temperature 57ŽC

From PPDS (see Chapter 8);

�v D 2.05 kg/m3, �L D 753 kg/m3

Molecular weight 55.6

Surface tension 23 ð 10�3 N/m

Column diameter

FLV bottom D 5.0

√0.72

954D 0.14 �11.82�

FLV top D 0.57

√2.05

753D 0.03

Take plate spacing as 0.5 mFrom Figure 11.27

base K1 D 7.5 ð 10�2

top K1 D 9.0 ð 10�2

Correction for surface tensions

base K1 D(

57

20

)0.2

ð 7.5 ð 10�2 D 9.3 ð 10�2

top K1 D(

23

20

)0.2

ð 9.0 ð 10�2 D 9.3 ð 10�2

base uf D 9.3 ð 10�2

√954 � 0.72

0.72D 3.38 m/s �11.81�

top uf D 9.3 ð 10�2

√753 � 2.05

2.05D 1.78 m/s


Design for 85 per cent flooding at maximum flow rate

base Ouv D 3.38 ð 0.85 D 2.87 m/s

top Ouv D 1.78 ð 0.85 D 1.51 m/s

Maximum volumetric flow-rate

base D 162.3 ð 18

0.72 ð 3600D 1.13 m3/s

top D 55.5 ð 55.6

2.05 ð 3600D 0.42 m3/s

Net area required

bottom D 1.13

2.87D 0.40 m2

top D 0.42

1.51D 0.28 m2

As first trial take downcomer area as 12 per cent of total.Column cross-sectioned area

base D 0.40

0.88D 0.46 m2

top D 0.28

0.88D 0.32 m2

Column diameter

base D√

0.46 ð 4

D 0.77 m

top D√

0.34 ð 4

D 0.64 m

Use same diameter above and below feed, reducing the perforated area for plates abovethe feed.

Nearest standard pipe size (BS 1600); outside diameter 812.8 mm (32 in); standardwall thickness 9.52 mm; inside diameter 794 mm.

Liquid flow pattern

Maximum volumetric liquid rate D 811.6 ð 18

3600 ð 954D 4.3 ð 10�3 m3/s

The plate diameter is outside the range of Figure 11.28, but it is clear that a single passplate can be used.

Provisional plate design

Column diameter Dc D 0.79 mColumn area Ac D 0.50 m2

Downcomer area Ad D 0.12 ð 0.50 D 0.06 m2, at 12 per centNet area An D Ac � Ad D 0.50 � 0.06 D 0.44 m2


Active area Aa D Ac � 2Ad D 0.50 � 0.12 D 0.38 m2

Hole area Ah take 10 per cent Aa as first trial D 0.038 m2

Weir length (from Figure 11.31) D 0.76 ð 0.79 D 0.60 m

Take weir height 50 mmHole diameter 5 mmPlate thickness 5 mm

Check weeping

Maximum liquid rate D(

811.6 ð 18

3600

)D 4.06 kg/s

Minimum liquid rate, at 70 per cent turn-down D 0.7 ð 4.06 D 2.84 kg/s

maximum how D 750(

4.06

954 ð 0.06

)2/3

D 27 mm liquid �11.85�

minimum how D 750(

2.85

954 ð 0.60

)2/3

D 22 mm liquid

at minimum rate hw C how D 50 C 22 D 72 mm

From Figure 11.30, K2 D 30.6

Luh�min� D 30.6 � 0.90�25.4 � 5�

�0.72�1/2D 14 m/s �11.84�

actual minimum vapour velocity D minimum vapour rate

Ah

D 0.7 ð 1.13

0.038D 20.8 m/s

So minimum operating rate will be well above weep point.

Plate pressure dropDry plate dropMaximum vapour velocity through holes

Ouh D 1.13

0.038D 29.7 m/s

From Figure 11.34, for plate thickness/hole dia. D 1, and Ah/Ap ' Ah/Aa D 0.1,C0 D 0.84

hd D 51(

29.7

0.84

)2 0.72

954D 48 mm liquid �11.88�

residual head

hr D 12.5 ð 103

954D 13.1 mm liquid �11.89�


total plate pressure drop

ht D 48 C �50 C 27�C 13 D 138 mm liquid

Note: 100 mm was assumed to calculate the base pressure. The calculation could berepeated with a revised estimate but the small change in physical properties will havelittle effect on the plate design. 138 mm per plate is considered acceptable.

Downcomer liquid back-up

Downcomer pressure lossTake hap D hw � 10 D 40 mm.Area under apron, Aap D 0.60 ð 40 ð 10�3 D 0.024 m2.As this is less than Ad D 0.06 m2 use Aap in equation 11.92

hdc D 166(

4.06

954 ð 0.024

)2

D 5.2 mm �11.92�

say 6 mm.

Back-up in downcomer

hb D �50 C 27�C 138 C 6 D 221 mm �11.91�

0.22 m

0.22 < 12 (plate spacing C weir height)

so plate spacing is acceptable

Check residence time

tr D 0.06 ð 0.22 ð 954

4.06D 3.1 s �11.95�

>3 s, satisfactory.

Check entrainment

uv D 1.13

0.44D 2.57 m/s

per cent flooding D 2.57

3.38D 76

FLV D 0.14, from Figure 11.29, D 0.018, well below 0.1.

As the per cent flooding is well below the design figure of 85, the column diametercould be reduced, but this would increase the pressure drop.

Trial layout

Use cartridge-type construction. Allow 50 mm unperforated strip round plate edge; 50 mmwide calming zones.


0.6

m

50 mm

0.79

m

50 mm

θc

Perforated area

From Figure 11.32, at lw/Dc D 0.6/0.79 D 0.76�c D 99Ž

angle subtended by the edge of the plate D 180 � 99 D 81Ž

mean length, unperforated edge strips D �0.79 � 50 ð 10�3� ð 81/180 D 1.05 marea of unperforated edge strips D 50 ð 10�3 ð 1.05 D 0.053 m2

mean length of calming zone, approx. D weir length C width of unperforated stripD 0.6 C 50 ð 10�3 D 0.65 m

area of calming zones D 2�0.65 ð 50 ð 10�3� D 0.065 m2

total area for perforations, Ap D 0.38 � 0.053 � 0.065 D 0.262 m2

Ah/Ap D 0.038/0.262 D 0.145From Figure 11.33, lp/dh D 2.6; satisfactory, within 2.5 to 4.0.

Number of holes

Area of one hole D 1.964 ð 10�5 m2

Number of holes D 0.038

1.964 ð 10�5D 1935

Plate specification

50 mm

50 mm

0.60

m

0.79

m

40 mm

50 mm

Plate No. 1 Turn-down 70 per cent max ratePlate I.D. 0.79 m Plate material Mild steelHole size 5 mm Downcomer material Mild steelHole pitch 12.5 mm Plate spacing 0.5 mTotal no. holes Plate thickness 5 mmActive holes 1935 Plate pressure drop 140 mm liquid D 1.3 kPaBlanking area

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CHAPTER 11 Separation Columns (Distillation, …...design calculations. If a column is poorly insulated, changes in the internal reﬂux due to sudden changes in the external conditions,