Design of Distillation Columns

07/03/2012 18:44

Lectures 1&2
Distillation- fundamental principle The vapour of a boiling liquid mixture will be richer in the components that have lower boiling points. Condensed vapour will contain more volatile components Distillation is one of the most common processes in industry, & is very energy intensive (heating and cooling), it can be up to 50% of costs. Design of distillation columns Involves determination of number of stages required for a given separation
Graphically by McCabe- Thiele method (uses operating lines and equilibrium curve)

Involves hydraulic design:

Selection of tray type or packing materials Column sizing (i.e diameter and height of column) Determination of pressure drop Consideration of flooding, weeping, entrainment and foaming ect. (for plate columns) or HETP, degree of wetting, flooding etc. (for packed columns)

Two main types of distillation

Batch- the feed introduced to the column batch wise. Continuous- no interruption occurs, ( Binary systems and multicomponent systems)

Column internals: Trays vs. Packings Trays: stagewise process (used to hold up the liquid to give better separation) Type of trays:
Sieve Valve Bubble cap

Packings: continuous process (packed columns are used to enhance contact between vapour & liquid) Type of packing:
Random packings Structured packings

Tray Columns Basic requirements of tray design:

Intimate mixing between liquid and vapour streams for efficient exchange of components Provide sufficient liquid hold-up for high efficiency mass transfer Ability to handle desired rates of vapour and liquid flows without excessive liquid entrainment or flooding Minimal pressure drop on each tray (especially important in vacuum operation)

Typical tray operation Single pass cross flow liquid arrangement as shown o Liquid flows across plate and vapour flows up through plate
o o

Transfer of liquid from plate to plate via downcomers (gravity) Outlet weir on edge of plate to retain a level of liquid on plate (i.e liquid hold-up)

Other types of liquid flow arrangements on trays o Reverse flow (low liquid rates) o Double pass (high liquid rates) o Four pass also possible with bigger trays (for even higher liquid rates) Different configurations have downcomers fitted at various positions on the tray to appropriately direct liquid flows Distillation Trays Sieve tray: metal, diameter & number of holes are design considerations (cheep and simple) Bubble Cap tray: has raised chimneys fitted over each holed, a cap covers the riser. There is a space between riser and cap to allow the passage of vapour. The vapour rises through the chimney directed downwards by the cap on discharging through slots in the cap bubbling through the liquid on the tray. Valve Tray: perforations are covered by lift able caps, self creating a flow area for passage of vapour through the liqu\id. The lifting caps direct the vapour to flow horizontally into the liquid (better mixing)

Recap Distillation: process in which a liquid or vapour mixture of two or more substances into its component fractions of desired purity. Vertical shell where separation of liquid components is carried out. Internal trays of packing; valve trays, bubble caps, side trays. Reboiler to provide the necessary tray vaporisation the distillation process. Condenser to cool and condense the vapour leaving the top of the column. Reflux drum to hold the condensate vapour from the top of the column, so that liquid (reflux) can be recycled back to the column.

Which tray type? Factors to consider: Cost Operation range/ flexibility Efficiency Pressure drop Generally sieve plates are satisfactory for many applications (except for very low vapour flow rates) Packed columns Packing characteristics in operation: Large surface area for maximum vapour/ liquid contact High degree of turbulence to promote rapid, efficient mass transfer between phases Open structure for low resistance to vapour flow, hence low pressure drops

Promote uniform liquid distribution on surface Promote uniform gas flow across column cross-section Liquid films flow down over the surface of packing gas flows up through the open structure of packing close contact between liquid and gas is achieved. Progressive or continued transfer of more volatile component from liquid to vapour and less volatile component from vapour to liquid. Interfacial area, turbulence and free flow area considerations are addressed by design of packing. Smaller packing: increased capital cost, higher pressure drop, increased surface area. Packings- note will need more energy to drive vapour up the column when using packing. Three types:

Broken solids; cheapest, hardly used, non-uniformity in size, unreliable performance, high pressure drop

Shaped packing/ random packing Structured packing Various random shaped packing including: Rasching Rings: simple hollow ring, oldest, cheapest, most widely used, less effective, not necessarily most economic. Can be made in various material and ceramic and carbon. Lessing Rings: Rasching Rings with partitions across its centre, increased surface area and strength. Ceramic and metals Pall Rings: superior performance, highly effective give better wetting and distillation. Liquid smaller pressure drop than Rasching under same conditions, available in metals, ceramics and plastics. Berl saddles: less free gas space better aerodynamic shape, ceramic or plastic.

(super) Intalox saddles Metal Hypac Mini Rings Mini rings and metal saddle design gives high performance and low pressure drop. Pall rings and interlox saddles most popular of packing, high efficiencies at low pressure drops. Selection of random packing Need to consider: Type Size Material

Choice of size of random packings Size of packing affects Height of column Pressure drop Cost Large packings Are cheaper (based on unit volume) Give lower pressure drop per meter of packing Give reduced mass transfer efficiency and therefore result in the need for taller columns (more separation stages)

 Do not necessarily result in reduced overall cost of column Typically, packing size 1/8 of column diameter

Choice of material for random packings Ceramics- easily broken not strong Plastics- organic solvents, cant be used at high temperatures Carbon Choice based on: Nature of fluids Operating temperature Strength of packing required

Structured Packings Wire mesh or perforated metal sheets High surface area and high voidage Lower HETP (height equivalent of theoretical plate), due to higher efficiency, and pressure drop than random packings. Significantly more expensive than random packings

H:L/N L: length of column N: number of theoretical plates

Plates or Packing Choice dependent on the following considerations: Column diameter Range of operating conditions required Liquid flowrates Liquid distribution Foaming Fouling systems Corrosive systems Heat evolution and sidestream Pressure drop Liquid hold-up Maintenance Weight

Lectures 3 & 4
Design of sieve tray columns (sievewise distillation) Downcomer: liquid falls down through downcomer by gravity from one tray to the one below it. Weir: ensure that there is always some liquid hold up Sieve tray, single pass cross flow liquid arrangement hdc : height of downcomer hw : height of weir how: height of liquid over weir Ts: Tray spacing hw + how = static liquid seal of a tray Design procedure of sieve trays For specified vapour and liquid flows (and physical properties), need to estimate tray diameter, spacing and layout which will give acceptable: Entrainment Approach to flooding Weeping Pressure drop on each tray Height of liquid back-up in downcomer

Entrainment Entrainment refers to the liquid carried by vapour up to the tray above, it occurs at high vapour flows and relatively low liquid flows. It is detrimental because: tray efficiency is reduced (less volatile material is carried to plate holding liquid of higher volatility), it could contaminate high purity distillate, excessive entrainment can lead to flooding. Chocking (blockage) of downcomer can set a limit to the liquid flowrate when the inflowing gas-liquid dispersion needs more space when large amount of gas is set free in the downcomer. The separated gas rises counter to the down flowing gas containing liquid and can induce blocking condition.

Flooding Brought about by excessive vapour flow Liquid entrainment in vapour (entrainment flooding) Backing up of liquid in the downcomer (downcomer flooding) Determines maximum capacity of the column, detected by: Sharp increases in column differential pressure Significant decrease in separation efficiency Flooding is brought about by excessive vapour flow causing liquid to be entrained in the vapour up the column. Depending on the degree of flooding the max capacity of the column severely reduced. Entrainment flooding Caused by excessive liquid droplets being carried up to tray above Occurs at high gas flows and with thin liquid layer on tray (gives rise to tray spray regime) Impact dependent on tray spacing Also referred to as bed expansion flooding

Downcomer flooding Occurs when height of gas- liquid mixture in downcomer (hdc) exceeds height of downcomer

Bed expansion flooding sets when the gas-liquid layer on the tray extends to the next (higher) tray the dispersion height becomes equal to the tray spacing. Depends on: liquid height on a tray, expansion of liquid. Equivalent to entrainment flooding, drop entrainment rises rapidly. Downcomer over flowing- when the height of gas liquid layer in the downcomer exceeds the height of the downcomer. Weeping/ Dumping Caused by low vapour flow: vapour is insufficient to hold up the liquid on the tray o liquid starts to leak through perforations (weeping) excessive weeping will lead to dumping o the liquid on all trays will crash through to the base of the column (via a domino effect) o detected by sharp pressure drop and separation efficiency

weep point, the gas flowrate at which the first leakage of liquid starts because the gas flowing up through perforation is no longer able to counter balance the hydrostatic head of liquid on a tray. Pressure drop Total tray pressure drop, PT, is made up of: Dry tray pressure drop, Pdry o Determined by gas flowing through holes in tray

Pressure drop due to liquid hold up o Liquid depth on tray offers additional resistance to gas flow The tray pressure drop is composed of at least two major contributions: 1) a pressure drop by the gas flowing through the perforations a. Depends on gas flowrate, fractions of free area, pressure drof coefficients of particular perfations. b. Depends on relative hole thickness, hole shape nearness of other holes. 2) a pressure drop caused by the liquid present on the tray. This liquid hold up effect primarily increases with an increase in outlet weir height, decreases with an increase in gas flowrate & increase in liquid flowrate. 3) Depends on physical properties of gas/liquid system hT = hd + h hd =dry tray pressure drop h=gas through liquid Foaming: expansion of liquid due to passages of vapour or gas Height of liquid back-up in downcomer (hdc) Caused by: Pressure drop over plate Resistance to flow in downcomer

Tray spacing, Ts, is a design parameter chosen to prevent liquid in the downcomer backing up to the tray above. For safe design avoiding downcomer flooding: hdc Ts Most factors that affect column operation is due to vapour flows. Weeping determines the minimum vapour flow. Flooding determines the maximum vapour flow.

Tutorial Question Liquid flowrate, L=0.14 kmol/s Vapour flowrate, V=0.15 kmol/s Average molecular mass of liquid vapour =70kg/kmol Liquid density, L = 700kg/m3 Vapour density, V = 2.26kg/m3 Flooding= 80% Height of weir hw =50mm Ts=0.45m hap=38mm single pass cross flow from liquid arrangement graph DT = 2.45m < 0.1 entrainment ok Weeping use weep point correlation, k2 vs (hw+how) chart q=(0.14*70)/700 =0.014m3/s Lw=0.77*DT=1.89 how= 750 (q/Lw)^0.67 how= 750 (0.014/1.89)^0.67 hw+how=50+28=78mm k2=30.7 Uh min= [k2-0.9(25.4-dh)]/(v) Uh min= [30.7-0.9(25.4-4.76)]/(2.26) Uh min= 8.06m/s Uh actual=QV/Aholes=4.65/0.076AT=4.65/0.076*4.7= 13m/s Uh actual > Uh min no weeping

Pressure drop total =dry +ha ha = due to aerated liquid on tray

dry= 50.8 (V/L)(Uh/Cv0)2 Cv0 =discharge coefficient, 0.76 dry= 50.8 (2.26/700)(13/0.76)2 =48mm of liquid=330N/m2 note dry is m of liquid to get in N/m2 dry =(mm of liquid) * L * g

ha =Qp (hw + how) =0.6(78) =46.8m Qp : depends on how much froth is produced (high flowrate + low Active area )=low Qp T = 48 + 46.8 =94.8 = 651 N/m2 axis ion the graph Qp vs Fv=Q/Aa(v) note : acceptable T between 300-1200 N?m2 per tray for atmospheric duty. Height of liquid back up in downcomer hdc= T +(hw +how ++ hda) : liquid gradient difference in liquid level needed to drive liquid flow across plate. is negligible for sieve tray, can be significant in vacuum operation.

hda= loss under down comer apron =165 (q/Ada)2 Clearance area under downcomer apron Ada = hap * LW (m2) =0.038 *1.89=0.072m2

Typically hap=hw-(5 to 10mm) hda =165 (0.014/0.072)2 =6.24 mm of liquid hdc = 94.8 + 50 +28 +0 +6.24 =179mm of liquid check hdc Ts Ts = 0.45m Ts = 0.179m hdc < Ts risk of flooding is low

residence time tr = (Adc * hdc)/ qL =0.12*AT*0.179/ 0.014 =0.12*4.7*0.179/ 0.014=7.25 >3s minimum

07/03/2012 18:44

07/03/2012 18:44