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<strong>Design</strong> <strong>of</strong> <strong>Distillation</strong> <strong>Columns</strong> 07/03/2012 18:44<br />

Lectures 1&2<br />

<strong>Distillation</strong>- fundamental principle<br />

The vapour <strong>of</strong> a boiling liquid mixture will be richer in the components that have<br />

lower boiling points.<br />

Condensed vapour will contain more volatile components<br />

<strong>Distillation</strong> is one <strong>of</strong> the most common processes in industry, & is very energy<br />

intensive (heating and cooling), it can be up to 50% <strong>of</strong> costs.<br />

<strong>Design</strong> <strong>of</strong> distillation columns<br />

Involves determination <strong>of</strong> number <strong>of</strong> stages required for a given separation<br />

• Graphically by McCabe- Thiele method (uses operating lines and equilibrium curve)<br />

Involves hydraulic design:<br />

• Selection <strong>of</strong> tray type or packing materials<br />

• Column sizing (i.e diameter and height <strong>of</strong> column)<br />

• Determination <strong>of</strong> pressure drop<br />

• Consideration <strong>of</strong> flooding, weeping, entrainment and foaming ect. (for plate columns) or HETP,<br />

degree <strong>of</strong> wetting, flooding etc. (for packed columns)<br />

Two main types <strong>of</strong> distillation<br />

• Batch- the feed introduced to the column batch wise.<br />

• Continuous- no interruption occurs, ( Binary systems and multicomponent systems)<br />

Column internals: Trays vs. Packings<br />

Trays: stagewise process (used to hold up the liquid to give better separation)<br />

• Type <strong>of</strong> trays:<br />

• Sieve<br />

• Valve<br />

• Bubble cap<br />

Packings: continuous process (packed columns are used to enhance contact<br />

between vapour & liquid)<br />

• Type <strong>of</strong> packing:<br />

• Random packings<br />

• Structured packings


Tray <strong>Columns</strong><br />

Basic requirements <strong>of</strong> tray design:<br />

• Intimate mixing between liquid and vapour streams for efficient exchange <strong>of</strong><br />

components<br />

• Provide sufficient liquid hold-up for high efficiency mass transfer<br />

• Ability to handle desired rates <strong>of</strong> vapour and liquid flows without excessive liquid<br />

entrainment or flooding<br />

• Minimal pressure drop on each tray (especially important in vacuum operation)<br />

Typical tray operation<br />

Single pass cross flow liquid arrangement as shown<br />

o Liquid flows across plate and vapour flows up through plate<br />

o Transfer <strong>of</strong> liquid from plate to plate via downcomers (gravity)<br />

o Outlet weir on edge <strong>of</strong> plate to retain a level <strong>of</strong> liquid on plate (i.e liquid<br />

hold-up)<br />

Other types <strong>of</strong> liquid flow arrangements on trays<br />

o Reverse flow (low liquid rates)<br />

o Double pass (high liquid rates)<br />

o Four pass also possible with bigger trays (for even higher liquid rates)<br />

Different configurations have downcomers fitted at various positions on the tray to<br />

appropriately direct liquid flows<br />

<strong>Distillation</strong> Trays<br />

Sieve tray: metal, diameter & number <strong>of</strong> holes are design considerations (cheep and<br />

simple)<br />

Bubble Cap tray: has raised chimneys fitted over each holed, a cap covers the<br />

riser. There is a space between riser and cap to allow the passage <strong>of</strong> vapour.<br />

The vapour rises through the chimney directed downwards by the cap on<br />

discharging through slots in the cap bubbling through the liquid on the tray.<br />

Valve Tray: perforations are covered by lift able caps, self creating a flow area for<br />

passage <strong>of</strong> vapour through the liqu\id. The lifting caps direct the vapour to flow<br />

horizontally into the liquid (better mixing)


Recap<br />

<strong>Distillation</strong>: process in which a liquid or vapour mixture <strong>of</strong> two or more substances<br />

into its component fractions <strong>of</strong> desired purity.<br />

• Vertical shell where separation <strong>of</strong> liquid components is carried out.<br />

• Internal trays <strong>of</strong> packing; valve trays, bubble caps, side trays.<br />

• Reboiler to provide the necessary tray vaporisation the distillation process.<br />

• Condenser to cool and condense the vapour leaving the top <strong>of</strong> the column.<br />

• Reflux drum to hold the condensate vapour from the top <strong>of</strong> the column, so<br />

Which tray type?<br />

Factors to consider:<br />

that liquid (reflux) can be recycled back to the column.<br />

• Cost<br />

• Operation range/ flexibility<br />

• Efficiency<br />

• Pressure drop<br />

Generally sieve plates are satisfactory for many applications (except for very low<br />

vapour flow rates)<br />

Packed columns<br />

Packing characteristics in operation:<br />

• Large surface area for maximum vapour/ liquid contact<br />

• High degree <strong>of</strong> turbulence to promote rapid, efficient mass transfer<br />

between phases<br />

• Open structure for low resistance to vapour flow, hence low pressure<br />

drops<br />

• Promote uniform liquid distribution on surface<br />

• Promote uniform gas flow across column cross-section<br />

Liquid films flow down over the surface <strong>of</strong> packing gas flows up through the open<br />

structure <strong>of</strong> packing close contact between liquid and gas is achieved.<br />

Progressive or continued transfer <strong>of</strong> more volatile component from liquid to vapour<br />

and less volatile component from vapour to liquid.<br />

Interfacial area, turbulence and free flow area considerations are addressed by<br />

design <strong>of</strong> packing. Smaller packing: increased capital cost, higher pressure drop,<br />

increased surface area.<br />

Packings- note will need more energy to drive vapour up the column when using packing.<br />

Three types:


• Broken solids; cheapest, hardly used, non-uniformity in size, unreliable<br />

performance, high pressure drop<br />

• Shaped packing/ random packing<br />

• Structured packing<br />

Various random shaped packing including:<br />

• Rasching Rings: simple hollow ring, oldest, cheapest, most widely used,<br />

less effective, not necessarily most economic. Can be made in various<br />

material and ceramic and carbon.<br />

• Lessing Rings: Rasching Rings with partitions across its centre,<br />

increased surface area and strength. Ceramic and metals<br />

• Pall Rings: superior performance, highly effective give better wetting and<br />

distillation. Liquid smaller pressure drop than Rasching under same<br />

conditions, available in metals, ceramics and plastics.<br />

• Berl saddles: less free gas space better aerodynamic shape, ceramic or<br />

plastic.<br />

• (super) Intalox saddles<br />

• Metal Hypac<br />

• Mini Rings<br />

Mini rings and metal saddle design gives high performance and low pressure<br />

drop. Pall rings and interlox saddles most popular <strong>of</strong> packing, high efficiencies at<br />

low pressure drops.<br />

Selection <strong>of</strong> random packing<br />

Need to consider:<br />

• Type<br />

• Size<br />

• Material<br />

Choice <strong>of</strong> size <strong>of</strong> random packings<br />

Size <strong>of</strong> packing affects<br />

• Height <strong>of</strong> column<br />

• Pressure drop<br />

• Cost<br />

Large packings<br />

• Are cheaper (based on unit volume)<br />

• Give lower pressure drop per meter <strong>of</strong> packing<br />

• Give reduced mass transfer efficiency and therefore result in the need for<br />

taller columns (more separation stages)


• Do not necessarily result in reduced overall cost <strong>of</strong> column<br />

Typically, packing size ≤ 1/8 <strong>of</strong> column diameter<br />

Choice <strong>of</strong> material for random packings<br />

• Ceramics- easily broken not strong<br />

• Plastics- organic solvents, cant be used at high temperatures<br />

• Carbon<br />

Choice based on:<br />

• Nature <strong>of</strong> fluids<br />

• Operating temperature<br />

• Strength <strong>of</strong> packing required<br />

Structured Packings<br />

• Wire mesh or perforated metal sheets<br />

• High surface area and high voidage<br />

• Lower HETP (height equivalent <strong>of</strong> theoretical plate), due to higher<br />

efficiency, and pressure drop than random packings.<br />

• Significantly more expensive than random packings<br />

H:L/N<br />

• L: length <strong>of</strong> column<br />

• N: number <strong>of</strong> theoretical plates<br />

Plates or Packing<br />

Choice dependent on the following considerations:<br />

• Column diameter<br />

• Range <strong>of</strong> operating conditions required<br />

• Liquid flowrates<br />

• Liquid distribution<br />

• Foaming<br />

• Fouling systems<br />

• Corrosive systems<br />

• Heat evolution and sidestream<br />

• Pressure drop<br />

• Liquid hold-up<br />

• Maintenance<br />

• Weight


Lectures 3 & 4<br />

<strong>Design</strong> <strong>of</strong> sieve tray columns (sievewise distillation)<br />

Downcomer: liquid falls down through downcomer by gravity from one tray to the<br />

one below it.<br />

Weir: ensure that there is always some liquid hold up<br />

Sieve tray, single pass cross flow liquid arrangement<br />

hdc : height <strong>of</strong> downcomer<br />

hw : height <strong>of</strong> weir<br />

how: height <strong>of</strong> liquid over weir<br />

Ts: Tray spacing<br />

hw + how = static liquid seal <strong>of</strong> a tray<br />

<strong>Design</strong> procedure <strong>of</strong> sieve trays<br />

For specified vapour and liquid flows (and physical properties), need to estimate tray<br />

diameter, spacing and layout which will give acceptable:<br />

• Entrainment<br />

• Approach to flooding<br />

• Weeping<br />

Entrainment<br />

• Pressure drop on each tray<br />

• Height <strong>of</strong> liquid back-up in downcomer<br />

Entrainment refers to the liquid carried by vapour up to the tray above, it occurs at<br />

high vapour flows and relatively low liquid flows. It is detrimental because: tray<br />

efficiency is reduced (less volatile material is carried to plate holding liquid <strong>of</strong><br />

higher volatility), it could contaminate high purity distillate, excessive entrainment<br />

can lead to flooding.<br />

Chocking (blockage) <strong>of</strong> downcomer can set a limit to the liquid flowrate when the<br />

inflowing gas-liquid dispersion needs more space when large amount <strong>of</strong> gas is<br />

set free in the downcomer. The separated gas rises counter to the down flowing<br />

gas containing liquid and can induce blocking condition.


Flooding<br />

Brought about by excessive vapour flow<br />

• Liquid entrainment in vapour (entrainment flooding)<br />

• Backing up <strong>of</strong> liquid in the downcomer (downcomer flooding)<br />

Determines maximum capacity <strong>of</strong> the column, detected by:<br />

• Sharp increases in column differential pressure<br />

• Significant decrease in separation efficiency<br />

Flooding is brought about by excessive vapour flow causing liquid to be entrained in<br />

the vapour up the column. Depending on the degree <strong>of</strong> flooding the max capacity<br />

<strong>of</strong> the column severely reduced.<br />

Entrainment flooding<br />

• Caused by excessive liquid droplets being carried up to tray above<br />

• Occurs at high gas flows and with thin liquid layer on tray (gives rise to tray<br />

spray regime)<br />

• Impact dependent on tray spacing<br />

• Also referred to as bed expansion flooding<br />

Downcomer flooding<br />

• Occurs when height <strong>of</strong> gas- liquid mixture in downcomer (hdc) exceeds<br />

height <strong>of</strong> downcomer<br />

Bed expansion flooding sets when the gas-liquid layer on the tray extends to the next<br />

(higher) tray the dispersion height becomes equal to the tray spacing.<br />

Depends on: liquid height on a tray, expansion <strong>of</strong> liquid.<br />

Equivalent to entrainment flooding, drop entrainment rises rapidly. Downcomer over<br />

flowing- when the height <strong>of</strong> gas liquid layer in the downcomer exceeds the height <strong>of</strong><br />

the downcomer.<br />

Weeping/ Dumping<br />

Caused by low vapour flow:<br />

• vapour is insufficient to hold up the liquid on the tray<br />

o liquid starts to leak through perforations (weeping)<br />

• excessive weeping will lead to dumping<br />

o the liquid on all trays will crash through to the base <strong>of</strong> the column<br />

(via a domino effect)<br />

o detected by sharp pressure drop and separation efficiency


weep point, the gas flowrate at which the first leakage <strong>of</strong> liquid starts because the<br />

gas flowing up through perforation is no longer able to counter balance the<br />

hydrostatic head <strong>of</strong> liquid on a tray.<br />

Pressure drop<br />

Total tray pressure drop, ΔPT, is made up <strong>of</strong>:<br />

• Dry tray pressure drop, ΔPdry<br />

o Determined by gas flowing through holes in tray<br />

• Pressure drop due to liquid hold up<br />

o Liquid depth on tray <strong>of</strong>fers additional resistance to gas flow<br />

The tray pressure drop is composed <strong>of</strong> at least two major contributions:<br />

1) a pressure drop by the gas flowing through the perforations<br />

a. Depends on gas flowrate, fractions <strong>of</strong> free area, pressure dr<strong>of</strong><br />

coefficients <strong>of</strong> particular perfations.<br />

b. Depends on relative hole thickness, hole shape nearness <strong>of</strong> other<br />

holes.<br />

2) a pressure drop caused by the liquid present on the tray. This liquid hold up<br />

effect primarily increases with an increase in outlet weir height, decreases<br />

with an increase in gas flowrate & increase in liquid flowrate.<br />

3) Depends on physical properties <strong>of</strong> gas/liquid system<br />

hT = hd + h<br />

hd =dry tray pressure drop<br />

h=gas through liquid<br />

Foaming: expansion <strong>of</strong> liquid due to passages <strong>of</strong> vapour or gas<br />

Height <strong>of</strong> liquid back-up in downcomer (hdc)<br />

Caused by:<br />

• Pressure drop over plate<br />

• Resistance to flow in downcomer<br />

Tray spacing, Ts, is a design parameter chosen to prevent liquid in the downcomer<br />

backing up to the tray above. For safe design avoiding downcomer flooding:<br />

hdc ≤ ½ Ts<br />

Most factors that affect column operation is due to vapour flows. Weeping<br />

determines the minimum vapour flow. Flooding determines the maximum<br />

vapour flow.


Tutorial Question<br />

Liquid flowrate, L=0.14 kmol/s<br />

Vapour flowrate, V=0.15 kmol/s<br />

Average molecular mass <strong>of</strong> liquid vapour =70kg/kmol<br />

Liquid density, ρL = 700kg/m 3<br />

Vapour density, ρV = 2.26kg/m 3<br />

Flooding= 80%<br />

Height <strong>of</strong> weir hw =50mm<br />

Ts=0.45m<br />

hap=38mm<br />

single pass cross flow from liquid arrangement graph<br />

DT = 2.45m<br />

Ψ< 0.1 è entrainment ok<br />

Weeping use weep point correlation, k2 vs (hw+how) chart<br />

• q=(0.14*70)/700<br />

• =0.014m 3 /s<br />

• Lw=0.77*DT=1.89<br />

how= 750 (q/Lw)^0.67<br />

• how= 750 (0.014/1.89)^0.67<br />

hw+how=50+28=78mm<br />

k2=30.7<br />

Uh min= [k2-0.9(25.4-dh)]/√(ρv)<br />

• Uh min= [30.7-0.9(25.4-4.76)]/√(2.26)<br />

• Uh min= 8.06m/s<br />

Uh actual=QV/Aholes=4.65/0.076AT=4.65/0.076*4.7= 13m/s<br />

Uh actual > Uh min<br />

èno weeping<br />

Pressure drop<br />

ΔΡtotal =ΔΡdry +ha<br />

• ha =ΔΡ due to aerated liquid on tray


ΔΡdry= 50.8 (ρV/ρL)(Uh/Cv0) 2<br />

• Cv0 =discharge coefficient, 0.76<br />

• ΔΡdry= 50.8 (2.26/700)(13/0.76) 2<br />

• =48mm <strong>of</strong> liquid=330N/m 2<br />

note ΔΡdry is m <strong>of</strong> liquid to get in N/m 2<br />

ΔΡdry =(mm <strong>of</strong> liquid) * ρL * g<br />

ha =Qp (hw + how)<br />

=0.6(78)<br />

=46.8m<br />

Qp : depends on how much froth is produced (high flowrate + low Active<br />

area )=low Qp<br />

ΔΡT = 48 + 46.8 =94.8<br />

= 651 N/m 2<br />

axis ion the graph Qp vs Fv=Q/Aa(√ρv)<br />

note : acceptable ΔΡT between 300-1200 N?m 2 per tray for atmospheric<br />

duty.<br />

Height <strong>of</strong> liquid back up in downcomer<br />

hdc= ΔΡT +(hw +how +Δ+ hda)<br />

Δ: liquid gradient difference in liquid level needed to drive liquid flow across plate. Δ<br />

is negligible for sieve tray, can be significant in vacuum operation.<br />

hda= loss under down comer apron<br />

=165 (q/Ada) 2<br />

Clearance area under downcomer apron<br />

Ada = hap * LW (m 2 ) =0.038 *1.89=0.072m 2


Typically hap=hw-(5 to 10mm)<br />

hda =165 (0.014/0.072) 2<br />

=6.24 mm <strong>of</strong> liquid<br />

hdc = 94.8 + 50 +28 +0 +6.24 =179mm <strong>of</strong> liquid<br />

check hdc ≤ ½ Ts<br />

Ts = 0.45m<br />

½Ts = 0.179m<br />

hdc < ½Ts è risk <strong>of</strong> flooding is low<br />

residence time<br />

tr = (Adc * hdc)/ qL<br />

=0.12*AT*0.179/ 0.014<br />

• =0.12*4.7*0.179/ 0.014=7.25 >3s minimum


07/03/2012 18:44


•<br />

07/03/2012 18:44

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