Operating Problems With Trays

Coning

❑Occurs at low liquid flowrates.

❑Vapor forces the liquid back from the slots,
and passes as a continuous stream through
holes.
❑Mixing of liquid and vapor on the tray is
severely affected.
 Pulsation, Dumping & Weeping
❑ Occur at low vapor flowrates.
❑ If the liquid flowrate is low, the vapor passes through the
slots intermittently, resulting in pulsation.
❑ If the liquid flowrate is high, slots start to dump liquid to
lower trays rather than allowing vapor to pass above. This is
called dumping.
❑ Both pulsating and dumping are collectively called weeping.
❑ On excessive weeping, liquid from all trays crashes to the
bottom of the column via a domino effect, and the column
has to be re‐started.
❑ Weeping is detected by a sharp pressure drop in the
column.
 Entrainment or Blowing

❑Occurs at very high vapor flowrates.

❑The vapor bubbles carry liquid droplets with
them as a spray or droplets to the plate above.
❑It contaminates the higher‐purity liquid of
above plate with the lower‐purity liquid of
plate below.
 Flooding
❑Occur at very high vapor flowrates and high liquid
flowrates.
❑If the vapor flowrate is high and the liquid
flowrate is gradually increased, a point is reached
where the pressure drop on the tray is equal to
the head of the liquid in the downcomer.
❑Beyond this point, liquid builds up in the
downcomer and starts to flood the trays.
❑Results in a marked decrease in capacity of the
column and separation efficiency, and a sudden
rise in column differential pressure.
Feed Conditions
Downcomer Layout
Reboiler Arrangements
Condenser Layouts
 Disturbances

The type and magnitude of disturbances

affecting a distillation column have a direct
effect on the resulting product variability.
 Feed composition upsets
❑Changes in the feed composition represent the
most significant upsets with which a distillation
control system must deal on a continuous basis.
❑A feed composition change shifts the
composition profile through the column resulting
in a large upset in the product compositions.
❑Most industrial columns do not have a feed
composition analyser; therefore, feed
composition upsets usually appear as
unmeasured disturbances.
 Feed Cases
Two dilute feed cases;
❑ More Volatile ( Methanol - water)
❑ Less Volatile (acetic acid – water)
 Feed flow rate upsets
❑The flow rates in a steady-state model of a
column with constant tray efficiencies scale
directly with column feed rate.
❑Dynamic compensation is normally required
to account for the dynamic mismatch between
the response of the product compositions to
feed flow rate changes and the response to
changes in the MVs.
 Feed enthalpy upsets
❑ For columns that use a low reflux ratio, feed enthalpy
changes can significantly alter the vapor/liquid rates inside
the column, causing a major shift in the internal
composition profile and, therefore, a significant upset in
the product compositions.
❑ This upset can be difficult to identify because (1) most
industrial columns do not have feed temperature
measurements and (2) even if a feed temperature
measurement is available, it does not detect feed enthalpy
changes for a two-phase feed.
❑ It may be necessary to install a feed preheater or cooler to
maintain a constant feed enthalpy to a column.
 Subcooled reflux changes
❑ When a thundershower passes over a plant, the reflux
temperatures for the columns can drop sharply.
❑ Columns that use finned-fan coolers as overhead
condensers are particularly susceptible to rapid
changes in ambient conditions.
❑ If internal reflux control is not applied, severe upsets in
the operation of the columns result because of major
shifts in the composition profiles of the columns.
❑ When internal reflux control is correctly applied, the
impact of a thunderstorm on column operations can be
effectively eliminated.
 Loss of reboiler steam pressure
❑ When a steep drop in steam header pressure occurs,
certain columns experience a sharp drop in reboiler
duty.
❑ This results in a sharp increase in the impurity levels in
the products.
❑ This disturbance is, in general, the most severe
disturbance that a control system on a distillation
column must handle and may require invoking
overrides that gradually bring the operation of the
column to its normal operating window instead of
expecting the composition controllers to handle this
severe upset by themselves.
 Column pressure upsets
❑Column pressure has a direct effect on the
relative volatility of the key components in the
column.
❑Thus, changes in the column pressure can
significantly affect product compositions.
 Intangible Factors
❑Product Purity 99% or 99.9999%
❑ Heat Sensitivity or Polymerization Capability
❑ Corrosively or Reactivity
Column Hydraulics
 Plate Hydraulic Design
• 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 acceptable
limits.
• Have sufficient down comer area for the liquid
to flow freely
 Design Procedure
1. Calculate the maximum and minimum vapour and
liquid flow- rates, for the down ratio required.
2. Collect, or estimate, the system physical properties.
3. Select a trial plate spacing.
4. Estimate the column diameter, based on flooding
considerations.
5. Decide the liquid flow arrangement.
6. Make a trial plate layout: down comer area, active
area, hole
• area, hole size, weir height.
7. Check the weeping rate if unsatisfactory
8. Check the plate pressure drop, if too high return
9. Check down comer back-up, if too high return to step 6 or
3.
10. Decide plate layout details: calming zones, unperforated
areas. Check hole
• pitch, if unsatisfactory return to step 6.
11. Recalculate the percentage flooding based on chosen
column diameter.
12. Check entrainment, if too high return to step 4.
13. Optimise design: repeat steps 3 to12 to find smallest
diameter acceptable (lowest cost).
14. Finalise design: draw up the plate specification.
 Diameter

where uf = flooding vapor velocity, m/s, based on the net column

cross- sectional area An (see Section 11.13.2)
K1 = a constant obtained from Figure
Liquid-flow arrangement
Entrainment
Weep Point
Weir Liquid Crest
Hole Size and Hole Pitch
 Hydraulic gradient

The hydraulic gradient is the difference in liquid

level needed to drive the liquid flow across the
plate.
 Plate Pressure Drop

Dry Plate Drop

 Pressure Drop
Residual head

Total Drop
 Packed-column design procedures
The design of a packed column will involve the
following steps:
1. Select the type and size of packing.
2. Determine the column height required for the
specified separation.
3. Determine the column diameter (capacity), to
handle the liquid and vapor flow rates.
4. Select and design the column internal features:
packing support, liquid distributor, redistributors.
 Types of Packing
They can be divided into two broad classes:

• Packings with a regular geometry: such as

stacked rings,
• grids and proprietary structured packings.
• Random packings: rings, saddles and
proprietary shapes, which are dumped into
the column and take up a random
arrangement.
Random Packings
Recommended size ranges:
 Structured Packings
They are being increasingly used in
the following applications:

• For difficult separations, requiring

many stages: such as the
separation of isotopes.
• High vacuum distillation.
• For column revamps: To increase
capacity and reduce reflux ratio
requirements
 Choice of plate or packing
• Plate columns can be designed to handle a wider range of liquid and gas flow-rates than
packed columns.
• Packed columns are not suitable for very low liquid rates.
• The efficiency of a plate can be predicted with more certainty than the equivalent term for
packing (HETP or HTU).
• Plate columns can be designed with more assurance than packed columns.

• It is easier to make provision for cooling in a plate column; coils can be installed on the
plates.
• For corrosive liquids a packed column will usually be cheaper than the equivalent plate
column.
• The liquid hold-up is appreciably lower in a packed column than a plate column.
• Packed columns are more suitable for handling foaming systems.
• Packing should always be considered for small diameter columns, say less than 0.6 m, where
plates would be difficult to install, and expensive.
 RESIDUE CURVE MAPS
AND
DISTILLATION BOUNDARY
REGION DIAGRAMS
 RESIDUE CURVE MAPS
❑ The simplest form of distillation involves boiling a
multicomponent liquid mixture batchwise in a single-stage
still pot.
❑ At any instant in time the vapor being generated and
removed from the pot is assumed to be in equilibrium with
the remaining liquid (assumed to be perfectly mixed) in the
still.
❑ Because the vapor is richer in the more volatile
components than the liquid, the composition and
temperature of the liquid remaining in the still changes
continuously over time and moves progressively toward
less volatile compositions and higher temperatures until
the last drop is vaporized.
 RESIDUE CURVE MAPS
❑ A residue curve is a tracing of this change in perfectly mixed
liquid composition for simple single-stage batch distillation
with respect to time.
❑ Arrows are sometimes added, pointing in the direction of
increasing time, increasing temperature, and decreasing
volatility.
❑ Because simple, batch distillation can be described
mathematically by
dxi /dξ = xi − yi for all i = 1, . . . N
where ξ is a nonlinear time scale
 RESIDUE CURVE MAPS
❑A residue curve map (RCM) is generated by varying
the initial composition and extrapolating Equation.
❑Residue curve maps can be constructed for mixtures
of any number of components, but can be pictured
graphically only for up to four components.
❑The simplest form of ternary RCM, as exemplified for
the ideal normal-paraffin system of pentane-hexane-
heptane, is illustrated in Fig., using a right-triangle
diagram.
Nonazeotropic pentane-hexane-
heptane System
 RESIDUE CURVE MAPS
❑Each of the infinite number of possible residue curves
originates at the pentane vertex, travels toward and
then away from the hexane vertex, and terminates at
the heptane vertex.
❑The family of all residue curves that originate at one
composition and terminate at another composition
defines a region.
 RESIDUE CURVE MAPS
❑ Systems that do not involve azeotropes have only one
region—the entire composition space.
❑ However, for many systems, not all residue curves
originate or terminate at the same two compositions.
Such systems will have more that one region.
❑ The demarcation between regions in which adjacent
residue curves originate from different compositions or
terminate at different compositions is called a
separatrix.
❑ Separatrices are related to the existence of azeotropes.
RESIDUE CURVE MAPS
 APPLICATIONS OF RCM AND DRD
❑Residue curve maps and distillation region
diagrams are very powerful tools for
understanding all types of batch and
continuous distillation operations, particularly
when combined with other information such
as liquid-liquid binodal curves.
 APPLICATIONS OF RCM AND DRD
System visualization: Location of distillation
boundaries, azeotropes, distillation regions, feasible
products, and liquid-liquid regions.
Evaluation of laboratory data: Location and
confirmation of saddle ternary azeotropes and a
check of thermodynamic consistency of data.
Process synthesis: Concept development,
construction of flowsheets for new processes, and
redesign or modification of existing process
flowsheets.
 APPLICATIONS OF RCM AND DRD
Process modeling: Identification of infeasible or
problematic column specifications that could
cause simulation convergence difficulties or
failure, and determination of initial estimates of
column parameters including feed-stage
location, number of stages in the stripping and
enriching sections, reflux ratio, and product
compositions.
 APPLICATIONS OF RCM AND DRD
Control analysis/design: Analysis of column
balances and profiles to aid in control system
design and operation.
Process trouble shooting: Analysis of separation
system operation and malfunction, examination
of composition profiles, and tracking of trace
impurities with implications for corrosion and
process specifications.