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Programme Contents
Distillation – Basic Theory
Packed Vs Tray Column and Tray Types
Column Calculation Methods
Column Internals
Column Data Sheet preparation
Distillation Control
Calculated Example
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Distillation – Basic Theory
Simple Rules of Vapor Liquid Equilibrium
Vapor pressure of liquid depends on temperature.
Heat input raises vapor pressure of liquid.
A liquid boils when its vapor pressure equals the
system pressure.
Higher the vapor pressure lower the boiling point.
Volatile liquids have high vapor pressure.
The vapor pressure and hence the boiling point of a
liquid mixture depends on the relative amounts of the
components in the mixture
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Distillation – Basic Theory
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Distillation – Basic Theory
Physical Separation Processes, contd..
Fractionation is a unit that has both a reboiler to supply heat at the
bottom and a condenser to take heat out from the top. This is
normally called distillation.
Absorption is a unit that has no method at the top of the tower to
take heat out. An external liquid is supplied from outside the
system to absorb material from the vapor.
Stripping is a unit that has an external stream (gas or steam)
supplied from outside the system to strip light material from the
liquid. It may have a reboiler at the bottom of the tower to put heat
in.
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Distillation – Basic Theory
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Distillation – Basic Theory
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Distillation – Basic Theory
Where-
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Distillation – Basic Theory
Fractionation System
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Distillation – Basic Theory
Fractionation Column
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Distillation – Basic Theory
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Distillation – Basic Theory
Fractionation Column
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Distillation – Basic Theory
Trays
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Distillation – Basic Theory
Packings
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Distillation – Basic Theory
Distillation Process
Description
Distillation columns carry out physical
separation of liquid chemical components
from a mixture by
a combination of transfer of heat energy (to
vaporize lighter components)
mass transfer between the liquid and vapor
phases.
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Distillation – Basic Theory
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Distillation – Basic Theory
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Distillation – Basic Theory
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Distillation – Basic Theory
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Distillation – Basic Theory
Basic Operation and Terminology, contd..
The vapor moves up the column, and as it exits the top
of the unit, it is cooled by a condenser.
The condensed liquid is collected in a vessel known as
the reflux drum. Some of this liquid is recycled back to
the top of the column and this is called the reflux.
Part of the condensed liquid is removed from the reflux
drum (or from one of the trays) system is known as the
distillate or top product.
Thus the distillate and the bottoms become the final
products. For multi-component distillation.
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Distillation – Basic Theory
Basic Operation and Terminology, contd..
Certain products can be drawn from one of the
trays and is called side draw off.
Each tray attains a “equilibrium temperature”. A
temperature profile takes place along the
distillation column, the highest being at the
bottom and the lowest being at the top.
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Distillation – Basic Theory
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Packed Vs Tray Column and Tray
Types
Packed Column Vs Tray Column
Packed Column Tray Column
Low pressure drop High pressure Drop
Good for vacuum service Not recommended for high vacuum
service
Less flexibility for side draw Flexible for side draw
Good for corrosive service Expensive for corrosive service
Ideal for small diameter Expensive for small diameter
Not preferred for high pressure Good at high pressure
Not used for Residence time Good when high Residence time
limitations required
Usually avoided for low Good for low liquid loading
Liquid loading
Can handle very large liquid Cannot handle very large liquid
load load
Requires smaller diameter Requires larger diameter column
column
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Packed Vs Tray Column and
Tray Types
Various types of trays are used in the Industry. The following are
commonly used:
Valves Trays or improved valve trays
Sieve Trays
Bubble cap trays
Baffle Trays
Valve trays are widely used and offer the following advantages
over other types:
Offer better efficiency at varying gas load
Cost is lower
Works better at lower vapour loading
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Packed Vs Tray Column and
Tray Types
Sieve trays are used often and are selected for fouling
service. They are one of the cheapest trays.
Bubble cap trays are most expensive and were used
widely, but lately use has diminished. It provides
positive sealing against weeping.
Baffle trays are the least efficient and are used only in
high fouling service
For small diameter column, cartridge trays are specified.
Multi-pass trays are used for large diameter columns
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Packed Vs Tray Column and
Tray Types
Packing
Packing were often used in the early years of development of
process industry and lately they are again gaining popularity
Random or structure pickings are used. Popular random packings
are pall rings, IMTP, CMR, rasching ring etc. Structure packings are
more proprietary. The most popular are corrugated plates.
Random packings are widely used compared to Structure packing
They are evaluated based on surface area per unit volume. Higher
the value, better the packing.
The design of distributors and redistributors is very critical for
satisfactory performance of the packing
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Distillation Calculation
Methods
Stream Specifications
Feed Specifications (Temp, Pressure and
Composition)
Variation in feed specifications
Top product specifications
Bottom product specifications
Side draw specifications
Provide design margin while making calculation
Estimate the recovery required
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Distillation Calculation
Methods
Thermodynamic Method
The selection of thermodynamic method is one of the
most critical decision a process engineer makes in
design. General guidelines are given in the software.
However, this is not adequate. Process engineer must
develop skill in selecting thermodynamics method. The
following may be used as a guideline:
Use S-R-K or P-R methods for most hydrocarbon service. The
improved methods also may be used. Both the methods are good
for high pressure also.
The software may have interaction parameters for methods like
Wilson, NRTL, Margules, etc. You may use this for non-ideal
services.
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Distillation Calculation
Methods
Thermodynamic Method, contd..
If experimental x-y data are available at one or more
conditions, the data can be regressed using the most
suitable thermodynamic model.
For vacuum services, vapour pressure (ideal) model
can be considered in absence of other data.
Use special methods for the given application such as
Amines or Sour Water etc.
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Distillation Calculation
Methods
Estimate using Short-cut methods
The operating pressure for column is to be decided. In
general lower the operating pressure, easier the
separation. However, lower the pressure, larger the
column size. Select optimum pressure based on
expected temperature, utilities available, product
degradation, refrigeration requirement etc.
Initial estimate on pressure drop may be done based on
70 mmwc for pressure drop in each tray and 40 mmwc
per meter of packed height for random packing.
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Distillation Calculation
Methods
Estimate using Short-cut methods, contd..
Based on the given feed and product specifications,
estimated recovery and K-model selection, use short-cut
methods to calculate the following:
Minimum Reflux Ratio
Minimum number of theoretical trays
Reflux ratio Vs No. of trays
Ideal Feed Location
Expected temperature and duty.
Based on short-cut method, select the number of trays required,
reflux ratio and feed tray location. This is the first estimate for
rigorous method
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Distillation Calculation
Methods
Rigorous Calculation Method
Select the column operating pressure at the top
Specify pressure drop for the condenser, may be 0.05 to 0.3
Kg/cm2, depending on service.
Select number of theoretical trays and define feed location based on
results of short cut method.
Specify minimum specification as per programme requirements.
This include reflux ratio and reflux rate, product purity, reboiler
duty, top temperature, bottom temperature etc.
For fast conversion of column, specify product rate, reflux rate,
reboiler duty etc.
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Distillation Calculation
Methods
Rigorous Calculation Method, contd..
Specify estimated quantities of other parameters, if known.
Develop one precise calculation.
Fine tune (optimize) on reflux ratio and feed-tray location.
The number of trays selected from short-cut method may not be
optimum. Therefore, develop few cases with different number of
trays.
Based on all these cases, select the case which seems to be the
optimum.
The theoretical number of trays can be converted to actual number
of trays based on tray efficiency or can be converted to equivalent
packed height based on HETP value.
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Distillation Calculation
Methods
Tray Efficiency
Tray efficiency vary from 30% to 100%, but most
hydrocarbon service, it is in the range of 60% to 80%.
Various co-relations are cited in literature for calculating
efficiency. However, they are not very reliable.
In-house data bank, tray vendor information and
published experimental information is more reliable for
tray efficiency.
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Distillation Calculation
Methods
HETP
HETP (Height Equivalent to a Theoretical Plate) values are used for
calculating total packed height from the number of trays calculated using
simulator.
HETP value is calculated based on experience and vendor information.
While calculating the HETP, the liquid distribution for each bed plays a
major role.
The typical value of HETP for most random packing is 300 mm to 800 mm.
The corresponding value for structural packing is some what lower. Smaller
the packing, lower the HETP value
The total packed height is divided into number of beds. Each bed may
have height equivalent to 6 to 15 theoretical trays for random packing.
H/D Ratio for a random packed bed is limited to 8. Often bed height is
restricted to 6 m. Higher packed height per bed is permitted for structure
packing.
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Distillation Calculation
Methods
Column Diameter and Height Calculation
Tray Column
Calculate total number of trays required
Calculate column diameter based on vapour and
liquid flow rates. Preliminary calculations can be
done using simulator. Tray vendor will give accurate
data. Tray diameter calculation depends on tray
spacing. Therefore, some optimization calculation
may be required.
Tray spacing varies from 250 mm to 750 mm. Most
hydrocarbon services use tray spacing of 450 mm to
600 mm. 37
Distillation Calculation
Methods
Column Diameter and Height Calculation
Provide space of about 800 mm to 1000 mm at the top
of 1st tray for man-way.
Provide liquid level at column bottom based on
residence time required. Note that liquid disappears
due to bottom product removal and due to
vaporization.
Provide adequate space between HHLL and the last
tray for proper separation of vapour and liquid.
Column hydraulics shall be such that normal
operation is away from entrainment, flooding,
choking etc. 38
Distillation Calculation Methods
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Distillation Calculation
Methods
Packed Column
Calculate HETP as described above. This includes selecting size of
the packing. Larger the packing, smaller the diameter, but higher the
HETP value.
Calculate total packed height above and below the feed location.
Divide the total packed height into number of beds such that each
bed has about 10 theoretical stages.
Calculate column diameter using simulator based on hydraulics data
and packing selected. Specify pressure drop in the range of 25
mmwc to 40 mmwc per meter of packed height. This is finalized
after discussion with packing vendor.
Calculate overall column dimensions as described for tray column.
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Distillation Calculation Methods
Packed Column Pressure-drop Calculation Chart
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Column Internals
Internals
Tray Column
Trays
Chimney Tray
Feed Pipes
Gas Distributor
Partition Plate
Packed Column
Packing
Distributor / Redistributor
Support Plate
Hold drum plate / bed limitors
Feed Pipe
Gas Distributor
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Column Internals
Chimney Trays are used for withdrawing side stream and collecting
liquid when the column uses trays as well as packing
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Column Internals
Feed Pipe
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Column Internals
Gas Distributor
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Column Internals
Partition Plate
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Column Internals
Support Plate
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Column Internals
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Column Internals
Redistributor
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Column Data Sheet Preparation
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Column Data Sheet Preparation
Data Sheet for Column (Quanta’s)
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Column Data Sheet Preparation
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Column Data Sheet Preparation
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Column Data Sheet Preparation
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Distillation Control
Pressure Control
For steady operation to meet the required performance it
is essential to have a steady pressure of column
operation.
Depending on the type of column and fraction of
condensation of the top vapors, (100% condensation to
minimal Condensation), there are several methods for
pressure control.
Distillation pressure control uses either mass or energy
balances around the unit.
Mass balance methods control pressure by regulating the
amount of flow into or out of the tower.
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Distillation Control
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Distillation Control
Column Pressure Control
PC
PC
M
M
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Distillation Control
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Distillation Control
Varying Condenser Area
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Distillation Control
Column & Reflux Drum at Different Pressure
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Distillation Control
Using Non-Condensible gas
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Distillation Control
Temperature Control
The column must operate at a fixed pressure, which is
the optimum pressure for the separation of the products,
meeting specifications.
In vapor liquid equilibrium phenomena like distillation,
there are three variables of thermodynamic equilibrium
relationship i.e. temperature , pressure and composition.
If any two are fixed, the third is automatically set at its
unique thermodynamic value.
Once the column pressure is fixed, it is necessary to
control the temperatures in the column to get the right
product specification.
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Distillation Control
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Distillation Control
Temperature Control in a Binary Distillation Column, contd.
Feed System FI-201
TI-201
TIC-102
AI-101 HB-101 FIC-101
HV-101
E-101
For fee stream, flow rate (capacity) and temperature are controlled
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Distillation Control
Temperature Control in a Binary Distillation Column, contd.
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Distillation Control
Temperature Control in a Binary Distillation Column, contd.
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Distillation Control
Temperature Control in a Binary Distillation Column, contd.
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Calculated Example
Problem
Consider separation of C2/C3 from a mixture of C2/C3/C4
Feed Pressure = 35 Kg/cm2g
Feed Temperature = 20oC
Feed Composition
C2 63.30 mole %
C3 24.70
1C4 4.75
NC4 7.25
Top Product 99.8 mole % C2/C3
Bottom product 2.0 mole % max. C2/C3
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Calculated Example
Calculation
Based on critical pressure and condensing temperature, select the
column top pressure. The column pressure of 25.0 Kg/cm2g require
condensing temperature of 16oC.
For this condition, short-cut distillation calculation were made with
C3 as key component
Used P-R thermodynamic method.
Calculated minimum number of trays = 18
Calculated minimum reflux ratio = 0.78
For reflux ratio 1.2, the number of trays = 34. Ideal feed location =
17.
Reflux Ratio Vs No. of trays
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Calculated Example
Calculation, contd..
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Calculated Example
Rigorous Calculation
Specified column top pressure = 25 kg/cm2,
condenser pressure drop = nil and column
pressure drop = 0.2 Kg/cm2
Specified number of ideal trays = 34.
Feed tray location = 17.
Two conditions specified for calculation
Reflux ratio = 1.2
C3 in bottom product = 2.0 mole %
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Calculated Example
Output Data
Stream summary for feed and product
Stream properties
Tray temperature, pressure and flow profile
Liquid-Vapour properties at each tray
Tray-to-tray vapour and liquid composition
Reboiler and condenser duty
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Calculated Example
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Calculated Example
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Calculated Example
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Calculated Example
Stream Composition
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Calculated Example
Stream Properties
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Calculated Example
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Calculated Example
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Calculated Example
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Calculated Example
Composition of Trays
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