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Distillation

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

Physical Separation Processes


Distillation Absorption Stripping Extraction
(Fractionation)

 Distillation is the most common separation technique


 Distillation is energy intensive process
 It has large heating and cooling load
 It can contribute to 30-60% of plant operating costs

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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

Some Important Concepts of Fractionation


Cut or Fraction
 Fractionation is a term used for distillation of multi-component
system. Each component has a boiling point.
 Q - What is the boiling point of a mixture of two liquids A and B
mixed 50-50, A and B having a boiling points of 70 and 80 0C?

Q - What is the boiling point of a mixture of four liquids in equal parts


having a boiling points of 100,200,300 and 400 0C?
In oil and gas processing sharp separation of a product of high purity is
not so common. Example – LPG is not a pure component.

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Distillation – Basic Theory

Boiling Point Curve of a Mixture


 The equilibrium
compositions of the
components in a liquid
mixture vary with
temperature at a fixed
pressure.
 When a liquid with mole
fraction of A=0.4 (point A) is
heated, its concentration
remains constant until it
reaches the bubble-point
(point B). It starts to boil.
The vapours evolved during
the boiling has the
equilibrium composition
given by point C.`
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Distillation – Basic Theory

Vapour Liquid Equilibrium Curve of a Binary Mixture


Constant Pressure VLE Data from Boiling Point Diagrams give
VLE Diagram

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Distillation – Basic Theory

Relative Volatility of component 1


and 2 in a mixture is given by-

Relative Volatility = [y1/x1] /


[y2/x2]

Where-

y is the composition in vapor phase


and x is the component in liquid
phase at a particular pressure and
temperature.

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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

Distillation Process, contd..


A typical distillation contains
several major components:
 A reboiler to provide the
necessary heat of
vaporization for the Trays
distillation process. Trays
 A condenser to cool and COLUMN
condense the vapor leaving COLUMN
the top of the column.
 A reflux drum to hold the
condensed vapor from the
top of the column so that
HEAT
HEATIN
HEAT IN
IN
liquid (reflux) can be
recycled back to the column
to enhance close separation.

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Distillation – Basic Theory

Heat Exchangers (Cooler, Reboiler)

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Distillation – Basic Theory

Basic Operation and Terminology

 The feed is introduced


usually somewhere
near the middle of the
column to a tray Trays
known as the feed
COLUMN
tray.
 The feed tray divides
the column into a top
(enriching or
rectification) section
and a bottom HEAT IN
(stripping) section.

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Distillation – Basic Theory

Basic Operation and Terminology, contd..


 The liquid (from feed
and condensing vapors
on the rectification
section) feed flows
down the column.
 Heat is supplied to the Trays
re-boiler to generate COLUMN
vapor.
 The liquid removed
from the reboiler is
known as the bottoms
product or simply,
bottoms. HEAT IN

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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

Conventional Expander Process

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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

Limits of Normal Operation

39
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

Tray Column Internals


Chimney Tray

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

Hold Down Plate

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Column Internals

Redistributor

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Column Data Sheet Preparation

Codes & Standards


 Use ASME Sec VIII Div. I for column.
 Use Company standards for nozzle sizing,
insulation, some of the internals, design
pressure and design temperature.

50
Column Data Sheet Preparation
Data Sheet for Column (Quanta’s)

51
Column Data Sheet Preparation

Data Sheet for Column (Quanta’s)

52
Column Data Sheet Preparation

Data Sheet for Internals (Quanta’s)

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Column Data Sheet Preparation

Data Sheet for Internals (Quanta’s)

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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

Pressure Control, contd..


 Energy methods regulate the heat flow into and out of
the tower.
 Increasing the heat load in the reboiler will result in
increased pressure of the column.
 Excessive heating load at the reboiler can generate over-
pressure and popping of safety valve.
 Some pressure control methods are shown in the next
slide.

56
Distillation Control
Column Pressure Control
PC

PC

M
M

Method 2: Vary condensing area.


Method 1: Direct control of Process: Can operate at zero
vapor product rate Method: Vary net vapor product rate. Should not be used in
vapor rate, no make-up gas. systems with large
Process: Must always have quantities of non- condensable gas.
vapor product. Advantages: Condenser may be
Advantages: Simple and direct. mounted below condensate drum.
Disadvantages: Generally none. Disadvantages: Concept is not
Response may be slow when vapor rate straightforward.
is low

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Distillation Control

Distillation Controls Varying Condenser Area

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Distillation Control
Varying Condenser Area

59
Distillation Control
Column & Reflux Drum at Different Pressure

60
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

Temperature Control, contd..


 The temperature depends on the heat balance achieved
between the following:
 Heat entering with the feed.
 Heat going out with the products.
 Heat going out at the top condenser.
 Condenser duty depends on Reflux ratio (Cooling and
condensing of top vapors takes out the heat)
 Reboiler heat input.
 Since the product have to go out at a temperature
consistent with its composition at the column operating
pressure, the control is achieved through the other three
variables.
63
Distillation Control

Temperature Control in a Binary Distillation Column


 The example is taken from Simcon training module SPM-700
Distillation Column.
 The control system is configured to separate a binary mixture of
any two of the paraffins C1 through C8 (methane, ethane, propane,
butane, pentane, hexane, heptane, and octane respectively).
 The default configuration is for hexane (C6) and heptane (C7). The
distillation column (C-301) feed is pumped (P-101/2) through a
preheater (E-101) where its temperature is raised to the optimum
temperature of the feed tray.
 The distillation column (C-301) is heated with a thermosyphon type
reboiler (E-401). The bottoms product is pumped (P-501/2) out of
the distillation column (C-301) to a product storage facility.
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Distillation Control

Temperature Control in a Binary Distillation Column


 (The distillation column (C-301) vapors are condensed in
an overhead condenser (E-601) and enter a reflux drum
(D-701) where the liquid is accumulated.
 The uncondensed vapors can be vented through a vent
line.
 Reflux pumps (P-801/2) draw liquid from the bottom of
the reflux drum (D-701) and pump part of the liquid
back (reflux) to the distillation column (C-301). The
balance of the liquid is sent to a product storage facility.

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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

P-101/2 FEED TO COLUMN


TI-101
HB-102 TI-202
HV-102

FEED SUPPLY HV-202 HV-201

For fee stream, flow rate (capacity) and temperature are controlled
66
Distillation Control
Temperature Control in a Binary Distillation Column, contd.

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Distillation Control
Temperature Control in a Binary Distillation Column, contd.

68
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

Output Summary – Short-cut Distillation

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Calculated Example

Reflux Ratio Vs Theoretical Stages

76
Calculated Example

Output Summary – Rigorous Model

77
Calculated Example

Stream Composition

78
Calculated Example

Stream Properties

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Calculated Example

Temperature – Pressure-Flow Profile

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Calculated Example

Temperature – Pressure-Flow Profile, contd..

81
Calculated Example

Liquid Properties at Trays

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Calculated Example

Composition of Trays

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