Unit no: 4

Instrumentation for distillation

columns

Instrumentation for distillation columns:

A: Operation of distillation column, manipulated and controlled
variables in distillation column control, instrumentation for flow
control of distillate, top and bottom composition control, reflux
ratio control pressure control schemes.
B: Material and energy balance of distillation column
(BOOK: LIPTAK II Process control )
Liptak - Distillation control and optimization.
k krishnaswamy ( Process control)

Contents:
Contents:
Introduction
What is a Distillation process
Examples
Flow sheet symbols
Types of Distillation column
Distillation equipment and operation
Distillation control
C-M Pairing of distillation

Composition control (Product quality control)

Inferring composition from Temperature (Inferential control)
Column pressure control

Introduction:
Distillation is a method of separating mixture of two or
more miscible liquids into their pure components
Separation of components from a liquid mixture through
distillation depends on the difference in boiling points of
individual components, also depending on concentration
of components present,
There for distillation process depends on vapor pressure
characterizes of liquid mixture.

Introduction:
Why do we need to separate different componets of a
mixture .Give two examples ?
Remove the unwanted impurities.
Remove the substance that are harmful for our health.
Obtain pure substances.
Separate two different , but useful componets.
Examples:
Grain is separated from stalks ,while harvesting
We filter tea leaves after preparing it.
Milk or curd is churned to separate the butter.

Introduction:

Flow sheet symbols of Distillation column:

TYPES OF DISTILLATION COLUMNS: Based on operation

1) Batch and.
2) Continuous columns.
Batch Columns:
In batch operation, the feed to the column is introduced
batch-wise. that is, the column is charged with a 'batch'
and then the distillation process is carried out. When the
desired task is achieved, a next batch of feed is
introduced.
Continuous columns:
In contrast, continuous columns process a continuous
feed stream. No interruptions occur unless there is a
problem with the column or surrounding process units.
They are capable of handling high throughputs and are
the most common of the two types. We shall concentrate
only on this class of columns.

Types of continuous column:

Continuous columns can be further classified according
to:
1) The nature of the feed that they are processing:
Binary column - feed contains only two components.
Multi-component column - feed contains more than two
components.
2)The number of product streams they have:
Multi-product column - column has more than two
product streams

Types of continuous column:

Where the extra feed exits when it is used to help
with the separation:
Extractive distillation - Where the extra feed
appears in the bottom product stream.
Azeotropic distillation - Where the extra feed
appears at the top product stream.

Types of continuous column:

The type of column internals:
Tray column - where trays of various designs are
used to hold up the liquid to provide better contact
between vapour and liquid, hence better separation.

Packed column - where instead of trays Packings'

are used to enhance contact between vapour and
liquid

Basic distillation equipment and operation:

Basic distillation equipment and operation:

Types of continuous column:

Main componets of distillation column:

Vertical shell: where the separation of liquid

components is carried out.

Column: Column internals such as trays/plates which

are used to enhance components separation.

Reboiler: Reboiler is a special type of heat

exchanger used to provide heat necessary for
distillation.

Condenser: The overhead vapor leaving the column

is sent to a cooler or condensers and is collected in
a Accumulator.

Reflux: A reflux drum to hold the condensed vapor so

that the liquid reflux can be recycled.

Types of continuous column:

Basic operation:
Heat is supplied to the reboiler to generate vapour. The
source of heat input can be any suitable fluid, although in
most chemical plants this is normally steam. In refineries, the
heating source may be the output streams of other
columns. The vapour raised in the reboiler is re-introduced
into the unit at the bottom of the column. The liquid removed
from the reboiler is known as the bottoms product or
simply, bottoms.

Basic operation:
The vapour moves up the column, and as it exits the top of
the unit, it is cooled by a condenser. The condensed liquid is
stored in a holding 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. The condensed liquid that is removed
from the system is known as the distillate or top product.

Types of continuous column:

Thus, there are internal flows of vapour and liquid within the
column as well as external flows of feeds and product
streams, into and out of the column.

Binary distillation:

Binary distillation:

Distillation controls:
Why Distillation control ?
1) Product composition should be constant.
2) To increase throughput.
3) Enhancing the column stability.
4) Safety of men and machineries.
The 3 main objectives of column control can be stated as:
1) To set stable conditions for column operation.
2) To regulate conditions in the column so that the
product(s) always meet the required specifications.
3) To achieve the above objective most efficiently,
e.g. by maximizing product yield, minimising energy
consumption, etc.

Evaluation of control strategies:

Controlled variables

Manipulated variable:

i) Overhead composition

i) Reflux flow rate.

ii) Bottoms composition

ii) Reboiler heating

medium

flow rate.

iii)Accumulator level

iii) Distillate flow rate.

iv)Bottoms level

iv) Bottom flow rate.

v)Column pressure

v) Condenser flow
rate/vapour bypass rate.

Paring can follow three general control structures:

Energy balance control:

Reflux and reboiler heatant flow to control composition
thus fixing the energy inputs
Material balance control:
uses the distillate and bottom product flows to control
composition ,thus fixing the overall material balance

Composition Measurement:
The direct measurement of composition is more
expensive, but also more accurate and versatile than is
indirect temperature measurement. Intermittent
analyzers, such as chromatographs (with cycle times of
a few minutes), are often provided with dead time
compensation for closed-loop control. The analyzer
update time must always be less than the response time
of the process. For improved accuracy, one usually
measures the impurity concentration in the controlled
stream. This way the upsets caused by feed composition
changes, tower pressure or efficiency variations can be
more accurately corrected.

Composition control:
A) Control with On-line Analyzer.
- high investment and maintenance costs.
- large measurement delay.

B) Tray Temperature Control.

Limited control performance
C) Inferential Control.

Product quality (composition) is estimated from

measured process variables, and the estimate is
used for control.

Control with On-line Analyzer.

Feedback control:

Feed forward control:

Inferential control: Temperature measurement

1.Uses easily measure process variables (T, P, F) to
inferential method more difficult to measure quantities
such as compositions and molecular weight.
2. Can substantially reduce analyzer delay.

3 . Can be much less expensive in terms of capital and

operating costs.
4.Can provide measurements that are not available any
other way.

Tray Temperature Control:

Inferential control: Temperature measurement

Inferential control: Temperature measurement

If the feed composition and column pressure are
constant, temperature can be used as indirect measure
of composition.
When the bottom product composition is controlled, the
temperature sensor is located in the lower half of the
column, and when overhead composition is controlled,
in the upper half.

Inferential control: Temperature measurement

The temperature sensor should be located on a tray that
strongly reflects changes in composition. This means
a 1% change in the manipulated variable (reflux or steam
flows in Figure 5, p. 10) should result in a temperature
change of at least 0.1 C to 0.5 C, and that this change should
be symmetrical, meaning that a 1% drop or rise in
these flows should result in approximately the same size of
drop or rise in the temperature on the control tray.

When two compounds of relatively close vapor pressures are

to be separated (for example normal butane from isobutene),
temperature measurement is not sensitive enough to measure
composition. In such cases, two temperatures or a
temperature difference (say, between Trays 5 and 15) can be
used instead of a single sensor. This configuration can also
be used to eliminate the effects of column pressure variations

Top composition control:

Bottom composition control:

Column pressure control:

In controlling the pressure of a column, the key
pieces of equipment are the condenser and the
accumulator.
First the overhead vapors enter the condenser
(partial or total).
If the condensation is incomplete, the condenser is
called a partial condenser, and the overhead product is
withdrawn in both vapor and liquid phases.

Column pressure control:

Total condensers are usually designed for accumulator
pressures up to 215 psia (1.48 MPa) at an operating
temperature of 120 F (49 C).
A partial condenser is usually used between 215 psia and
365 psia (1.48 to 2.52 MPa), and refrigerant coolant, such
as propane, is used if the operating pressure is greater
than 365 psia (2.52 MPa). The condenser pressure drop
is usually about 5 psia (34.4 KPa).

Column pressure control:

Most distillation columns are operated under
constant pressure, because at constant pressure,
temperature measurement is an indirect indication of
composition,
but floating the operating pressure can have
advantages in many applications. When the
column pressure is allowed to float, the composition
must be measured by analyzers or by pressure
compensated thermometers.

Column pressure control:

The primary advantage of floating-pressure
control is that one can operate at minimum
pressure, and this reduces the required heat input
needed at the reboiler.
Other advantages of operating at lower
temperatures include increased reboiler capacity
and reduced reboiler fouling.

Column pressure control:

In the following paragraphs, floating and constant
pressure control strategies will be described for
operations when
1) Liquid distillate is withdrawn in the presence
of non condensables.
2) Vapor distillate is withdrawn in the presence
of non condensables .
3) Liquid distillate is withdrawn when the amount of
non condensables is negligible.

Cooling Water Control, Negligible Inerts:

In distillation processes where the distillate is in the
liquid phase and the quantity of inerts is negligible,
the column pressure is usually controlled by
modulating the rate of condensation in the
condenser.
In the control system shown for Column A in Figure
10 (p. 18), the column pressure is controlled by
throttling the cooling water flow through the
condenser. This control scheme is recommended
only when the cooling water is treated, because
condenser tube fouling due to high temperature rise
across the tubes can occur.

Cooling Water Control, Negligible Inerts:

The advantage of this configuration is simplicity and low
maintenance cost, because the control valve is on the
water side and gives acceptable control performance,
provided the condenser is the bundle type, and the
cooling water is flowing through the tubes at a rate over
4.5 feet per second (1.35 m/s), or the water has
residence time of less than 45 seconds.
With such short residence time, the pressure controller
requires only a narrow proportional mode.
As the residence time increases, the controller will
require wider and wider throttling ranges and will also
need the addition of an integral mode to compensate for
the load changes.

Cooling Water Control, Negligible Inerts:

Liquid Distillate with Inerts:

The problem of pressure control can be complicated
by the presence of large quantities of inert gases,
which must be removed, because otherwise they will
blanket the condensing surface and cause the
loss of pressure control.

Distillate with Inerts:

When the amount of inerts is variable, the purge
stream has to be modulated. In the control system
shown for Column B in Figure 10, as the inerts build
up in the condenser, the pressure controller will
first open up the control valve (PCV-1), which
lowers the flooding level in the condenser and, by
increasing the heat transfer surface area, also
increases the rate of condensation.
When PCV-1 is nearly fully open (say 95%), the
valve position controller (VPC-2) is activated. Its set
point is 95%, so when PCV-1 has opened to 95%, it
starts purging the inerts by opening control valve
(VPCV-2).

Liquid Distillate with Inerts:

Vapour distillate with inerts:

The control system shown for Column C in Figure 10
is used when the distillate is in the vapor phase and
inerts are present. As the overhead product is
removed under pressure control, the system
pressure will quickly respond to changes in the
distillate vapor flow.

Column pressure with Vapour distillate with

inerts presents:

Vapour distillate with inerts:

Here, the level of the overhead receiver regulates
the condensate generated by throttling the cooling
water supply.This way it will condense only enough
material to provide the column with reflux.

This control system will give acceptable performance

only if the condenser residence time on the
coolant side is short.

Vapour distillate with inerts:

If this is not the case, the cooling water flow should
be held constant, and the control system shown for
Column D in Figure 10 should be used. In this case,
some liquid condensate is sent to a small vaporizer,
which flow is regulated by the accumulator level,
and the resulting vapors are mixed with the vapors
from the pressure-control valve.

Vapour distillate with inerts:

Vapour Recompression pressure control:

Diagram :
Working:
Cv and MV:

Types of continuous column:

THANK YOU

FOR YOUR ATTENTION

Types of continuous column:

Unit no : 5
Instrumentation for Evaporators &
Crystallizer

Types of continuous column:

Evaporators

Contents:
Introduction
Single effect evaporator
Multi effect evaporator
Types of evaporator
Different parameters in Evaporator

Various Instrumentation schemes for the evaporator

A:Types and operation of evaporators, Controlled and manipulated

variables in evaporator control problem, instrumentation for

feedback, feed-forward, cascade control strategies for evaporators,

types and operation of crystallizers, controlled and manipulated
variables in crystallizer control problem, instrumentation for control

of various types of crystallizers.

B: Selection of devices required in instrumentation

Introduction

Evaporation is one of the oldest unit operation.

It is the process of concentrating aqueous solution in a
closed vessel or group of vessel in which concentrated
solution is the desired product and indirect
heating(usually steam) is the energy source.
Evaporation is an energy intensive process
Its efficiency can be improved by increasing the number
of evaporator in series and some of the energy can be
recovered by vapor recompression
The product concentration can be measured by a variety
of analysers,including density, conductivity

Flow sheet symbols of Evaporator:

Single effect evaporation:

Multieffect evaporator:

Types of evaporator:
1) Horizontal tube evaporator
2) forced circulation
3) Short tube vertical
4) Long tube vertical
5)Falling film evaporator
6) Agitated film evaporator

Horizontal tube evaporator:

The liquid is evaporated at the outside of the tubes. It flows
from one tube to the other in form of droplets, jets or as a
continuous sheet.

Horizontal tube evaporator:

Due to the impinging effect when flowing from one tube to the
other the heat transfer is higher compared to vertical falling
film evaporators.
In addition this unit type can be operated with even lower
pressure drops compared to the vertical design.
It is also possible to design a higher heat transfer area for a
given shell compared to the vertical units. Perforated plates
or specially designed spray nozzles can be used in order to
guarantee a even liquid distribution for each tube.
Cleaning of the outside tubes can be difficult, therefore this
type of evaporators is not used for processes with tendency
to foul.
Tube dimensions are typically 0.75 to 1''.

Horizontal tube evaporator:

Feed
Vapour

Distributor
Steam
Condensate

Concentrate

Concentrate

Forced Circulation evaporator:

Disadvantages:
i) High cost
I ii) High residence time
iii) High operating cost

Short tube vertical evaporator:

Application:
i) Sugar industry

Control:
i) Level control

Long tube vertical evaporator: RFC

Long tube vertical evaporator: RFC

APPLICATION:
a)Black liquor in the pulp
and paper industry.
b) Corn syrup in the food
industry.
Control:
Level

Falling film vertical evaporator:

In falling film evaporators the
liquid feed usually enters the
evaporator at the head of the
evaporator.
In the head, the feed is evenly
distributed into the heating
tubes.
A thin film enters the heating
tube and it flows downwards
at boiling temperature and is
partially evaporated.

Falling film vertical evaporator:

The liquid and the vapor both flow downwards in a parallel flow.
This gravity-induced downward movement is increasingly augmented by the
co-current vapor flow.
The separation of the concentrated product from its vapor takes place in the
lower part of the heat exchanger and the separator.
In most cases steam is used for heating.

Falling film evaporators can be operated with very low temperature

differences between the heating media and the boiling liquid.
They also have very short product contact times, typically just a few seconds
per pass.

These characteristics make the falling film evaporator particularly suitable

for heat-sensitive products, and it is today the most frequently used type of
evaporator.

Falling film vertical evaporator:

Variables in evaporator:

Variables in evaporator:
Manipulated variables:
i) Flow rate
ii) Flow rate of steam
Controlled variables:
i ) Density of liquid
ii) Temperature
iii) Liquid level in evaporator
iv) Steam enthalpy
Disturbance:
i)Variation in steam flow
ii)Disturbance in case of steam run out
iii)Disturbance due to noisy measurement signal

Evaporator controls methods:( Instru and control)

The control systems are mainly to achieve the final product
concentration.
Method used to measure the product density.
Common methods are:
A) temperature rise, boiling point rise
B) Conductivity
C) Differential pressure
D) Gamma gauge
E) U Tube densitometer
F) Buoyancy float
G) Refractive index

Why use Density measurement ?

Real time process control.
On line measurement
Low maintenance and high reliability
Measurement of difficult and extreme process materials.
True density measurement
Low total installation cost.

Evaporator controls methods:( Instru and control)

i) Feedback control of evaporator
ii) Cascade control of evaporator
iii)Selective control of evaporator
iv) Feed forward evaporator control

Feedback control system of evaporator:

Cascade control of evaporator:

Selective control of evaporator:

Product density measurement:( Methods)

i)Temperature rise, boiling point rise
ii) Conductivity
iii) Differential pressure
iv) Gamma gauge
v) U-Tube densitometer
vi) Buoyancy float
vii) Refractive index

Note:
Page no 1289 Liptak II

Product density measurement:( Methods)

Crystallizer controls

Crystallizer controls

Crystallizer

Types of continuous column:

Crystallization:
is a unit operation that involves the separation of
a solute from its solution in the form of crystals.

Crystallization usually involves : Concentration of

solution and cooling of solution until the solute
concentration becomes greater than its solubility at
that temp then the solute comes out of the solution
in the form of pure crystals

Flow sheet symbols of Crystalizer

Crystallization
Crystallization is the unit operation that is best suited
to the recovery of dissolved substances from
solutions
solid product has many desirable properties such
has good flow charetercistes, handling easy, suitable
for packing
Methods to achieve crystallization:
i) Cooling
ii) Evaporation
iii) Vacuum or reaction
The choice of method depends upon the feed liquid
composition, product specification ,and other engg
consideration

Crystallization process(operation):
Three basics steps:
i) Achievement of super saturation
ii) Formation of nuclei
iii) Growth of nuclei into crystal

Crystallization process(operation):

Super saturation:

Degree of freedom of crystallization:

Types of continuous column:

Three methods:
i) Indirect heating Crystallizer
ii) Submerged combustion
iii) Spray evaporation

Indirect heating Crystallizer:

Indirect heating Crystallizer:

Submerged combustion:

Thanks

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