DISTILLATION COLUMN PROCESS CONTROL STRATEGIES

Today, distillation is one of the most used unit operations and is the largest consumer of energy in the
process industries. Separation operations achieve their objective by the creation of two or more
coexisting zones which differ in temperature, pressure, composition, and/or phase state. In chemical
and process industries, distillation makes a major chunk of energy consumption and hence having a
suitable process control strategy in order to save cost is a topic of great importance. The types of
variables are as follows:

Controlled Variable: The process variable which we want to maintain at particular value .

Manipulated Variable:Process variable that is adjusted to bring the controlled variable back to set point.
Disturbance Variable: Any process variable that can cause the controlled variable to change.

Controlled Variable Manipulated Variable Disturbance Variable

Distillate composition Distillate flow Feed Flow
Bottom Composition Bottom Flow Feed Composition
Accumulator level Reflux Flow Feed Temperature
Sump Level Reboiler Duty Reboiler heat supply
Column Pressure Condenser Duty Condenser cooling supply Weather
General guidelines for identifying which manipulated variables to associate with which controlled
variables are:

1. Manipulate the stream that has the greatest influence on associated controlled variable

2. Manipulate the smaller stream if two streams have the same effect on controlled variable.

3. Manipulate the stream that has the mostly near linear correlation with controlled variable

4. Manipulate the stream that is least sensitive to ambient conditions.

5. Manipulate the stream least likely to cause interaction problems.

Degrees of Freedom analysis for a Distillation Column:- The degrees of freedom of a process system are
the independent variables that must be specified in order to define the process completely.

There are two and only two additional variables that can (and must) be controlled in the distillation
column. a simple, ideal, binary system has two degrees of freedom; a complex, multi-component system
also has two degrees of freedom.

Types of Column control and variables which are mainly controlled:

 Pressure
 Temperature

The control schemes include the following:-

 Overhead Condensation
 Overhead Reflux
 Feed Preheat
 Reboiler Steam
There are a number of benefits of closing a reasonably fast temperature loop:

(1) Stabilizes the column composition profile (and thus keeps disturbances within the column).
(2) Gives indirect level control: Reduces the need for level control.
(3) Gives indirect composition control: Strongly reduces disturbance sensitivity.
(4) Makes the remaining composition problem less interactive and thus makes it possible to have
good twopoint composition control.
(5) Makes the column behave more linearly.

 Level

Levels may also be controlled such that ratios remain as degrees of freedom, for example the L/DV-
and L/DV
L – Liquid
V – Vapour
B – Bottoms
D – Distillate

 Flow Rate

 Composition

Concentrations of the top and bottom product streams are affected as well - higher bottom
temperature will results in more heavy components being vapourised from the bottoms product.

This can be illustrated using a multi-component separation of 8 products: C1, C2, C3, C4, C5, C6, C7 and C8+.
The main separation is between 2 key components: the light key (C4) and heavy key (C5). This is shown in
the Figure below.
If the bottom temperature is too high, more of the heavy key (HK) will be vapourised from the bottom
product. The vapour thus had become heavier due to the presence of the HK. The final boiling
point (FBP) of the top product will be higher but the initial boiling point (IBP) did not change.

On the other hand, the IBP of the bottoms product will be higher, because the bottoms product has
been depleted of the HK and become heavier. The FBP of the bottoms product is not affected by the
bottom temperature increase.

Other possible disturbances

Possible events that can disrupt the smooth operation of a plant are:

1) Reboiler and other heat exchangers: fouling of heat transfer surfaces, tube leaks, etc
2) Charge heater: loss of fuel gas and/or fuel oil (e.g. due to low fuel gas pressure trip)
3) Overhead condenser: loss of cooling water or loss of power supply (for air-fin coolers)
4) Pumps: overload trip, loss of power, cavitation, etc
5) Control valves failure: e.g. loss of instrument air, jammed valve, faulty positioners, etc.
6) Faulty instruments: wrong signals transmitted, false alarms, etc.
7) Feed changes: feed rate, more lower boiling components, contaminations, etc.
8) Tower internals: e.g. flooding, weeping, channelling, etc.
 Heat exchangers
Heat Exchanger System : Heat exchanger transfers heat between two fluids without mixing them
up. The dynamics of heat exchanger depends on many factors like temperature difference, heat
transfer area, flow rate of fluids, flow patterns. Heat exchanger finds wide spread applications in
different industries such as petroleum, food, petrochemical, power generation, nuclear, space craft
etc. The basic principle of heat exchanger is shown in Fig. 1.
There are various types of heat exchanger which are categorized with respect to construction,
transfer process, flow and phase. A brief classification of heat exchanger is shown in Fig. 2. Shell and
tube heat exchanger probably is the most common type of heat exchangers applicable for wide
range of operating temperature and pressure. It has larger ratio of heat transfer surface to volume
than double-pipe heat exchangers, and it is easy to manufacture in a large variety of size and
configuration. Shell and tube heat exchanger can operate at high pressures, and its construction
facilitates disassembly for periodic maintenance and cleaning. A shell-and-tube heat exchanger is an
extension of the double-pipe configuration. Instead of a single pipe within a larger pipe, a shell-and-
tube heat exchanger consists of a bundle of pipes or tubes enclosed within a cylindrical shell. In shell
and tube heat exchanger one fluid flows through the tubes, and a second fluid flows within the
space between the tubes and the shell.
 REACTORS
REACTORS IN PROCESS ENGINEERING

Generalized Reactor Design

Design of a chemical reactor starts with a knowledge of the chemical reactions that take place in the
reactor. The ultimate product of the design is the reactor and the supporting equipment such as
piping, valves, control systems, heat exchangers, and mixers. The reactor must have sufficient
volume to handle the capacity required and to allow time for the reaction to reach a predetermined
level of conversion or yield.

 Product sequence. Polymerization reactors are rarely built to make only one product over the
entire life of the equipment. Normally, a reactor switches among a handful of products. In
addition, markets change, so manufacturers prefer a flexible design — one that is good today,
and, with little or no modification, 30 years from now.
 Reactor configuration. Reactor configuration is determined by the reaction scheme for making
the product of choice with the desired molecular architecture. Living polymers, for example,
maintain their narrow distributions as long as all chains have the same residence time, which can
be achieved in a well-mixed batch reactor or a plug-flow reactor.
 Reactor conditions. Polymer properties, like catalyst activity, also vary with temperature and with
the level of chain-transfer agent. Reactor conditions depend on the reactor configuration. Some
reactors are vulnerable to temporal or spatial variations, the products of which are really
composites of chain populations produced at various times or various locations in the reactor.
 Heat removal. The heat released by many polymerization reactions of commercial interest is
usually more than a simple heat-removal mechanism, such as a jacket or a coil, can handle. As a
result, engineers need to be creative in developing mechanisms that do not significantly increase
capital cost — for example, an external heat exchanger with a recirculation pump. The high
viscosities of most polymerization systems, and the corresponding low heat-transfer coefficients,
make this task particularly challenging.
 Fluid mechanics. Polymers and their mixtures do not always behave like Newtonian fluids. This
issue is particularly critical in a monomer-injection system, where fluids with very different
properties and temperatures must mix rapidly to avoid creating polymer populations with the
wrong properties.
  Mass-transfer limitations. Mass-transfer limitations are common in heterogeneous systems,
because the monomer and other components must diffuse through a continuous phase in order
to reach the discrete phase where polymerization takes place. Systems that appear to be simpler
can have these limitations as well. For example, if the monomer is volatile and a headspace exists
in the reactor, the monomer may accumulate in the headspace, lowering its rate of consumption
in the liquid phase.
 Thermodynamic constraints. Even if only one phase is expected to exist in the reactor, process
operators and engineers should stay vigilant to ensure that a second phase does not form.
Running the reactor at a very low pressure risks the formation of a vapor phase. Running at a very
low temperature risks coating the reactor internals with polymer. Neither of these is a welcome
sight, especially the latter.
 Process dynamics. In continuous processes, the more complex the product sequence, the more
important it is to manage a quick transition between polymer grades. Some grades might be
completely incompatible because of the markets to which they are destined, so the need to avoid
cross-contamination puts an additional stress on the manufacturer, and highlights the need for
efficient product-grade-transition schemes.
 Reactor stability. The thought of releasing increasing amounts of energy from a reactor brings to
mind the possibility of multiple steady states, sustained oscillations, chaotic behavior, and the
danger of a reactor runaway. A good reaction system design avoids operating a reactor too close
to a limit point, for example, where a small disturbance causes a rapid deviation from the desired
steady state.

LAB: Linear alkylbenzenes

HAB: Heavy alkylbenzenes

Adiabatic reactor: Vessel that is well insulated to minimize heat transfer and has an increase
or decrease in temperature from the initial inlet conditions due solely to the heats of
reaction.
Batch reactor: Vessel used for chemical reaction that has no feed or effluent streams. The
reactor is well stirred and usually run either isothermally or adiabatically. The main design
variable is how much time the reactants are allowed to remain in the reactor to achieve the
desired level of conversion.
Continuous stirred tank reactor: Sometimes called a continuous-flow stirred-tank reactor,
ideal mixer, or mixed-flow reactor, all describing reactors with continuous input and output
of material. The outlet concentration is assumed to be the same as the concentration at
any point in the reactor.
Isothermal reactor: Any type of chemical reactor operated at constant temperature.
 Plug flow reactor: Sometimes called a piston flow or a perfect flow reactor. The plug flow
reactor has continuous input and output of material. The plug flow assumption generally
requires turbulent flow. No radial concentration gradients are assumed.
Reactor Terminology
Conversion: Fraction or percentage that describes the extent of a chemical reaction.
Conversion is calculated by dividing the number of moles of a reactant that reacted by the
initial moles of reactant. Conversion is defined only in terms of a reactant.
Catalyst: Substance that increases the rate of a chemical reaction without being consumed in
the reaction.

Elementary reaction: Reaction that has a rate equation that can be written directly from a
knowledge of the stoichiometry.
Mean residence time: Average time molecules remain in the reactor. Note that this is different
from space time.
Multiple reactions: Series or parallel reactions that take place simultaneously in a reactor. For
example, A + B → C and A + D → E are parallel reactions, and A + B → C + D → E + F are
series reactions.
Product distribution: Fraction or percent of products in the reactor effluent.
Rate constant: Constant that allows the proportionality between rate and concentration to be
written as a mathematical relationship. The rate constant is a function of temperature only
and is generally modeled by an exponential relationship such as the Arrhenius equation.
Rate equation: Mathematical expression that is a function of both concentration of reactants
or products, and temperature.
Reaction mechanism: Series of elementary reaction steps that when combined, gives the
overall rate of reaction.
Space time: Time to process one reactor volume based on inlet conditions.
Yield: Moles of a desired product divided by moles of a limiting reactant.

I. Reactor Classifications
Reactors may be classified by several different methods depending on the variables of interest.
There is no single clear cut procedure for reactor classification. As a result, several of the more
common classification schemes are presented here.
A. OPERATION TYPE
The operational configuration for the reactor can be a primary method of classification.
1. Batch
Batch reactors are operated with all the material placed in the reactor prior to the start of
reaction, and all the material is removed after the reaction has been completed. There is no
addition or withdrawal of material during the reaction process.
2. Semibatch
The semibatch reactor combines attributes of the batch and the continuous-stirred tank. The
reactor is essentially batch but has either a continuous input or output stream during operation.
3. Continuous Flow Reactors
Continuous flow reactors represent the largest group of reactor types by operational
classification. Several continuous flow reactors are used industrially.
B. NUMBER OF PHASES
Reactors can also be classified by the number of phases present in the reactor at any time.
1. Homogeneous
Homogeneous reactors contain only one phase throughout the reactor.
2. Heterogeneous
Heterogeneous reactors contain more than one phase. Several heterogeneous reactor types
are available due to various combinations of phases .
a. Gas-liquid
 b. Gas-solid
c. Liquid-solid
d. Gas-liquid-solid
Multiphase reactor configurations are strongly influenced by mass transfer operations. Any of
the reactor types presented above can be operated as multiphase reactors.
C. REACTION TYPES
Classification of reactors can also be made by reaction type.

1. Catalytic
Reactions that require the presence of a catalyst to obtain the rate conditions necessary for
that particular reactor design.
2. Noncatalytic
Reactions that do not include either a homogeneous or heterogeneous catalyst.
3. Autocatalytic
Reaction scheme whereby one of the products increases the overall rate of reaction.
4. Biological
Reactions that involve living cells (enzymes, bacteria, or yeast), parts of cells, or products from
cells required for the reaction scheme.
5. Polymerization
Reactions that involve formation of molecular chains, whether on a solid support or in
solution.
 FURNACE
FURNACE Furnace is a device used in heat transfer unit operation in many processes where the charge
(feed) or process fluid entering the furnace is heated to a desired temperature in a controlled manner.
The major difference in furnace and heat exchanger is that in heat exchangers the heat is transferred
between two fluids one being the process and other being utility such as hot stem, hot oil etc while in
the furnace the source of heat is combustion of the fuel gas; used to transfer the heat energy to the
process fluid to heat it to the desired temperature.
Furnaces are generally available in many designs depending on their area of application and function.
Furnaces are used in industries for many major heat transfer operations and their functions can be
broken down in following three categories:
 To heat or vaporize the charge.
 To provide heat of reaction to the reacting feeds
 To provide and evaluate the controlled temperature for the physical change of charge material.

Some of the commonly used furnaces in industries are Start up Heater, Fired Reboilers, Reformer
Furnace, Cracking (Pyrolysis) Furnaces etc ,operation they all perform remain same i.e. heat transfer

Principle of operation of furnace A typical furnace used in industries look like a metallic housing lined
with a heat conserving refractory.

The major components of the furnace system consist of air blower, burner, combustion chamber,
heated coils and air vent path with adjustable damper.

The charge can enter the furnace and flow in to the heated coils or tubes as solid, liquid or gas and may
or may not be converted to a different state by the heat energy supplied.
The charge is carried through the furnace in to the metal coils where it can be heated continuously or
batch heated by remaining stationary after entering. This depends on the function that the furnace is
employed for i.e. vaporization of charge, provide heat of reaction etc.

Now from the process point of view the furnace can be required in two phase of the process, one while
the process is being initialized or start up and second while the process have already been initialized i.e.
to maintain the sustainability of the process.

The basic operation of furnace in both the phases remain same however the requirement by the process
varies widely, this gives rise to two different categories of the furnace called Start-up Heaters which are
required to start up a process unit and are normally functional till certain hours to few weeks and
reboilers which are functional till the process last.

It is necessary to be noted that no matter what category of the furnace we are looking at the basic
operation remains almost same which is to heat the process fluid to the desired temperature.
Furnace control system The primary functions of furnace control systems can be listed as following:

 To ensure that the charge receives the heat energy at the proper rate, the controlled variable is the
exit temperature of the charge.

 To maintain efficient combustion of the fuel. Proper combustion of the fuel requires the regulation of
the air-fuel ratio.

 To maintain the safety during all phases of furnace operation so as to prevent explosions or fires.

The recommended control strategies can be thus broken down into the following three categories:

1. Process controls.

2. Fuel firing controls.

3. Safety controls.

Process control ensure that the charge receives the heat energy at the proper rate,

Safety control is implemented to ensure the safety in furnace operations.

The potential sources of hazards include

 Fire or explosion caused by tube rupture. Such rupture can occur because of tube overheating due to
feed flow loss or because of flame impingement

 Explosion in the firebox caused by the loss of flame or by improper ignition or purge procedures The
standard ANSI/ISA-84.01–1996, “Application of Safety Instrumented Systems (SIS) for the Process
Industries,” is implemented to ensure the safety of a furnace operation.
 MINERAL PROCESSING INDUSTRY

Process system – Introduction A machine working in a mineral process flow cannot perform better
than the process environment will allow it to. Parameters like type, size and amount of feed, %
solids in slurries, additives, discharge conditions etc. will always guide equipment performance and
operation economy.
Basic operations

Size reduction

Crushing

Grinding

Size control

Screening

Classification

Enrichment

Washing

Gravity separation

Flotation

Magnetic separation

Leaching

Upgrading

Sedimentation

Mechanical dewatering

Thermal drying

Thermal processing

Materials handling

Unloading

Storing

Feeding

Conveying

Slurry handling

Slurry transportation

Agitation and mixing

'Everything in the 21st century begins with mining.' For example, 46,000 pounds of new minerals
including 7,500 pounds of coal energy must be provided annually for every person in the US to
maintain their standard of living. In the course of a lifetime, each American will use 3.5 million
pounds of minerals, metals, and fuels1. In addition to individual impacts, mining also has a strong
impact on US economy

It is projected that improvements in mineral processing technology will lead to the following
benefits:

• Energy Efficiency - Improved energy efficiency per unit of output

• Environment - Reduced emissions per unit of output

• Health and Safety - Improved worker safety in processing activities

• Productivity - Reduced cost and higher value per unit of output

• Reserve Base - Increased reserves through technological advances and improved economics

This roadmap identifies three areas of processing technology where the most impact and the
greatest progress toward the mining vision goals can be expected.

1. Mineral Preparation

2. Physical Separations

3. Chemical Separations

1. Mineral Preparation
Mineral processing includes the following:

• Comminution - the gradual reduction of a hard mineral to a fine powder or dust by crushing,

grinding, or attrition for direct use or further processing.

• Makedown - the conversion of extracted soft rock minerals into a slurry.

• Classification - the process of separating particles of various sizes, densities, composition, and

shapes as part of the preparation circuit to control the final product.

• Blasting and drilling – it includes those activities associated with identifying optimum locations
within mineral deposits for the placement of explosive charges and the detonation of those charges.

There is a wide range of mineral preparation research and development activities that, if
implemented, can improve energy efficiency, environmental performance, health and safety, and
productivity. These research activities are grouped into four categories:

Dust Emissions Improvements of both active and passive methods for dust control are needed to
further reduce dust emissions.

Blasting and Drilling - Significant opportunities exist to improve productivity and energy efficiency in
the early stages of mineral preparation operations, This includes research to improve tools for
analyzing mineral deposits and to better understand the characteristics of mineral deposits. This can
be achieved by
 1 Improved models, sensors, and instrumentation.

2 Improved blasting design

3 improve energy efficiency in crushing

4 reduced maintenance and wear

5 process integration

6 reduced dust emissions.

Classification - The ability to improve the efficiency of machinery currently used in altering or
reducing the particle size will help to improve overall processing energy efficiency and productivity.

Instrumentation and Sensors - Advanced sensors and instrumentation can result in crosscutting

efficiency and productivity

Materials - In addition to the above, the mining industry is looking to future advances in existing
structural and containment materials and the development of new materials to improve wear
resistance in crushing and grinding.

2. Physical Separations
physical Separations are those processes where valued substances are separated from undesired

substances based on the physical properties of the materials.. Typical physical separation processes
and their definitions include:

• Flotation - Mineral separation, in which a variety of reagents are added to an agitated and
aerated

mixture of liquids and solids. This causes certain finely crushed minerals to adhere to air bubbles

and to rise to the surface where they enter a froth, leaving the remaining minerals behind.

• Dewatering - Separates solid materials from water in which it is dispersed, performed by

equipment

such as thickeners, classifiers, hydrocyclones, filters, and centrifuges.

• Thickening or Settling - Reduces the proportion of water in a material by means of

sedimentation

or elutriation.

• Filtering - Separates suspended solid particles from liquids, or fine dust from air.

• Drying - Removes water using air or heat.

• Flocculation - Selective agglomeration, or adhesion of material components to water or other

immicible liquids. In this process, loosely bonded associations of particles and bubbles are formed
that are lighter than water.

• Screening - The uses of one or more screens or sieves to separate particles into defined sizes.

• Magnetic Separation - The uses of permanent or electromagnets to separate magnetic particles

from other process streams.

• Classification - The separation of particles of various sizes, densities, and shapes through their

movement in a fluid. Includes centrifugal separation.

• Washing - Removes ash, shale, sulfur, and other unwanted products from crushed material
using water.

3. Chemical Separations
Chemical Separations involve isolating metals and minerals from their ore by chemical processes.

• Solvent extraction - The separation of one or more substances from a mixture by treating an

aqueous solution of the mixture with a solvent that will extract the required substances, leaving the

other undesirable materials behind.

• Leaching - The extraction of soluble metals or salts from an ore by means of slowly percolating

solutions.

• Bioleaching - The catalytic action of bacteria, such as Thiobacillus ferroxidans and Thiobacillus

thiooxidans, to accelerate chemical oxidation reactions by as much as one million times those of

chemical reactions alone; especially useful in leaching copper and uranium systems.

• Smelting - The chemical reduction of a metal from its ore by a process usually involving fusion,
so that earthly and other impurities separate as lighter and more fusible slags and can readily be

removed from the reduced metal.

• Refining - An electrolytic or chemical process that produces a pure metal.

• Electrowinning - An electrochemical process in which a metal dissolved within an electrolyte is

plated onto an electrode resulting in a pure metal.

• Pelletizing or Briquetting - A process by which coke breeze, coal dust, iron ore, or any other

pulverized mineral is bound together under pressure, with or without a binding agent such as

asphalt, and thus made conveniently available for further processing or for commercial markets.
Improving Heat Efficiency - Optimizing the use of process heat, maximizing combustion efficiency,
utilizing waste heat, and streamlining processes to minimize heating and cooling can all lead to
increased conversion efficiency.

Increasing Direct Conversion and in-situ Recovery - The most effective way to increase conversion

efficiency is through the reduction or elimination of processing steps.

Decreasing Time to Close Processing Operations - The energy, time, and effort in preparing for and
in closing of processing operations has been targeted for improvement.
USE OF CONTROL SCHEMES FOR PROCESS OPTIMIZATION

Using modern DCS and/or PLCs, various powerful, robust, money-making control schemes can be
implemented.

The powerful techniques for designing and implementing DCS or PLC-based APC schemes, which are
optimized using the 3G algorithm are:

1. Process dynamics identification

2. Primary PID and APC optimization

3. Online adaptive control

4. Model-based control for product quality and production rate maximization.

II. Advanced Control Theory

In this section, the concept of multivariable control and optimization will be described.

• Input (Independent) Variable - A variable that independently stimulates the process and can

induce change in the internal conditions of the process. One may or may not have the ability to
manipulate these variables. Examples include flow rate of gas into a furnace, the setpoint of a

furnace temperature controller and the ambient air temperature.

• Output (Dependent) Variable - A variable by which information about the internal state of the

process can be obtained. One cannot directly manipulate these types of variables. Examples

include the dew point in the furnace atmosphere or the furnace temperature.

• Manipulated Variable - An input variable that can be altered (or manipulated) in order to

achieve a control objective.

• Controlled Variable - A variable that is to be controlled by making changes to manipulated

variables.

• Disturbance Variable (Feedforward) - An input variable that one has no control over. An

example might be the ambient air temperature outside the furnace.

• Single-Input, Single-Output (SISO) - A system with one input and one output.

• Multi-Input, Multi-Output (MIMO) - A system with multiple inputs and multiple outputs.

To overcome some of the difficulties in using SISO controllers on a multivariable process, some of
the following techniques are used:

• Cascade control: Two SISO controllers are linked, with output of the primary controller

changing the setpoint of the second controller. Controlling purity by manipulating the setpoint

of a flow controller is an example of cascade control.

• Feedforward control: Changes in measured disturbances are sent to the SISO controller. The

idea is that the controller can begin to account for the effect of the disturbance before it actually

affects the output variable being controlled.

• Ratio control: Manipulating one flow rate in order to keep the ratio between it and another flow

rate constant is an example of ratio control.

• Override control: When more outputs exist than inputs, override control is often used. Input 1

is used to control output 1 unless output 2 exceeds a certain value. In that case, input 1 switches

to control output 2.
The characteristics of this type of control strategy include:

(1) Most of the setpoints of the controllers are fixed. It usually takes operator intervention to change

the setpoint. No optimization is taking place and the process usually runs at non-optimal conditions.

(2) Feedback control is used. Control action is generally taken only after a disturbance or event has

already occurred and affected the process. Adding a feedfoward component to the SISO controller
can help improve the control.

(3) Because a SISO control strategy is used, each Control Variable (output) is paired with a single,

unique Manipulated Variable (input). The interaction issues described previously are present.

An MPC scheme for the same reactor process is pictured in Figure 5. The main characteristics of this

type of controller include:

(1) The MPC controller attempts to optimize the process. Dynamic models representing how the

process behaves are used to predict future behavior and to determine the optimal operating point.

(2) The predictions of the future behavior are also used to determine the control action taken by the

controller. Disturbances can be rejected before they affect the process.

(3) MPC is a multi-input, multi-output (MIMO) controller. No input/output pairings need to be

identified. All manipulated variables are moved simultaneously to control all the controlled
variables.Interaction is accounted for with the dynamic models and used as an advantage in the
control. Also, thenumber of inputs does not need to be equal to the number of outputs. MPC can
handle non-square systems very easily