Group A

Janinne Liz Steve Janice Andrea

A distillation column was being recommissioned following a routine shut down. The plant operators began to slowly, bring the unit up to normal operating conditions. At 7:00am the following morning there was a violent explosion and subsequent fire. The explosion was heard and felt up to 30km away.

Applying the principles learned throughout the course of this presentation we will discover how this explosion could have been prevented.
Source: (www.hse.gov.uk, 2002)

OVER 40% OF THE ENERGY USED ANNUALLY IN CHEMICAL PROCESS INDUSTRIES IN THE UNITED STATES GOES TO DISTILLATION PROCESSES *

*Source: (Sabarathinam, 2002)

How Much Energy is that?

2,499,743,943,870,000,000 Joules
That is enough energy to run around the world a trillion times!!!! In fact, distillation accounts for almost 15% of all industrial energy consumed in the United States!!!*
*Source: (Sabarathinam, 2002)

How much is Distillation Used?

Worldwide, distillation accounts for 95% of all separation processes* In the United States alone how many columns do you think exist?

40,000+
*Source: (Sabarathinam, 2002)

How much money is locked up in distillation operations?

In the United States:

Over $8 billion

THATS $12.8 BILLION CANADIAN!!

When is Distillation Used?*

When the relative volatility is greater than 1.5 When the product is not temperature sensitive When there are negligible solids in the feed
*Source: (Woods, 1995)

Two-Component Distillation:
The diagram below displays a typical 2 component distillation column we have seen so many times before
Distillation is a combination of mass transfer, heat transfer, fluid mechanics, thermodynamics, and of course.Process Control!!!!

2A04 Heat Exchangers 3M04 Tray Selection/Design 3D03 Component Equilibrium

3004 Fluid Flow Properties

3P03 System Operation
Source: http://lorien.ncl.ac.uk/ming/distil/distileqp.htm

Interesting Equipment.
Reboilers
Purpose?
Essentially act as a heat exchanger which brings the liquid at the bottom of the column to its boiling point, and returns vapour back into the column.

Types:
Thermosyphon Reboiler Kettle Reboiler

Kettle Reboiler (Gravity-fed)

Liquid from tower is partially vapourized 2. Domed section of the reboiler separates liquid and vapour 3. Vapour flows back to the tower 4. Liquid overflows the baffle
1.

Source: http://lorien.ncl.ac.uk/ming/distil/reboil.htm

Thermosyphon Reboiler:
Driving force to promote flow through the reboiler is a density difference between the reboiler feed line and the reboiler return line

Source: http://lorien.ncl.ac.uk/ming/distil/reboil.htm

Operability Operating Window

In the operation of a distillation tower, narrow limits are imposed to avoid inefficiency.

Inefficiencies include: flooding weeping reboiler and condenser violations Response to these violations act to: protect the equipment protect distillation tower against overpressure, overtemperature and overflow achieve desired separation

Operability
The Three Objectives of Operability in Distillation are as follows:
1. Locating constraints within the distillation column 2. Provide protection against violations 3. Permit operation to proceed in the presence of violations by remaining inside the operating window

Operability Operating Window

Locating Constraints within Distillation Column: 1. Tray 2. Reboiler 3. Condenser

TRAYS
Typical Sieve Tray Construction Liquid falls through the downcomer Outlet weir ensures a set liquid height (hold up) on tray Trays act to provide separation of components within the distillation tower
vapour

Weir Downcomer Tray Deck

Tray Efficiency
Vapour flow conditions effect tray efficiency Tray efficiency is a measure of deviation from vapour liquid equilibrium Tray efficiency can be inferred by comparing vapour temperature leaving a tray to liquid temperature leaving a tray

400F Vapour

350F Liquid

400F Vapour

350F Liquid
450F Vapour

400F Vapour

BAD

100% Tray Efficiency

0% Tray Efficiency

Implication of Tray Efficiency

WEEPING CAN OCCUR occurs at low vapour flow rates causing liquid on the tray deck to flow through the tray perforations rather than the downcomer

What could cause weeping?

Implication of Tray Efficiency

FLOODING CAN OCCUR
Due to high vapour flow rates or Due to high liquid flow rates

In both cases this causes liquid to accumulate on the tray deck which results in the back up of liquid in the downcomer

What could cause flooding?

Distillation Column Operating Window

Column pressure is the one of the major constraints in distillation operation Column pressure is typically controlled by adjusting the heat removal in the condenser Overall distillation operation is determined by: 1. Trays which define separation efficiency 2. Condensers which define column pressure 3. Reboilers which define the vapour flow conditions and drive the distillation tower by supplying sufficient amount of vapour

Distillation Column Operating Window

In normal operation, there are two primary handles that can be adjusted to manipulate the behaviour of the distillation column (assuming pressure and level control)

1. Condenser Duty (reflux flow) 2. Reboiler Duty (boilup flow)

Steering the Distillation Column

Flare

Condenser
P
PC

LC

Reflux Drum

Distillate

Feed
dP

T TC LC

Bottoms

Reboiler

Distillation Column Operating Window

Four Possible Violations that can Occur:
1. 2. 3. 4. Weeping Flooding Condensing Pressure Vessel
Steam condensate capacity
Maximum production

Flooding

Vessel Pressure limit

Interested in frame of window in order to design the towers and operate them efficiently and troubleshoot them accordingly

Weeping

Weeping Violation
Steam condensate capacity
Maximum production

Flooding Vessel Pressure limit

Increasing reboiler duty at a constant pressure.

Weeping

Column Pressure

Case 1: Weeping
Flare

Temperature indicates separation efficiency. A change in differential pressure could be an indication of weeping

Condenser
P PC

LC T

Reflux Drum

Distillate Feed
dP
T

TC
LC

Increasing the steam rate will increase the boilup and pressure rising through the column, in order to hold up the liquid on each tray
Reboiler

Bottoms

Flooding Violation
Steam condensate capacity
Maximum production

Flooding Vessel Pressure limit

Decreasing reboiler duty at a constant pressure.

Weeping

Column Pressure

Case 2: Flooding
Temperature indicates separation efficiency. A change in differential pressure could be an indication of flooding. The flow sensor indicates a loss of liquid level in the bottom of the column.
Flare

Condenser
P
PC

LC

Reflux Drum

Distillate

Feed
dP

T TC LC

Decrease reboiler duty in order to reduce the vapour being condensed. This allows the column to reach equilibrium.
Reboiler

Bottoms

Condensing Violation
Steam condensate capacity
Maximum production

Flooding Vessel Pressure limit

DO NOTHING!

Weeping

Column Pressure

Case 3: Not Enough Condensing

Flare

Condenser
P PC

The level control will indicate a high level in the reflux drum and condenser.

LC

Reflux Drum

Distillate Feed
dP

TC LC

Bottoms

Reboiler

DO NOTHING: The high level of vapour will increase the column pressure overtime. The column will correct itself using the pressure and level controls.

Vessel Pressure Violation

Steam condensate capacity
Maximum production

Flooding Vessel Pressure limit

Decreasing reboiler duty.

Weeping

Column Pressure

Case 4: Activated Safety Valve

The vessel pressure limit is exceeded as indicated by the pressure sensors and the activation of the safety valve.
Flare

Condenser
P PC

LC

Reflux Drum

Distillate Feed
dP

TC
LC

Decrease reboiler duty in order to produce less vapour and decrease the column pressure.
Reboiler

Bottoms

Main Safety Concerns

Fire Risk
Dealing with flammable liquids Need to isolate system in case of fire

Over Pressuring
Occurs when the condenser is restricted Must provide pressure relief

Safety Equipment
Relief Valves Corrosion Monitoring
X-Ray Techniques Radioactivity Ultrasonic Testing Corrosion Coupons Corrosion Probes

Alarms and Trips

Fail position of valves

Points of Control
Feed Rate and Production Rates Temperature Pressure Level in Reflux Drum and Column Bottom Coolant Flow and Steam Flow Reflux Rate

7 Control Objectives
1. 2. 3. 4. 5. 6. 7. Safety Environmental Protection Equipment Protection Smooth Operation and Production Rates Product Quality Profit Monitoring and Diagnosis

Source: Process Control: Designing Processes and Control Systems for Dynamic Performance, Marlin 2002.

1. Safety
Pressure control and relief in case of condenser restriction. Alarms warn of potential hazards.
Flare
PAH PAH

Condenser
P

PC

LC

Reflux Drum

Feed

FC

FC dP

Distillate

LAH LAH LAL LAL

LC

TC

Bottoms

Reboiler

2. Environmental Protection
Avoiding flaring by it in emergency situations protects the environment for undue contamination
Flare

Condenser
P

PAH

PC

LC

Reflux Drum

Feed

FC

FC dP

Distillate

LAH LAL
LC

Bottoms

Reboiler

3. Equipment Protection
Uses pressure drop to determine if corrosion is present. Tray temperatures can also be used.
Flare

Condenser
P

PAH PC

LC

Reflux Drum

Feed

FC dP

FC

Distillate

LAH LAL

LC

Bottoms

Reboiler

4. Smooth Operation
Levels are non-self regulatory and therefore need to be controlled. These level controllers will allow for stable operation.
Flare

Condenser
P

PAH

PC

LC

Reflux Drum

Feed

FC

FC dP

Distillate

LAH LAL
LC

Bottoms

Reboiler

How do we Control Product Quality?

What variables do we want to control? What knobs do we have to control quality? Are there any limits to this control?

5. Product Quality
Controls distillate composition using distillate rate or reflux rate. Controls composition of the bottoms product using the temperature as an inferential control variable
FC

Flare

Condenser
P

PAH

PC

LC

Reflux Drum

FC dP

Distillate

Feed

LAH LAL
LC

TC

Bottoms

Reboiler

Inferential Control
Use a measurable variable to infer a needed variable Design Criteria
Measurement of a true controlled variable Inferential variable available Relationship between inferential and measured variable insensitive to operational changes Dynamics favourable for feedback control
(Process Control, Marlin 2002)

In this case using Temperature to infer Composition and therefore required heating.

TRAY TEMPERATURE VERSUS ANALYZERS

Tray Temperature Product quality not stringent Less costly Allows for quick analysis Analyzers Product quality important Costly (requires more equipment) Dead time encountered in transporting a sample to chromatograph detector Directly measures concentration of several components in a mixture to achieve accuracy and control

Cannot directly measure concentration

6. Profit
This depends on plant wide operations
Energy Use Production Rates and Requirements

7. Monitoring and Diagnosis

Covered in the Operability Section

Troubleshooting: Class Exercise

During re-commissioning of plant PRV was removed for re-rating. Plant operators began to slowly bring unit up to normal operating conditions At 5:00am you receive a page that the High Pressure Alarm has been activated. We have 2 hours to prevent the explosion

Troubleshooting Symptoms
Pressure is High on all sensors High level in reflux drum Reflux valve fully open Feed Flow rate at half of normal operations Higher than normal temperature within column Lets Find the Solution

Troubleshooting Diagram
Condenser
P
PAH

LC

Reflux Drum

Steam

What is the Solution?

FC

FC

Distillate

dP

Feed
LAH LAL
LC

TC

Bottoms

Reboiler

Troubleshooting: Solution
Pressure Relief Valve was removed Flow Rate too low for the amount of heat transfer occurring Too much vapour is being produced in the column, leading to condenser restriction Reduce Boilup Long term: A bypass on the steam flow is required to avoid overheating/excessive vapourization