Manual for the distillation column

Jørgen K. Johnsen

June 21, 2005

Contents
1 Introduction 2

2 Experimental column setup 2

2.1 The column . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
2.2 Instrumentation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
2.2.1 Actuators . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
2.2.2 Sensors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
2.3 Control loops . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5

3 LabView User Interface 5

4 Operator instructions 7

5 Data logging 8

6 Source code 8

A I/O connections 11

References 12

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1 Introduction
This is a manual for the continuous distillation column separating methanol and
water. First a description of the column setup is presented in section 2. A control
program for the column has been implemented in LabView, and the user interface
to this program is presented in section 3. Then detailed start-up and operating
instructions are given in section 4 and 5. A short description of the underlying
source code is given in section 6. For reference, the I/O module connections are
given in appendix A.
The manual does not intend to give a detailed description of the underlying
control algorithms, instead the reader is referred to [1] for controller details.

2 Experimental column setup

In this section a short description of the dierent components in the experimental
column is given, together with an overview of inputs to and outputs from the
system. The dierent control loops involved in the automatic control system are
presented.

2.1 The column

Figure 1 shows a picture of the distillation column together with a ow sheet.
Table 1 gives the most important column data.
The column consists of two sections lled with 6mm Raschig-rings unstructured
packing. A condenser is connected to the top of the column. The condensate ows
into the reux drum, from where a fraction is pumped back into the column as
reux to get desired composition. The distillate pumped out of the system and
into the distillate product tank is used to control the level in the reux drum.
Vapor is produced by heating coils in the boiler connected to the bottom of the
column. The boiler level is controlled through the bottoms ow pumped out of the
system and into the bottoms product tank. For security, the boiler is protected
with a plexi-glass cover shield.
A feed mixture of methanol and water is pumped from the feed tank and into
the feed section approximately in the center of the column. To avoid spill after
nishing an experiment, a manually controlled recycle pump is used to transfer
distillate and bottoms back into the feed product tank.
The entire system is mounted in an aluminum frame which can be moved as a
single unit.

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(a) Experimental setup (b) Flow sheet with sensors and actuators

Figure 1: Distillation system

Table 1: Column data

Material: Glass and steel
Column height: 250cm
Diameter: 50mm
Condenser: 0.3m2 i.d.
Max boiler power: 3kW
Max reux rate: 4ml/s
Max feed rate: 5ml/s
Boiler volume: 10l
Reux drum volume: 5l
Product tanks volume: 25l
Frame dimensions: 120 × 125 × 285cm (l×w×h)

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2.2 Instrumentation

2.2.1 Actuators

Five pumps are connected to the column system to control the dierent ows.
The reux and feed pumps are continuous with 4-20mA input. The distillate and
bottoms pumps are on/o pumps which are pulse width modulated to allow for
dierent pump rates.
The recycle pump is of on/o type and is turned on manually by the operator
when recycling the products before a new experiment. This pump is not a part of
the automatic control system.
Four heating coils generate the vapor inside the column. Two coils are 1000W
each, the two other ones are 500W, giving a total of 3kW power input. The heating
coils are turned on and o by relays, and are pulse width modulated.

2.2.2 Sensors

There are eight PT-100 temperature sensors inside the column to measure the
temperature prole. One of the sensors is in the boiler, the remaining ones are
inserted via the feed section and the top, and are held in place by the column
packing. A Fieldpoint RTD I/O module measures temperature sensor resistance
and converts resistance to temperature.
Two pressure sensors are located at the top and at the bottom of the boiler
respectively. The pressure dierence between the sensors is proportional to liquid
level in the boiler and is used as input to the boiler level controller. The column is
open to air after the condenser in the top, hence the absolute pressure above the
liquid boiler holdup gives the pressure fall over the column.
A level sensor is placed in the reux drum to give feedback to the reux level
controller.
The cooling water is equipped with a ow meter to assist the operator when
turning on cooling. The sensor output is also monitored during operation, and
warnings are issued if the cooling water for some reason should stop.
Flow meters are placed on the feed, reux and distillate ows. These sensors
give visual feedback to the operator through displays on the sensors. They are
not used as measurements in the control system for two reasons: The squeezing
tube pumps produce pulsating ows which are below the measurement range of
the ow meters in parts of the oscillation period. Hence the measurement signal
is unsymmetrical and averaging or possibly a notch lter on the signal is not very
suitable. The other reason why the ow meters are not used in the controller, is
that especially the feed ow meter quite often gets stuck on a specic ow value.
The ow meters use the angle of a small pendulum as a measurement proportional
to mass ow rates. Small particles in the feed jam the pendulum in a certain

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position thereby making the measurement signal useless. Instead of using ow
meters, pump characteristics are used to give estimates of the actual feed and
reux ows.

2.3 Control loops

As mentioned there are two level control loops in the system. A conventional
LV-conguration is used where reux and vapor ows are used for composition
control, the level in the reux drum is controlled through the distillate ow, and
the boiler liquid level is controlled through the bottoms ow. Both of the level
controllers are P-controllers where suitable gains were found by trial and error.
Steady state level osets are unimportant in this conguration, which is why no
integral terms are included in the controllers.
If dangerous situations occur, an emergency switch is placed on the aluminum
frame. Pressing the emergency switch cuts the main power supply and the column
will be shut down. Dangerous situations happens very rarely, but the operator
should pay attention to especially boiler and reux drum holdup. If the boiler
level gets below the heating coils, the coils may get overheated and possibly ignite
the methanol gas, thereby causing an explosion. Another situation is if cooling
water stops; after a while the condensator will then not be suciently cooled to
condensate the distillate, possibly causing a gas leak.
With level loops closed, what is left to control are the compositions of the
bottoms and distillate ows. The operator's job is to make sure the composition
controller does this properly. Two dierent controllers are implemented; a conven-
tional diagonal PI-controller where reux is used to control distillate composition
and boilup is used to control bottoms composition, and a 2 × 2 H∞ controller
where both of the inputs are used to control both composition outputs together.

3 LabView User Interface

Figure 2 shows a screen shot of the operator interface for the control program.
The operator sees various controlled and manipulated variables in the left chart.
All the temperatures are displayed in the center chart, and the temperature prole
is displayed in the right chart.
In manual control mode, the operator can turn on and o the bottoms and
distillate pumps by pushing the buttons in the lower left part. Reux, heat and
feed can be set by typing in numerical values in the corresponding input dialogs.
These are the nominal inputs.
Nominal distillate and bottoms composition outputs (steady state outputs with
a given nominal input) are typed into the the elds ydnom and xbnom respectively.

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 Figure 2: User interface

Desired outputs (reference values) are typed into the elds labeled yddesired and
xbdesired .
In the box marked Activate controllers and reference lters, the operator
selects what kind of controller to use. Available options are: Open loop (manual
control), Level control, Composition control H∞ , and Composition control PI.
In open loop, the operator decides all actuator values. With level control, the
holdup in the reux drum and in the boiler is controlled using the distillate and
bottoms pump, but the operator is still in charge of reux, heat input and feed rate.
With composition control the two composition loops are closed, and the automatic
controller will compensate for osets between measured and desired compositions
using the reux and heat inputs. When using PI composition control, the two
composition loops for yd and xb can be closed independently.
Steps in desired compositions are low-pass ltered to avoid large actuator
changes. The lter can be initialized to the nominal values ydnom and xbnom by
pushing the button labeled initialize reference lter.
PI controller gains can be changed by the operator in the lower left dialog
boxes. The default controller gains are believed to be reasonably good.

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4 Operator instructions
Before you start, make sure the boiler is lled with water up to the black line, the
reux drum lled with methanol to just above where the glass begins and that
there is feed in the feed tank. If the boiler level is low, pump some feed into the
column. If the reux drum level is low, you will have to run the column with little
reux for a while. Pump all the distillate and bottoms one at a time back into the
feed tank using the recycle pump. Open the valve underneath the product tanks
and turn on the recycle pump pushing the green button on the door of the I/O
module enclosure. Close the valves and stir in the feed tank when nished. The
column is now ready to be used. If this is the rst time the column is used, and
all product tanks are empty you can rst ll the feed tank with 6 liters of water
which you pump directly into the column to ll the boiler. Then pour 10 liters of
methanol and 10 liters of water into the feed tank, and use this as feed.
Open the LabView program column.vi located in the folder C:\Documents
and Settings\Administrator\My Documents\destillasjonskollonne\column
control final. User name and password for the computer is Administrator/etanol.
Turn on cooling water, adjust the rate to 100-150liters/hour. Turn the boiler
on full power (3kW). Wait until it boils and the temperature starts rising in the
feed section, indicating that the vapor has reached the middle of the column. Then
turn on the feed pump, and set feed rate F=1ml/s. When the vapor reaches the
top temperature sensor, reduce boiler power to 1.5kW and turn on reux. Try a
reux rate of L=2ml/s. This takes around 15 minutes. Turn on level control.
Let the column settle for a few minutes and adjust the nominal boiler and reux
inputs to get as close as possible to the desired operating region. Increasing reux
increases top composition, increasing boiler input increases bottoms composition.
When you are satised, use the displayed composition estimates as nominal out-
puts. Set the desired composition outputs. There should not be a larger dierence
than 0.01 between nominal and desired composition. The composition estimates
is not accurate outside 0.94 < yd < 0.99, 0.005 < xb < 0.015, so select a desired
composition between these values and try to keep the system within these bounds
before turning on automatic control. Finally, turn on the composition controller.
Select either the H∞ controller or the PI controller. If using PI controller, you have
the option to close one loop at a time by activating each controller independently
with the corresponding on/o buttons. This is sometimes easier if the column is
relatively far away from the desired setpoints.
Problems may occur when switching from manual to automatic control. If
actual compositions are too far away from the desired compositions, or if there are
large temperature oscillations when turning on the controller, output saturation
is likely to occur. If the output saturates only for a short period of time (less
than 15sec) this may not be a problem, the controller will go into oscillations but

7
 Table 2: Start-up procedure for distillation column
Condition Operation to be done
Time = 0 Boiler input = 3kW
Cooling water > 100l/h
Feed ow = 0ml/s
Reux ow = 0ml/s
Temp4> 40◦ Feed ow = 1ml/s
◦
Temp1> 40 Boiler input = 1.5kW
Reux ow = 2ml/s
Level control on
Temp. settled Nominal compositions := actual compositions
Desired compositions := something not too far from nominal values
Composition control on

may be able to recover by itself. Wait and see if the time of saturation decreases,
if it does the transition from manual to automatic control will most likely be
successful. If on the other hand, saturation persists, eventually ooding will occur
or the reux drum will run empty. If this happens, turn of the controller, wait
for the column to settle with only nominal inputs and restart the controller, this
time with desired composition equal to actual composition. It may be necessary
to restart the program (push stop, then play) to initialize the controllers, more
specically to nullify the integrated error for integral action.

5 Data logging
Inputs to and outputs from the column during operation are logged to le data\columndata_x.dat
with x being an appended running number. This log le may be processed using
the matlab script readData.m, placed in the same folder, which reads the log le
and presents composition outputs and column inputs in plots. The le may easily
be changed to display other variables.

6 Source code
The program is divided into two parallel loops. One loop runs every 0.1 seconds
and writes actuator values to the column. This loop pulse width modulates the
actuator values to the boiler and the distillate and bottoms pump. The second
parallel loop is the main loop and runs every 2 seconds. This loop reads sensor
data, does the necessary scalings, calculates actuator values, presents signals to the

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 Figure 3: Control program ow sheet

operator and is responsible for logging data. A ow sheet for the control program
is presented in gure 3. The LabView block diagram showing the two loops is
shown in gure 4. The upper timed loop is the fast loop, while the lower one is
the slow loop. The slow loop is in the read sensor values state in the shown gure.

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Figure 4: User interface

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A I/O connections
Below follows a summary of equipment connected to the NI FieldPoint I/O mod-
ules.

Table 3: FieldPoint I/O connections

FP-AO-200
Channel 0 Heating coils, relay 1
Channel 1 Heating coils, relay 2
Channel 2 Heating coils, relay 3
Channel 3 Pump Distillate, relay
Channel 4 Pump Bottoms, relay
Channel 5 Pump Reux
Channel 6 Pump Feed
Channel 7
FP-AI-100
Channel 0 Flow meter, Reux
Channel 1 Flow meter, Distillate
Channel 2 Flow meter, Feed
Channel 3 Level sensor, reux drum
Channel 4
Channel 5 Boiler pressure sensor, bottom
Channel 6 Boiler pressure sensor, top
Channel 7
FP-RTD-124
Channel 0 Temperature 0 (top)
Channel 1 Temperature 1
Channel 2 Temperature 2
Channel 3 Temperature 3 (broken)
Channel 4 Temperature 4
Channel 5 Temperature 5
Channel 6 Temperature 6
Channel 7 Temperature 7 (boiler)

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References
[1] Jørgen K. Johnsen.Robust Distillaton Control - Application of H-innity
Loop Shaping, Master Thesis, NTNU, 2005

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