RUHR-UNIVERSITÄT BOCHUM

Lehrstuhl für Fluidverfahrenstechnik

Laboratory Course
Experiment: “Continuous Distillation”

Summer Semester 2017

Advisors: Mrs. Iris Rieth, M.Sc.

Mrs. Carolin Stegehake, M.Sc.

Room: IC 3/099

IC 3/113

Phone Number: +49 (0)234 / 32 – 25 849

+49 (0)234 / 32 – 260193

E-Mail: rieth@fluidvt.rub.de

stegehake@fluidvt.rub.de

Laboratory: IDN 02 / 751

1
Inhaltsverzeichnis
1. Introduction ....................................................................................................................... 3
2. Operating Principle of a Continuous Distillation Column .................................................... 3
2.1. Forming a two-phase System...................................................................................... 3
2.2. Mass Transfer across the Phase Boundary................................................................. 4
2.3. Separation of the two phases ...................................................................................... 4
3. Design of a Continuous Distillation Column ....................................................................... 4
4. Thermodynamic Fundamentals ......................................................................................... 5
4.1. Boiling und Equilibrium Diagram of Binary Systems .................................................... 5
4.2. Classification of Real Systems .................................................................................... 7
4.2.1. Ideal Mixtures ....................................................................................................... 7
4.2.2. Mixtures with Negative Deviation .......................................................................... 8
4.2.3. Mixtures with Positive Deviation ........................................................................... 9
5. Equilibrium-Stage Operations ...........................................................................................10
5.1 Concept of Equilibrium-Stage Operation .....................................................................10
5.2 Packed Columns .........................................................................................................11
6. McCabe-Thiele Design Method ........................................................................................11
6.1 Determination of the Equilibrium-Stages by Using the McCabe-Thiele-Method ...........12
6.1.1. Operating Line for the Rectification Section .........................................................12
6.1.2. Operating Line for the Stripping Section ..................................................................14
6.1.3. The Intersection Line/Feed Line ..........................................................................16
6.1.4. Construction of the McCabe-Thiele Diagram .......................................................19
7. Instructions .......................................................................................................................20
7.1. Preparation of the Experimental Setup .......................................................................20
7.2. Operation of the Software ..........................................................................................20
7.3. Experimental Procedure.............................................................................................23
8. Task Formulation ..............................................................................................................23
9. Special Safety Instructions ...............................................................................................24
10. Short Questions ..............................................................................................................24
11. Appendix ........................................................................................................................25
12. Literature ........................................................................................................................32

2
1. Introduction
Continuous distillation is widely used in the chemical process industry where large
quantities of homogeneous liquids need to be distilled. This operation yields products
of high purity, even if the system is difficult to separate. [1] Continuous distillation is
used when a simple distillation will not achieve a high enough product purity.

The task of this experiment is to investigate a continuous distillation of an ethanol/water

system.

2. Operating Principle of a Continuous Distillation Column

The principle of continuous distillation is the same as the principle of normal distillation.
It consists of three steps:

1. Forming a two-phase system

2. Mass transfer across the phase boundary
3. Separation of the two phases

1. Step 2. Step 3. Step

Figure 1: Principle of continuous distillation [7]

2.1. Forming a two-phase System

To separate a mixture of substances into its components, a second phase is required.

The separating component transfers into the second phase. The second phase is
generated by partially boiling the initial phase – this means to supply heat in the
vaporizer. Thereby, the mixture of substances is separated into a vapor and a liquid
phase.

3
2.2. Mass Transfer across the Phase Boundary

Mass transfer between the two phases is caused by disequilibrium of the substances
– a difference in the intensive variables. Due to the difference in boiling point
temperatures of the pure substances, the thermodynamic properties can be influenced
such that the components which have to be separated accumulate in different phases.
This effect is enhanced by intensive contact of the two phases and a large surface
caused by packing material.

2.3. Separation of the two phases

Mass transfer between the two phases leads to separation of the mixture into the vapor
and the liquid phase. The composition of the two phases is different: the vapor phase
mainly consists of lighter boilers and the liquid phase of higher boilers. By condensing
the vapor phase, there are two (liquid) output fractions in the distillation: the first one
at the upper part of the column with lighter boilers of high purity (depending on the
separation efficiency of the column) and the second one mainly with high boilers at the
bottom. Condenser

3. Design of a Continuous Distillation

Column overhead reflux divider
Reflux
In order to distinguish between the types of
Rectification

packing material, the Continuous Distillation overhead

section

product
Columns are called plate columns, distillation
tower or distillation columns. [2]
Feed
These designs can be operated as a batch or, Feed tray
like in this laboratory, as a continuous
distillation. Continuous distillation columns
Stripping
section

consist of a bottom part with a reboiler, a

separation column, and a head part with a Reboiler
reflux condenser and “reflux divider”. The lower
part of the column is called the stripping section
bottom
and the upper part is called rectification section.
bottoms product
The feed section with a preheater is located in
Figure 2: Continuous distillation column [3]

4
between the upper and the lower part. The schematic of a Continuous Distillation tower
is presented in Figure 2.

In the bottom part (sump) of the column, a section of the liquid is extracted and the rest
of it is partially vaporized and supplied to the stripping section again. In the stripping
section the reduction of the light boilers in the condensate phase takes place. In the
rectification section the enrichment of the lighter boilers, in the vapor phase, takes
place. The lighter boilers are partly removed after condensation as the head product
and partly recycled to the column. The reflux liquid gets in contact with the vapor and
leads to further mass transfer. The ratio between reflux and overhead product is
controlled by a reflux divider. With high reflux ratio, the residence time is increased.
Residence time is the average amount of time that the substances spend within the
column during mass transfer. The purity of the head product increases as residence
time increases.

4. Thermodynamic Fundamentals

To analyze the separation efficiency of a Continuous Distillation Column it is important

to understand some particular diagrams. The diagrams are based on theoretical
principles.

4.1. Boiling und Equilibrium Diagram of Binary Systems

In a mixture of a binary system there are specific intensive properties, e.g. composition
of liquids xi, composition of vapor yi and boiling temperature Ti. It is common to refer
the compositions of each phase to the lighter boiler “i”. The drawing of the related
properties into a diagram results in the boiling point diagram and the vapor-liquid
equilibrium diagram.

The boiling point diagram (Figure 3) shows how the equilibrium compositions of the
components in a liquid mixture vary with temperature at a fixed pressure. The boiling
point diagram consists of the bubble-point curve (bubble-point is the temperature at
which the liquid starts to boil) and the dew-point curve (dew point is the temperature at
which the saturated vapor starts to condense). With the boiling point diagram it is
possible to determine the composition of the liquid phase xi and the composition of the
vapor phase yi at different temperatures at a fixed pressure. Allowing the boiling point
and the dew point of a specific composition to be investigated.
5
 vapor

dew-point curve
two-phase

bubble-point curve
curvecurve
liquid

Figure 3: Boiling Point diagram [9]

The vapor-liquid-equilibrium diagram (Figure 4) expresses the bubble-point and the

dew-point of a binary mixture at a constant pressure. By using this diagram, the amount
of equilibrium stages (theoretical trays) of the column can be determined.

equilibrium line

Figure 4: Vapor-Liquid-Equilibrium Diagram [9]

6
4.2. Classification of Real Systems

4.2.1. Ideal Mixtures

Systems of ideal mixtures do not have any deviations from the ideal behavior. In this
case Raoult’s law is applicable – the partial vapor pressure pi of component i of an
ideal mixture of liquids is equal to the vapor pressure of the pure component 𝑝𝑖0
multiplied by its mole fraction 𝑥𝑖 in the mixture: [3]

𝑝𝑖 = 𝑝𝑖0 ∙ 𝑥𝑖 (1)

Dalton’s law is also applicable for the ideal case. It states that in a mixture of non-
reacting gases, the total pressure exerted is equal to the sum of the partial pressures
of the individual gases. [4]

𝑝𝐺𝑒𝑠 = ∑ 𝑝𝑖 (2)

Moreover, the partial pressures of the components of the mixture can be calculated by
the concentration of the component of the vapor phase and the total pressure:

𝑝𝑖 = 𝑦𝑖 ∙ 𝑝𝐺𝑒𝑠 (3)

The linear behavior of the partial pressures for ideal systems is shown in the vapor
pressure diagram (Figure 5, left). The bubble point diagram (Figure 5, middle) features
the typical boiling point curve. This diagram shows the dependence of phase
transitions of a mixture on temperature and composition. The vapor-liquid-equilibrium
diagram (Figure 5, right) is typically determined experimentally but for ideal binary
mixtures it can be calculated by knowing the separation factor α. The separation factor
characterizes the separation behavior of an ideal binary system and describes the ratio
of the ratios of the vapor-liquid-composition of the pure components A and B:

𝑦𝐴 𝑦𝐴 𝑝𝐴
⁄𝑥𝐴 𝑥𝐴 ∙ 𝑝𝐺𝑒𝑠 ⁄𝑥 𝑝𝐴0
𝛼=𝑦 =𝑦 =𝑝 𝐴 = 0 (4)
𝑥𝐵 𝑝𝐵
𝐵⁄ 𝐵 𝐵⁄
𝑥𝐵 𝑥 ∙ 𝑝𝐺𝑒𝑠
𝐵

7
The vapor-liquid-equilibrium curve for ideal mixtures is determined by Dalton’s law,
Raoult’s law and the separation factor:

𝛼 ∙ 𝑥𝐵
𝑦𝐴 = (5)
1 + 𝑥𝐴 ∙ (𝛼 − 1)

Many real component systems deviate from the ideal behavior. These systems are
divided into two categories, depending on the trend of deviation.

4.2.2. Mixtures with Negative Deviation

If the real partial pressures of the components in the mixture are lower than the (ideal)
partial pressures calculated by Raoult’s law, the mixture is called “mixture with negative
deviation” (Figure 5).

This behavior results in a vapor pressure minimum shown in the vapor-pressure

diagram and a temperature maximum shown in the boiling point curve. The
composition of the mixture in the extreme value is called azeotrope: the boiling
temperature of the azeotrope of a mixture with temperature maximum is higher than
the boiling temperature of the single components. For the continuous distillation it
means in fact that the lighter boilers vaporize first (mainly). The temperature increases
to the boiling point of the azeotrope and then the remaining mixture vaporizes as an
azeotrope. Thereby the liquid and vapor phase have the same composition – the
phases cannot be more purified by a simple distillation.

8
4.2.3. Mixtures with Positive Deviation

For mixtures with positive deviation there are the same considerations applied as for
the ones with negative deviation. The effects concerning maximum and minimum are
reverse. The boiling temperature of the azeotrope is lower than the boiling temperature
of the single components. The azeotrope vaporizes first (mainly). A complete
separation of this mixture is not possible by using a simple distillation.

vapor pressure diagram boiling point diagram equilibrium diagram

ideal mixtures

negative
deviation

positive
deviation

Figure 5: vapor pressure diagram, boiling point diagram, equilibrium diagram for the three
classifications of real systems [9]

9
5. Equilibrium-Stage Operations

The number of equilibrium-stages and the reflux ratio (equation 10) of a distillation
column, for a certain separation task, are important characteristics used to estimate
investment and operation costs.

5.1 Concept of Equilibrium-Stage Operation

The definition of equilibrium-stages was once established for columns that used trays
as packing material. Mass transfer in tray columns takes place spatially, separated by
each tray, and not steadily over the whole column. The highest enrichment of a
component on an ideally operated tray is characterized by the equilibrium-stage, if the
following conditions are fulfilled:

1. Ideal mixing of the liquid

2. Ideal heat and mass transfer between vapor and liquid
3. Vapor is dry saturated – no liquid droplets are drawn along.

condenser

Reflux

3. Tray
re-cooler

distillate
2. Tray F4

1. Tray

Figure 6: Vapor and liquid Hold-up on the different trays [3]

The number of equilibrium stages is determined by using the McCabe-Thiele method

with the required purity of the products as described in section 6.

10
5.2 Packed Columns

Packing material is used to minimize pressure losses in case of high separation effects.
To transfer the theory of equilibrium-stages to packed columns, the HETP-value
(height equivalent to one theoretical plate) is defined [6]:

𝑙𝑒𝑛𝑔𝑡ℎ 𝑜𝑓 𝑝𝑎𝑐𝑘𝑖𝑛𝑔 𝑚𝑎𝑡𝑒𝑟𝑖𝑎𝑙 𝑙𝑎𝑦𝑒𝑟

𝐻𝐸𝑇𝑃 = (6)
𝑛𝑢𝑚𝑏𝑒𝑟𝑠 𝑜𝑓 𝑒𝑞𝑢𝑖𝑙𝑖𝑏𝑟𝑖𝑢𝑚 − 𝑠𝑡𝑎𝑔𝑒𝑠

liquid vapor

Figure 7: Examples of packing material

6. McCabe-Thiele Design Method

The McCabe-Thiele method is used to graphically examine the function of a distillation

column for binary systems, such as the one in the laboratory (ethanol and water). This
method is based on the vapor-liquid-equilibrium data and it assumes constant molar
overflow which implies that: [5]

- Molar heats of vaporization of the components are roughly the same

- Heat effects (heats of solution, heat losses to and from column, etc.) are
negligible
- For every mole of vapor condensed, 1 mole of liquid is vaporized

11
6.1 Determination of the Equilibrium-Stages by Using the McCabe-Thiele-
Method

The design procedure is simple. Given the vapor-liquid-equilibrium diagram of the

binary mixture, operating lines are drawn first. Operating lines define the mass balance
relationships between the liquid and vapor phases in the column. There is one
operating line for the bottom (stripping) section of the column, and one for the top
(rectification or enriching) section of the column. The use of the constant molar
overflow assumption also ensures the operating lines are straight lines. [6]

6.1.1. Operating Line for the Rectification Section

The operating line for the Rectification Section is based on the following relations.

The mass balance of the total flow and of the flow of the lighter boiler component lead
to the following relations according to Figure 8:

𝐺̇ = 𝐿̇ + 𝐾̇ (7)

𝐺̇ ∙ 𝑦 = 𝐿̇ ∙ 𝑥 + K̇ ∙ 𝑥𝐾 (8)

Figure 8: mass-balance rectification section [7]

Solving equation (8) for 𝑦 results in equation (9):

𝐿̇ 𝐾̇
𝑦= ∙ 𝑥 + ∙ 𝑥𝐾 (9)
𝐺̇ 𝐺̇

12
The reflux ratio 𝑣 – the ratio of the reflux flow 𝑅̇ to the distillate flow 𝐾̇ – leads to
equation (10):

𝑅̇
𝑣= (10)
𝐾̇

Substituting equation (7) in equation (9) and expanding the fractions results in equation
(11):

𝐿̇⁄ 𝐾̇⁄
𝐿̇ 𝐾̇ 𝐾̇ 𝐾̇
𝑦= ∙𝑥+ ∙ 𝑥𝐾 = ∙𝑥+ ∙ 𝑥𝐾 (11)
𝐿̇ + 𝐾̇ 𝐿̇ + 𝐾̇ 𝐿̇⁄ + 𝐾̇⁄ 𝐿̇⁄ + 𝐾̇⁄
𝐾̇ 𝐾̇ 𝐾̇ 𝐾̇

Substituting equation (10) in equation (11), in consideration of 𝐿̇ ≈ 𝑅̇ results in the

operating line for the rectification section (12):

𝑣 1
𝑦= ∙𝑥+ ∙𝑥 (12)
𝑣+1 𝑣+1 𝐾

A complete reflux (𝐾̇ = 0) is expressed in equation (13) based on equation (8).

𝐺̇ ∙ 𝑦 = 𝐿̇ ∙ 𝑥 (13)

Using the relation of the incoming amount of vapor to be equal to the outcoming
amount of liquid, the operating line for complete reflux is according to equation (14):

𝑦=𝑥 (14)

The operating line for complete reflux is equivalent to the diagonal line of the vapor-
liquid-equilibrium diagram.

The operating line for the rectification section with a certain reflux ratio is constructed
as follows. First the desired top product composition is located on the vapor-liquid-
equilibrium diagram, and a vertical line drawn until it intersects the diagonal line. A line
from this intersection point is drawn to the y-axis intercept according to equation (16),
as shown in Figure 9. [6]

𝑥 = 𝑥𝐾 (15)

𝑥𝐾 (16)
𝑦=
𝑣+1

13
6.1.2. Operating Line for the Stripping Section
The operating line for the stripping section is constructed in a similar manner.

equilibrium
line
rectification
line

Figure 9: rectification line in vapor-liquid-diagram

The mass balance of the total flow and the lighter component make up the system
boundary of the stripping section, and results in equations (17) and (18) according to
Figure 10. 𝑆̇ is the extracted liquid in the bottom part of the distillation column.

𝐿̇∗ = 𝐺̇ ∗ + 𝑆̇ (17)

𝐿̇∗ ∙ 𝑥 ∗ = 𝐺̇ ∗ ∙ 𝑦 ∗ + 𝑆̇ ∙ 𝑥𝑆 (18)

Figure 10: mass balance stripping section [7]

14
Analogous to the operating line for the refraction section results the operating line for
the stripping section in equation (19):

∗
𝐿̇∗ 𝑆̇
𝑦 = ∙ 𝑥∗ − ∙ 𝑥𝑆 (19)
𝐿̇∗ − 𝑆̇ 𝐿̇∗ − 𝑆̇

The starting point for the construction is the desired bottom product composition
(equation 20) on the x-axis. A vertical line is drawn from this point to the diagonal line,
and a line of slope β according to equation (21) as illustrated in the diagram in Figure
11.

𝑥 = 𝑥𝑆 (20)

𝐿̇∗
tan 𝛽 = (21)
𝐿̇∗ − 𝑆̇

equilibrium
stripping line
line

Figure 11: stripping line in vapor-liquid-diagram

The intersection point of the operation line for the rectification section changes based
on the state of the feed and the slope of the operation line for the stripping section.

15
6.1.3. The Intersection Line/Feed Line
A separation of a mixture by continuous distillation is possible if the operating line for
the rectification section and the stripping section intersect at a point below the vapor-
liquid-equilibrium line. The thermal state of the feed influences the liquid and the vapor
flow in the feed-section of the column which results in the intersection point of the
operating lines. [6]

However, if the feed composition is saturated liquid, the vapor flow does not change
but the liquid flow in the lower part of the column increases. If the feed composition is
saturated vapor, the vapor flow increases. [5] Figure 12 shows the influence of the
thermal state of the feed on the internal flows of the column.

a) subcooled liquid e>1

b) saturated liquid e=1
c) mix of liquid and vapour 0<e<1
d) saturated vapour e=0
e) superheated vapour e<0

Figure 12: influence of the condition of feed on vapor and liquid flows in feed section [5]

The condition of the feed can be deduced by the slope of the feed line or e-line. The
e-line is drawn between the intersection of the operating lines, and shows where the
feed composition lies on the diagonal. e is the caloric factor, and represents the ratio
of the feed that flows downward through the column as a liquid. (1-e) is the ratio of the
feed that flows upward through the column as a vapor. [8]

The heat balance around the feed section results in equation (22):

ℎ𝐹′ − ℎ𝐹
𝑒 =1+ (22)
∆ℎ𝑣

ℎ𝐹 is the molar enthalpy of the feed, ℎ𝐹′ is the molar enthalpy of the boling liquid and
∆ℎ𝑣 the molar evaporation enthalpy.

16
The intersection line is determined by using the caloric factor and the heat balance
around the feed section:

𝑒 1
𝑦= ∙𝑥− ∙𝑥 (23)
𝑒−1 𝑒−1 𝐹

Figure 13 shows the vapor-liquid-equilibrium diagram with the intersection line and the
resulting intersection with the rectification line and stripping line.

equilibrium
line
intersection
line

stripping
line
compound of vapor

rectification
line

compound of liquid
Figure 13: Intersection line in vapor-liquid-diagram [8]

The intersection line intersects the diagonal line according to equation (24):

𝑥 = 𝑥𝐹 (24)

The intersection of the intersection line with the x-axis results in equation (25):
𝑥𝐹
𝑥= (25)
𝑒

17
The intersection lines for the various feed conditions are shown in Figure 14.

Table 1: Examples of various feed conditions [2]

Example state of feed e-factor

1 superheated vapour <0

2 saturated vapour =0

3 mix of liquid and vapour 0<e<1

4 saturated liquid =1

5 subcooled liquid >1

Figure 14: Insection line in depency on

thermical feed conditions (qualitative). [8]

18
6.1.4. Construction of the McCabe-Thiele Diagram

The McCabe-Thiele method assumes the equilibrium between the liquid on a tray and
the vapor above it. Using the constructed operation line for the used reflux ratio and
the thermal state of the feed for a certain separation as described above, the required
number of theoretical stages is graphically determined as a stage-construction, shown
in Figure 15. The construction begins with a horizontal line from the intersection point
of rectification line and diagonal line to the vapor-liquid-equilibrium line. A vertical line
follows to the operation line. The construction of horizontal and vertical lines between
operation line and vapor-liquid-equilibrium line repeated until the vertical line intersects
the diagonal line. The resulting trays are equivalent to the necessary trays of a
distillation column with respect to the number and composition of liquid and vapor
phase. [6]

equilibrium
line
compound of vapor

rectification
line

compound of liquid

Figure 15: Stage construction in McCabe-Thiele-Diagram

19
7. Instructions

This chapter describes the procedure of the experimental setup. A flow chart and
process picture of the distillation column are shown in the appendix.

7.1. Preparation of the Experimental Setup

The following aspects have to be denoted to startup the distillation column:

1. Switch on the Refractrometer

The weight proportions of the head and bottom product are determined by the
refractive index. The refractive index is measured by a refractrometer.

2. Open the coolant valve

The cooling water of the whole plant is run in a closed loop. The water tap is on
the wall behind the distillation column. The coolant flow has to be high to ensure
a sufficient cooling capacity. Inside of the stainless steel tray below the plant,
there is a flow controller to check the flow.

3. Switch on the Main Switch

The power supply of the plant is ensured by the box on the left of the plant. The
Main Switch has to be turned on.

4. Turn on the Computer

Temperature and pump settings are controlled by a software on the computer.
The computer is located on the left of the power box. After booting the computer,
log in with the user name “user” and the password “user”.

7.2. Operation of the Software

The software opens automatically after logging in on the computer. By clicking the left
mouse button of the user interface, the process picture (Figure 22) shows up. Each
required numerical value has to be confirmed by pressing “Enter”. Activated buttons
are flashing green.

20
1. Voltage Supply
By pressing the button „230 V” of the control panel
(Figure 16), the voltage supply of the pumps and of the
heaters are released. Not until the release occurred,
heater and pumps can be started. The status of the
emergency shut-off which is located on the power box is
symbolized by a small triangle.
Figure 16: Voltage
Abbildung
supply 1:
Allgemein
2. Sump Temperature
The sump of the column is heated by
two quartz crystal heater. The desired
temperature is entered by a left-click
on “Feld 1” in the operating field
“Regelung Sumpftemperatur” (Figure
17). By pressing the button “Temp.
Figure 17: Sump Temperature
Sumpf” the heater of the sump is
turned on and the button flashes green.
The automatic control of the sump temperature may have oscillations.
Therefore, a manual control of the sump temperature is recommended. To
activate the manual control, the button “Manuell” has to be clicked and the
desired power in % has to be entered in “Feld 2” (Figure 17).
The heating of the sump switches off automatically, if the filling level of the sump
tank B01 is dropping below or above the minimum or maximum height.

3. Sump Pump
To keep the filling of the sump tank constant during operation
and to determine the concentration of the components in the
sump, a sample has to be taken. The flow of the sump is
controlled by the gear pump P02. The power of the pump is Figure 18: Sump
pump
entered in “Feld 3” (Figure 18). The pump is turned on by
pressing the button “Start P02” so that the liquid is pumped into tank B04.

21
4. Feed Temperature
The temperature of the feed is controlled by the preheater.
The preheater is heated by a quartz crystal heating rod. The
power is controlled, appropriate to the power of the sump
pump, automatically or manually in the operating field
“Regelung Vorheizer” (Figure 19). The automatic control is
started by pressing the button “Start Temp.”. The desired
temperature can be entered in “Feld 4” (figure 18). The
Figure 19: Feed
manual control is activated by pressing the button “Manuell”. Temperature
The power of heating can be entered in “Feld 5”. The current
temperature is shown in “Feld 4”. Note that the preheater is active just if the feed
pump P01 is switched on!

5. Feed Pump
The feed is supplied to the distillation column by a
reciprocating pump. The unit of the pumping capacity is
1/min. The maximum pumping capacity is 180 1/min. By
pressing the button “Start P01” (Figure 20), the pump is
Figure 20: Feed
started. The desired pumping capacity is entered in „Feld 6“ pump
(Figure 20).

6. Reflux Separator
The reflux separator works electrically and is
controlled by the operation field „Rücklaufteiler“
(Figure 21). If the reflux separator is turned off,
the condensate flows back into the column
completely (reflux = infinity). Activating the Figure 21: reflux separator
button “Automatik” turns on the automatic control of the reflux separator, which
switches between supply pipe and return pipe. The value in “Feld 7” shows the
time in which the condensate (as a product) flows from the column into the tank
B03 (Figure 23). „Feld 8“ shows the time in which the condensate is fed back to
the column. The example in Figure 21 expresses a reflux ratio of 𝑣 = 5⁄1. If the
reflux separator is turned on, the button „Automatik“ flashes green. The

22
 extraction of condensate with infinite reflux occurs with activating the button
„Abnahme“.

7.3. Experimental Procedure

After preparation of the plant and refractrometer, as shown in chapter 7.1, it is possible
to start the experiment. First, the feed has to be prepared by using a balance. The
refractive index and the mass fractions of the solution have to be determined. Then the
solution is filled into the column and the desired sump temperature must be set. The
sump heater cannot be turned on if the fluid level is too low or too high. In these cases
the sump tank has to be filled or flushed. As soon as the vapor starts condensing, the
supply feed can flow, the desired reflux ratio can be set, and the reflux separator can
be turned on. Depending on the parameters and the mass fractions of the feed, the
distillation process becomes steady-state (equilibrium state) after 40-45 minutes. The
samples of the head product are taken from tank B03. The samples of the sump
product are taken from tank B04 (Figure 23). The refractive indices have to be
determined directly after extraction due to the high volatility of ethanol. It is necessary
to take three samples of each operating condition at intervals of seven minutes. Finally,
pumps and heater are turned off. The coolant is not turned off until the column is cooled
down.

8. Task Formulation

The number of equilibrium stages is supposed to determine for the following

operating conditions:

Sump Temperature: 92- 93°C

Feed Flow: 60 min-1

Reflux Ratios: (∞); (5:1) ; (5:2) ; (2:5)

Feed Composition:

1. Mass fraction of Ethanol in Feed:

- 30%
Thermical State of Feed::
- Subcooled Liquid (23°C)

23
9. Special Safety Instructions

 During operation the plant gets hot. There is danger of burning!

 There is risk of shock from the electrical components of the plant. Avoid liquids
coming into direct contact with electronics!
 Ethanol is highly flammable – avoid ignition sources!
 Operate at atmospheric pressure! Negative pressure caused by vacuum pump
P03 (Figure 23) may lead to implosion. The vacuum pump must not be used
during the experiment!

10. Short Questions

1. Draw the schematic layout of a distillation column.

2. Explain the functional principle of a distillation column.
3. Which diagram shows the composition of the vapor and liquid phase (at
constant pressure)?
4. How are mixtures classified?
5. Which laws describe the behavior of these mixture?
6. What is an azeotrope?
7. What kind of column types exist?
8. How are the different column types designed?
9. Explain the McCabe-Thiele method for the determination of the number of
equilibrium stages by using the x,y-diagram.
10. Does the feed state have an influence on the distillation?
11. Which function does the reflux ratio in a distillation column have?
12. Which property is measured by a refractometer?

24
11. Appendix

Figure 22: Process picture of the used distillation column

25
Figure 23: Flow sheet of the used distillation column

26
 boiling-point diagram Ethanol-Water
100°C
bubble-point curve
dew-point curve

95°C

90°C
temperature

85°C

80°C

75°C
0% 10% 20% 30% 40% 50% 60% 70% 80% 90% 100%
mass percent Ethanol

27
28
Table 2: refracting index at various mass percent ethanol

measurement 1 measurement 2 measurement 3

mass%
Ethanol refracting index Temperature refracting index Temperature refracting index Temperature

100% 1,362 19,1 1,363 19,0 1,363 18,8

90% 1,364 19,5 1,364 19,1 1,364 19,0

80% 1,364 19,5 1,364 19,5 1,364 18,9

70% 1,364 19,9 1,364 19,6 1,364 19,4

60% 1,363 20,0 1,363 19,8 1,364 19,8

50% 1,360 20,1 1,360 20,0 1,360 19,9

40% 1,358 20,4 1,358 20,5 1,358 20,6

30% 1,353 20,4 1,352 20,6 1,352 20,8

20% 1,347 20,2 1,346 20,5 1,346 20,8

10% 1,344 19,4 1,342 19,7 1,342 20,0

0% 1,332 19,8 1,332 19,9 1,332 19,8

Azeotropic point
xETOH=95,6%

Table 3: enthalpie

Enthalpie
temperature pressure
30 mass% Ethanol in Water
[°C] [bar] [kJ/kg]
23,0 0063,16
84,0 0310,53
1
86,0 0595,00
95,7 2198,92

29
 equilibrium diagramm Ethanol-Water
1

0,9

0,8 Azeotropic point

xETOH=95,6%

0,7
mass percent Ethanol in vapor

0,6

0,5

0,4

0,3

0,2

0,1

0
0 0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9 1
mass percent Ethanol in liquid
30
Table 4: vapor-liquid equilibrium for the system ethanol-water

pressure [bar] temperature [°C] Mass percent ethanol in water

liquid vapor
99,6288479 0 0
96,7856255 0,025 0,2328148
94,4820698 0,050 0,3689599
92,5789585 0,075 0,4582788
90,9818473 0,100 0,5213259
89,6255695 0,125 0,5681531
1 88,4629583 0,150 0,6042613
87,4587360 0,175 0,6329184
86,5875692 0,200 0,6561343
85,8251803 0,225 0,6753756
85,1555691 0,250 0,6915564
84,5647358 0,275 0,7053575
84,0409024 0,300 0,7172811
83,5743468 0,325 0,7277075
83,1564579 0,350 0,7369322
82,7801245 0,375 0,7451902
82,4388467 0,400 0,7526721
82,1271245 0,425 0,7595370
81,8400134 0,450 0,7659200
81,5730689 0,475 0,7719388
81,3224578 0,500 0,7776987
81,0845689 0,525 0,7832957
80,8563466 0,550 0,7888201
80,6350688 0,575 0,7943585
80,4184022 0,600 0,7999961
80,2043466 0,625 0,8058186
79,9913466 0,650 0,8119140
79,7781799 0,675 0,8183741
79,5641799 0,700 0,8252969
79,3491799 0,725 0,8327880

31
 79,1337354 0,750 0,8409632
78,9190687 0,775 0,8499508
78,7073465 0,800 0,8598947
78,5019576 0,825 0,8709582
78,3077353 0,850 0,8833278
78,1312909 0,875 0,8972188
77,9797353 0,900 0,9128930
77,8699575 0,925 0,9306173
77,8160686 0,950 0,9507564
77,8406798 0,975 0,9737210
77,9763464 1 1

12. Literature

[1] R. Perry und D. Green, Perry's Chemical Engineers' Handbbok, McGraw-Hill, 1984.

[2] H. Bockhorn, „Versuchsbeschreibung zum Chemisch-Technischen Grundpraktikum,“

Universität Karlsruhe.

[3] P. Perrot, A to Z of Thermodynamics, Oxford University Press, 1998.

[4] M. Silberberg, Chemistry_ the molecular nature of matter and change, Boston: McGraw-
Hill, 2009.

[5] M. Baerns, Technische Chemie, Wiley-VCH, 2006.

[6] M. T. Tham, „Distillation,“ 1997. [Online]. Available:

http://www.istitutofermiverona.it/LEZIONI/distil/distildes.htm. [Zugriff am 22 02 2016].

[7] J. Apelt, „Thermische Verfahrenstechnik,“ Hochschule Fulda, 2009.

[8] D. Christen, Praxiswissen der chemischen Verfahrenstechnik, Springer, 2009.

[9] „Praktikum Grundoperationen,“ Universität Paderborn.

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