CE 620 LIQUID-LIQUID EXTRACTION

3 Description of the device

3.1 Objective of the extraction, designation of the substances involved

The main objective of liquid-liquid extraction is

to transfer a transition component from a liquid
mixture into a liquid solvent.

The substances involved in liquid-liquid

extraction have various common names. This
can easily give rise to misunderstandings,
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especially when comparing different sources.

Therefore, we shall explain here which
designations are used in these experiment
instructions. More detailed information will follow
in Chapter 4, Page 59ff.

The simplest form of liquid-liquid extraction

involves three liquids:
• Transition component
• Carrier liquid
• Solvent

The liquid mixture of the transition component and

carrier liquid is called the feed. In the feed, the
transition component is dissolved in the carrier
liquid.
Carrier liquid and solvent together form the
solvent system. The transition component must
be soluble in both the carrier liquid and the
solvent.
The carrier liquid and solvent should together
form a phase boundary in order to allow the
separation of the two phases. Therefore, carrier

3 Description of the device 15

CE 620 LIQUID-LIQUID EXTRACTION

liquid and solvent should be as mutually insoluble

in each other as possible.
The two phases, which we get at the end of
liquid-liquid extraction are called the extract
and the raffinate.
The extract is essentially a solution of the transition
component in the original solvent.
The raffinate is essentially the original feed, less
the extracted proportion of the transition
component.

3.2 Process diagram

Fig. 3.1, Page 17 shows the process diagram for

the CE 620 liquid-liquid extraction unit.
The identification letters used are explained in
Chapter 6.4, Page 117f.
All main components and measuring points are
shown and labelled in the process diagram. The
flow through the trainer is illustrated.
More detailed information on the design of the
device and its functions follows in Chapter 3.3
and Chapter 3.4.
These chapters also use extracts from the
process diagram to illustrate details.

16 3 Description of the device

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Media

Fig. 3.1
Feed CE 620
Solvent
Extract
Raffinate
Residue
Distillate
Cold water

3 Description of the device

Main components
B1 Solvent tank
B2 Distillate tank
B3 Extract tank
B4 Raffinate tank
B5 Feed tank
D1 Round-bottomed flask
H1 Heating mantle
K1 Extraction column
K2 Distillation column
P1 Solvent pump
LIQUID-LIQUID EXTRACTION

P2 Feed pump
P3 Vacuum pump
W1 Distillation bridge
F1 Strainer
V1-V4 Control valve
V5, V6 Relief valve

Process diagram of the CE 620 liquid-liquid extraction system

V7, V8 3-way ball valve
V10-V30 Valve

Measurement and control

FI01 Solvent flow
FI02 Feed flow
LI01-LI05 Fill level
PI01, PI02 Pressure
TI01 Residue temperature
TI02 Vapour temperature
TIC1 Temperature controller

17
CE 620 LIQUID-LIQUID EXTRACTION

3.3 Device design

Front view
6 5 4 3

2
8

10
1

Rear view

11 12 13 14 15 16 17

1 Distillate tank (B2) 11 Heating mantle (H1)

2 Control cabinet 12 Regulating valve for solvent return (V3)
3 Regulating valve for solvent inflow (V1) 13 Solvent tank (B1)
4 Regulating valve for feed inflow (V2) 14 Feed tank (B5)
5 Extract tank (B3) 15 Raffinate tank (B4)
6 Regulating valve for feed return (V4) 16 Feed pump (P2)
7 Distillation bridge (W1) 17 Solvent pump (P1)
8 Distillation column (K2)
9 Extraction column (K1)
10 Round-bottomed flask (D1)

Fig. 3.2 Overview of the CE 620 liquid-liquid extraction system

18 3 Description of the device

 CE 620 LIQUID-LIQUID EXTRACTION

3.4 Device function and main components

This chapter is divided into several subsections.

Firstly, we will look at the trainer's different
operating modes (continuous mode and batch
mode). In doing so, we will describe the process.
Then, we will explain the structure of the
extraction column K1 (9).
Then we will explain how the phase boundary is
set up in the extraction column.
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Finally, we will describe the distillation unit.

The numbers in brackets in the following text

refer:
• mainly to the position numbers in the overview
in Fig. 3.2, Page 18, as well as
• occasionally to the labels in the process
diagram in Fig. 3.1, Page 17. This applies to
those components that are only illustrated in
the process diagram (some of the valves and
instrumentation).
Wherever the function of the components is
meant to be emphasised, both are added: first the
label according to the process diagram, then the
position number in brackets.

3 Description of the device 19

CE 620 LIQUID-LIQUID EXTRACTION

3.4.1 Operating mode and process description

The CE 620 trainer can be operated either

continuously or in batch mode (i.e.
discontinuously).
The desired operating mode is selected using the
3-way ball valves V7 and V8. The photo opposite
shows V7 and V8 in the front view.

The following subsections describe the two

operating modes using variations of the process
diagram from Fig. 3.1, Page 17.
In these variations of the process diagram, thicker
line widths denote the pipelines which are flowed
through. In addition, the flow through the tank
involved and through the extraction column is
Fig. 3.3 3-way ball valves V7 and V8 colour coded.

3.4.1.1 Batch mode

Fig. 3.4, Page 21 shows the variation of the

process diagram for batch mode, without
distillation.

20 3 Description of the device

 CE 620 LIQUID-LIQUID EXTRACTION
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Media
Feed
Solvent

Fig. 3.4 CE 620 process diagram, batch mode variant, without distillation

On the names of the materials and material flows

in batch mode:
The naming of materials and material flows for
batch mode requires some explanation.

3 Description of the device 21

CE 620 LIQUID-LIQUID EXTRACTION

Key facts:
• At the beginning of extraction, solvent is
located in the solvent tank.

Feed
• At the beginning of extraction, feed is located in
return the feed tank.
• After extraction, extract is located in the solvent
tank.
• After extraction, raffinate is located in the feed
tank.
But how long does extraction have to last to get
extract from solvent and raffinate from feed?
In these experiment instructions, the name
corresponds to the colour coding in Fig. 3.4,
Page 21, for batch operation during extraction.
The point where solvent is renamed as extract
and feed as raffinate is known as extraction end.

Process description for batch mode, without

distillation:
The mass transfer of liquid-liquid extraction takes
place in the extraction column K1(9). This is
where feed and solvent meet. When this
Solvent
return happens, a part of the transition component is
Solvent inflow

Feed inflow

extracted from the feed into the solvent.

Fig. 3.5 CE 620 process diagram,
extraction column section
Fig. 3.5 shows the extraction column K1, as an
excerpt from the process diagram in Fig. 3.4,
Page 21.
The feed is continuously pumped from the feed
tank B5(14) by the feed pump P2(16) into the
bottom of the extraction column (feed inflow).
The feed moves upwards in the extraction
column.

22 3 Description of the device

 CE 620 LIQUID-LIQUID EXTRACTION

From the top of the extraction column the feed

returns to the feed tank (feed return).
The solvent is continuously pumped from the
solvent tank B1(13) by the solvent pump
P1(17) into the top of the extraction column
(solvent inflow). The solvent moves downwards
in counterflow to the feed. From the bottom of
the extraction column, the solvent returns to the
solvent tank (solvent return).
The driving force for the counterflow is the
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density difference between solvent and feed.

Therefore, the material and/or the mixture with the
lower density must be pumped into the bottom of
the extraction column.
This condition is satisfied for the recommended
Quick couplings
rapeseed oil-ethanol-water model material
system. The density of the feed (solution of
ethanol in rapeseed oil) is less than the density of
the solvent (water).
If this condition is not satisfied for any possible
alternative material system that you may have
chosen, then the trainer can be adapted
accordingly.
Quick couplings

Colour coded quick couplings are installed for

this adaptation (see Fig. 3.6). These can be
uncoupled and both the inflows (feed inflow and
solvent inflow) and the returns can be swapped
with each other.
The colour coding helps when you have to restore
Fig. 3.6 Quick couplings
the normal state again (coupling and plug nipple
of the same colour belong together).

3 Description of the device 23

CE 620 LIQUID-LIQUID EXTRACTION

The tanks B1-B5 are available for feed, solvent,

raffinate, extract and distillate. These tanks
have a level indicator (LI01-LI05) in addition to
the drainage and the necessary inlet and outlet
nozzles. The tanks B1 and B3-B5 have a
removable lid.
The distillate tank B2(1) is designed with a
screwed lid and seal (see Fig. 3.7). This seal
allows distillation at reduced pressure.
Solvent pump P1(17) and feed pump P2(16)
Fig. 3.7 Distillate tank B2(1),
top view are designed as positive displacement pumps.
Recirculation lines are provided in order to allow
adjustment of the desired flow rates and to protect
the pumps. The pumps are also protected by
internal relief valves.
The following figure uses the solvent system to
illustrate the principle (excerpt from the process
diagram in Fig. 3.4, Page 21).
Solvent inflow

Solvent return

Recirculation

Fig. 3.8 Excerpt from the process diagram, solvent system

24 3 Description of the device

 CE 620 LIQUID-LIQUID EXTRACTION

When unthrottled and with free run-off, the solvent

pump delivers with maximum flow rate. The flow
rate is reduced by the counter pressure in the
extraction column K1. In addition, flow can be
throttled using the regulating valve V1. The
relief valve V5 starts when the corresponding
response pressure is reached. From the relief
valve, the excess solvent returns to the solvent
FI01
tank B1(13) via the recirculation line. The actual
solvent flow rate is thus divided into the desired
flow to the extraction column and the excess back
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Float into the solvent tank.

The flow measurement (FI01) and throttling
V1 (regulating valve V1) functions are combined in
a single component (see photo opposite). FI01 is
designed as a variable-area flowmeter.

Fig. 3.9 Flow meter FI01

with regulating valve V1 The valve V27 is used to vent the suction line in the
event of any suction problems.

The valve V29 is used for emptying, cleaning and

rinsing the extraction column and solvent system

3.4.1.2 Continuous mode

Fig. 3.10, Page 26 shows the variation of the

process diagram for continuous mode, without
distillation.

3 Description of the device 25

CE 620 LIQUID-LIQUID EXTRACTION

Media
Feed
Solvent
Extract
Raffinate

Fig. 3.10 CE 620 process diagram, continuous mode variant, without distillation

26 3 Description of the device

 CE 620 LIQUID-LIQUID EXTRACTION

The process description is largely similar to the

process description for batch mode (see
Chapter 3.4.1.1, Page 20ff).
The key difference is that in continuous mode,
only a single cycle of feed and solvent through the
extraction column K1(9) takes place.
The solvent return goes directly into the extract
tank B3(5) as extract. The feed return goes
directly into the raffinate tank B4(15) as raffinate.
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By comparison, in batch mode multiple cycles of

feed and solvent are possible.
Therefore, in batch mode we usually obtain a
better mass transfer and a higher concentration
of the transition component in the extract.

3 Description of the device 27

CE 620 LIQUID-LIQUID EXTRACTION

3.4.2 Extraction column

The cylinder of the extraction column K1(9) is

transparent to allow the process to be observed.
The cylinder is made of borosilicate glass.
During extraction, solvent and feed flow through
the extraction column in counterflow.
Head

The feed passes through a guide pipe into the

bottom of the extraction column. The exiting feed
Distributor
pipe flow is directed upwards. This supports the lift of
the specifically lighter feed through the downward
directed solvent flow.
A perforated plate is positioned approximately
Perforated level with the upper edge of the inlet pipe.
plate
The perforated plate allows packing to be
Guide pipe inserted. The packed bed is then located above
the perforated plate (see also Chapter 3.8,
Page 45ff).

Base
The space between upper edge of the guide pipe
and the base of the extraction column is called the
Fig. 3.11 Extraction column K1(9), solvent stabilising zone (see Fig. 3.13, Page 29).
head and base
Purpose of the solvent stabilising zone:
• Additional separation of the liquid mixture. In
Head other words, any feed components present in
the downward solvent flow can still float.
• Avoiding a possible short circuit current where
Feed the feed that has just exited goes directly into
return
the solvent return.
Distributor
pipe

Fig. 3.12 Extraction column, showing

removed head with distributor
pipe

28 3 Description of the device

 CE 620 LIQUID-LIQUID EXTRACTION

The specifically heavier solvent enters the

Feed extraction column via a distributor pipe, coming
stabilising zone
from above and directed downwards. The
distributor pipe consists of a vertical pipe, under
which a horizontal pipe section is attached. This
horizontal pipe section has a few small holes on
the underneath. Thus, the solvent inflow is divided
into several small partial flows. This improves the
mass transfer of the transition component. Fig.
Extraction zone
3.12, Page 28 shows the removed head with
distributor pipe.
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Solvent

Feed

Similar to the solvent stabilising zone, the space

between the head of the extraction column and
the lower edge of the distributor pipe is called the
feed stabilising zone.
The principles described above apply to the feed
stabilising zone accordingly (separation and
avoidance of short circuit current).
The space between solvent stabilising zone and
feed stabilising zone is called the extraction
Solvent
stabilising zone zone. The mass transfer of the transition
component from the feed into the solvent takes
Fig. 3.13 Extraction column zones place in the extraction zone.

Note on safety:

WARNING
The cylinder of the extraction column is made
of glass.
Injuries from glass splinters are possible.
• Wear safety goggles.
• Avoid water hammers. When filling the
extraction column, open valve V30 for
ventilation.

3 Description of the device 29

CE 620 LIQUID-LIQUID EXTRACTION

3.4.3 Setting the phase boundary

A phase boundary forms at the point where the

mutually insoluble solvents (carrier liquid and
solvent) meet.
Solvent inflow Feed return If the phase boundary moves up or down in the
· · extraction column, then this will result in
V Solv,in V Feed,out unwanted breaks. In other words, either feed
enters the solvent/the extract, or solvent enters
the feed/the raffinate.
The aim is to keep the phase boundary at a similar
level during the entire extraction time to enable
reproducible experiments.
Material balance envelope

Setting the phase boundary during the

experiment requires some practice. It requires an
understanding of the hydraulic system.
A key component of the hydraulic system is the
extraction column K1(9).
The phase boundary is determined by the
interaction of the two incoming and two outgoing
material flows.
The material balance envelope with the volume
flows around the complete filled extraction column
is shown in Fig. 3.14.
This is based on the standard case, where the
feed has a lower density than the solvent. This
Feed inflow Solvent return
means that the feed enters the extraction column
· ·
V Feed,in V Solv,out at the bottom and the solvent enters at the top.

Fig. 3.14 Material balance envelope

around
extraction column

30 3 Description of the device

 CE 620 LIQUID-LIQUID EXTRACTION

The balance shows: the sum of the incoming

volume flows is equal to the sum of the exiting
volume flows:

· · · ·
V Solv,in + V Feed,in = V Solv,out + V Feed,out (3.1)

After a long extraction time, in the steady state, if

mass transfer of the transition component from
the carrier liquid into the solvent is no longer
taking place, the following also applies:
· ·
• Where V Solv,in > V Solv,out the phase boundary
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moves upwards in the extraction column.

In words: an excess of solvent displaces the
phase boundary upwards.
· ·
• Where V Feed,in > V Feed,out the phase boundary
moves downwards in the extraction column.
In words: an excess of feed displaces the
phase boundary downwards.
• An excess of solvent is equivalent to a decrease
of feed in the extraction column, and vice versa.
This describes the main influence on the level of
the phase boundary. From this, we can deduce
how to respond to a shift in the phase boundary
(see below).
It should be noted here that the shift in the phase
boundary in the actual extraction process (no
steady state) is more complicated. The mass
transfer of the transition component along the
extraction path is constantly affecting the material
compositions and densities.

3 Description of the device 31

CE 620 LIQUID-LIQUID EXTRACTION

This results in an additional influence on the level

of the phase boundary.

Feed Fig. 3.15 repeats Fig. 3.5, Page 22 and shows the
return excerpt from the process diagram, which relates
to this material balance envelope.
We can see:
• The flow of the incoming solvent and feed
material flows is measured (FI01 and FI02).
• The volumes of the exiting material flows are
unknown.
• Both the incoming and the exiting material
flows can be throttled using regulating valves
V1 to V4.
• Any change to only one of the four regulating
valves in principle changes all four material
flows.

The values of FI01 and FI02 flow measurements

refer to water at 20°C. For materials with
significantly different properties, the value must
be corrected (see also Chapter 5.3, Page 83f).
Solvent
return We must also note that the exiting materials may
Solvent inflow

Feed inflow

have very different viscosities. The material flow

of the viscous material is much lower with the
same opening of the regulating valve. It therefore
makes sense to only throttle the material flow of
the less viscous exiting material.

Fig. 3.15 CE 620 process diagram,

extraction column section

32 3 Description of the device

 CE 620 LIQUID-LIQUID EXTRACTION

We recommend the following procedure to keep

the level of the phase boundary in the extraction
column as constant as possible (assuming the
feed is much more viscous than the solvent):
• Allow inflowing material flows, set the
beginning of extraction and keep constant
during extraction. Readjust in the event of
variances.
• During extraction, fully open regulating valve
V4 for the more viscous exiting material.
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• Set phase boundary by throttling the regulating

valve V3(12) for the less viscous exiting
material.
• Regularly note down the position of this
regulating valve V3 and the phase boundary in
the extraction column. The change in level can
then be used to derive whether V3 should be
opened a little more or closed.
A worksheet designed for this purpose can be
found in the appendix (see Tab. 6.3, Page 119).
The photo opposite shows the mark for half the
extraction height (50%).
Fig. 3.16 Mark for the level of the phase
boundary The distance between the mark and the phase
boundary can be measured with a ruler.
• If the phase boundary is falling, close
regulating valve V3 a little more.
• If the phase boundary is rising, open regulating
valve V3 a little more.

3 Description of the device 33