Experiment Instructions: Liquid-Liquid Extraction

CE 620 LIQUID-LIQUID EXTRACTION
All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 06/2012
Experiment Instructions
Dipl.-Ing. (FH) Klaus Schröder
This manual must be kept by the unit.
Before operating the unit:

- Read this manual.
- All participants must be instructed on
handling of the unit and, where appropriate,
on the necessary safety precautions.
Version 1.1 Subject to technical alterations
i
ii
Table of Contents
1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
2 Safety . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2.1 Intended use . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2.2 Structure of safety instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
2.3 Safety instructions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 7
3 Description of the device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

3.1 Objective of the extraction, designation of the substances involved . 15

3.2 Process diagram . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
3.3 Device design . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
3.4 Device function and main components . . . . . . . . . . . . . . . . . . . . . . . 19
3.4.1 Operating mode and process description . . . . . . . . . . . . . . . 20
3.4.1.1 Batch mode. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 20
3.4.1.2 Continuous mode . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 25
3.4.2 Extraction column . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28
3.4.3 Setting the phase boundary . . . . . . . . . . . . . . . . . . . . . . . . . 30
3.4.4 Distillation unit. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 34
3.5 Control cabinet with controller . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
3.6 Special features of individual components . . . . . . . . . . . . . . . . . . . . 41
3.7 Accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 42
3.8 Inserting packing into the extraction column . . . . . . . . . . . . . . . . . . . 45
3.9 Positioning the trainer . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 49
3.10 Commissioning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 51
3.11 Decommissioning . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 56
3.12 Care and maintenance . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 57
3.12.1 Vacuum grease for glass valves. . . . . . . . . . . . . . . . . . . . . . 57
3.12.2 Descaling the round-bottomed flask . . . . . . . . . . . . . . . . . . . 57
iii
4 Basic principles . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
4.1 Liquid-liquid extraction. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 59
4.2 Types of liquid-liquid extraction systems . . . . . . . . . . . . . . . . . . . . . . 63
4.3 Refining crude vegetable oil, removal of lecithin . . . . . . . . . . . . . . . . 65
4.4 Model material system for CE 620 . . . . . . . . . . . . . . . . . . . . . . . . . . 67
4.5 Distillation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69
4.6 Thermophysical properties and determining concentration. . . . . . . . 70
5 Experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75
5.1 Beaker experiments. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 77
5.2 Conducting the density measurement . . . . . . . . . . . . . . . . . . . . . . . . 78
5.3 Preliminary experiment for flow measurement . . . . . . . . . . . . . . . . . 83
5.4 Experiments with the device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 85
5.4.1 Stirring feed and solvent . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86
5.4.2 Standard experiment, basic conditions,
series of experiments . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 87
5.4.3 Objectives of the experiment . . . . . . . . . . . . . . . . . . . . . . . . 88
5.4.4 Experiment setup . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88
5.4.5 Conducting the experiment and cleaning . . . . . . . . . . . . . . . 89
5.4.5.1 Conducting the liquid-liquid extraction experiment, batch . . 90
5.4.5.2 Conducting the distillation experiment . . . . . . . . . . . . . . . . . 96
5.4.5.3 Normal cleaning after the end of the experiment . . . . . . . . 100
5.4.5.4 Additional cleaning with methylated spirits . . . . . . . . . . . . . 102
5.4.6 Measurements . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 106
5.4.7 Evaluation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 108
5.4.8 Comment and evaluation . . . . . . . . . . . . . . . . . . . . . . . . . . 110
iv
6 Appendix . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113
6.1 Technical data . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 113
6.2 Scope of delivery, accessories . . . . . . . . . . . . . . . . . . . . . . . . . . . . 116
6.3 List of abbreviations. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 117
6.4 List of identification letters used in the process diagram . . . . . . . . . 117
6.5 Worksheet . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 118
v
vi
1 Introduction
Technical classification
CE 620 enables the liquid-liquid extraction of a
transition component from a liquid mixture in a
solvent.
We recommend the " Extraction of ethanol from
refined plant oil with water" model material
system for experiments with CE 620.
This model material system copies the "refined
vegetable oil and water" solvent system, in a

similar way to the real application "removal of
lecithin from crude vegetable oil."
Layout and function of the device

The liquid mixture to be extracted (feed = carrier
liquid with transition component) is pumped into
the bottom of the transparent extraction column.
There, it moves in counterflow to the solvent,
which is pumped into the top of the extraction
column. In doing so, the transition component
transfers from the feed into the solvent. Carrier
liquid and solvent are insoluble in one another and
form a phase boundary in the extraction column.
Feed and solvent each leave the extraction
column at the side opposite the inlet.
The trainer can be operated in both discontinuous
(batch) and continuous modes.
The integrated distillation unit is used for
enriching the transition component in the extract.
The distillation unit consists of a heated round-
bottomed flask with packed columns and Liebig
condenser.
1 Introduction 1
The vacuum pump supplied allows distillation at

low pressure.
The learning objectives are:

• Transition of a component from a two-
component liquid mixture (feed) into a solvent
by extraction.
• Scale-up from the beaker to the pilot plant
scale.
• Enrichment of the transition component in the
extract by distillation.
• Evaluation of the separation processes via
concentration measurements and mass
balances.
• Influence of experimental variations on the
separation processes.
Structure of the instructions

In addition to these experiment instructions, a
separate installation manual is included in the
delivery. In this manual you will find details on how
to install the distillation unit.
Didactic notes for teachers

CE 620 can be used to carry out practical liquid-
liquid extraction at the scale of a pilot plant.
The trainer is designed such that the processes
are largely visible and can be observed.
The field of application is education in the subject
of process engineering.
A suitable laboratory environment with water
supply and water drainage is required for the
2 1 Introduction
operation of the trainer. Operating the system

requires good prior experimental experience.
These experiment instructions include a
description of the trainer and its functional
principle.
A standard experiment is presented for the
recommended "extraction of ethanol from refined
vegetable oil with water" model material system.
Areas where the trainer can be employed include:

• Practical experiments
Small groups of two or three students can carry
out experiments for themselves. The time
required to conduct an experiment can be
estimated at about five hours. Additional time is
required to clean the trainer on the following
day.
• Project work
The trainer is particularly suited to carrying out
project work.
A series of experiments can be used to work
out how changing the experimental conditions
affects the results.
The experiments can be performed by a single
experienced student after thorough instruction.
1 Introduction 3
These materials are intended to be used to help

you prepare your lessons. You can compile parts
of the materials as information for students for use
in the classroom.
We also provide you with these experiment
instructions in PDF format on a CD to support
your lessons. We grant you unlimited
reproduction rights for use within the context of
your teaching duties.
4 1 Introduction
2 Safety
2.1 Intended use
The unit is to be used only for teaching purposes.
2.2 Structure of safety instructions
The signal words DANGER, WARNING or

CAUTION indicate the probability and potential
severity of injury.
An additional symbol indicates the nature of the

hazard or a required action.
Signal word Explanation
Indicates a situation which, if not avoided, will

DANGER result in death or serious injury.
Indicates a situation which, if not avoided, may

WARNING result in death or serious injury.
Indicates a situation which, if not avoided, may

CAUTION result in minor or moderately serious injury.
Indicates a situation which may result in

NOTICE damage to equipment, or provides instructions
on operation of the equipment.
2 Safety 5
Symbol Explanation
Electrical voltage
Explosive materials
Flammable substances
Hazard area (general)
Hot surface
Rotating parts
Risk of slipping
Notice
Wear eye protection
Wear gloves
Wear safety shoes
No smoking
6 2 Safety
2.3 Safety instructions
These safety instructions relate to the model

material system that is recommended for
operating the CE 620 trainer:
• Refined rapeseed oil as carrier liquid,
• Ethanol as transition component,
• Water as solvent,
as well as methylated spirits, detergent and dilute
acetic acid as cleaning agents.
NOTICE
If starting materials other than those specified
are used, the customer must carry out his own
safety analysis. This applies to both the different
starting material and to any possibly resulting
intermediate and final products.
NOTICE
If starting materials other than those specified are
used, the customer must check the material
compatibility beforehand.
2 Safety 7
WARNING
Electrical connections are exposed when the
control cabinet is open.
Risk of electrical shock.
• Disconnect the plug from the power supply
before opening the switch cabinet.
• All work must be performed by trained
electricians only.
• Protect the switch cabinet from humidity.
WARNING
Irritant chemicals.
Contact with ethanol, methylated spirits and
detergent irritates the eyes and skin. Repeated
contact may cause dermatitis due to the
degreasing effect.
Contact with acetic acid irritates the eyes and
skin.
• Wear protective gloves and protective goggles.
• In case of contact with the skin, wash with
plenty of water.
• In case of contact with the eyes, hold eyelid
open and rinse immediately with plenty of
water. Seek medical attention.
WARNING
Irritant chemical vapours.
Vapours from ethanol and methylated spirits can
cause drowsiness and dizziness.
• Do not inhale directly.
• Ensure adequate ventilation.
8 2 Safety
WARNING
Flammable solvents.
The vapours from ethanol and methylated spirits
can form explosive mixtures with air.
• Keep away from sources of ignition.
• Do not smoke.
• Ensure adequate ventilation.
• Do not empty ethanol and methylated spirits
into drains undiluted.
• Observe national and local regulations.
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.
WARNING
Parts of the distillation unit are made of glass.
Injuries from glass splinters are possible.
• Wear safety goggles.
2 Safety 9
WARNING
Localised overheating is possible when
heating the round-bottomed flask without
sufficient fill level.
The vapours from ethanol and methylated spirits
can form explosive mixtures with air.
• Read through the separate manufacturer's
documentation before using the heating mantle
for the first time.
• The heating mantle may not be operated
unattended.
• Never heat the round-bottomed flask without
liquid.
• Depending on the number of heating zones
switched on, ensure the level in the round-
bottomed flask remains continuously sufficient.
WARNING
Heating mantle is sensitive to moisture.
Risk of electrical shock.
• Read through the separate manufacturer's
documentation before using for the first time.
• Prevent moisture from penetrating the heating
mantle.
unattended.
• Turn off moist heating mantle immediately.
• Only re-start moist heating mantle after it has
been fully dried.
10 2 Safety
WARNING
Hot surfaces of switched on heating mantle.
Burns are possible.
unattended.
• Do not touch the heating mantle when it is
switched on.
WARNING
Hot liquids at the outlet of the round-bottomed
flask.
Scalds are possible.
• Do not touch during operation.
• Wear safety goggles and protective gloves
when draining.
WARNING
Rotating shaft when agitator is operated with
a hand drill.
Risk of hand injuries.
• Do not touch the shaft.
WARNING
Rapeseed oil spillages.
Possible injury from falls.
• Clean up rapeseed oil spillages immediately.
2 Safety 11

Experiment Instructions: Liquid-Liquid Extraction

Uploaded by

Document Information

Original Description:

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Experiment Instructions: Liquid-Liquid Extraction

Uploaded by

Copyright:

Available Formats

CE 620 LIQUID-LIQUID EXTRACTION

All rights reserved, G.U.N.T. Gerätebau, Barsbüttel, Germany 06/2012

This manual must be kept by the unit.

Before operating the unit:

Version 1.1 Subject to technical alterations

3 Description of the device . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15

3.1 Objective of the extraction, designation of the substances involved . 15

vegetable oil and water" solvent system, in a

Layout and function of the device

The vacuum pump supplied allows distillation at

The learning objectives are:

Structure of the instructions

Didactic notes for teachers

operation of the trainer. Operating the system

Areas where the trainer can be employed include:

These materials are intended to be used to help

2.1 Intended use

The unit is to be used only for teaching purposes.

2.2 Structure of safety instructions

The signal words DANGER, WARNING or

An additional symbol indicates the nature of the

Signal word Explanation

Indicates a situation which, if not avoided, will

Indicates a situation which, if not avoided, may

Indicates a situation which, if not avoided, may

Indicates a situation which may result in

Hazard area (general)

Wear eye protection

Wear safety shoes

2.3 Safety instructions

These safety instructions relate to the model

• Observe national and local regulations.

You might also like