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Sulzer Chemtech

Liquid-Liquid Extraction Technology

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Liquid-Liquid Extraction Technology at Sulzer Chemtech

Sulzer Chemtech, a member of the Sulzer Corporation, with headquarters in Winterthur, Switzerland, is active in the field of process
engineering, employing 3000 persons worldwide. Sulzer Chemtech is represented in all important industrial countries setting standards
in the field of mass transfer and static mixing with its advanced and economical solutions.

Sulzer Chemtech is organized into four business units, one of which is the Process Technology group. This business unit was formed in
early 2009 following the acquisition of Khni, a Swiss company with more than 75 years experience in innovative separation processes.
Today, Sulzer Chemtech Process Technology is headquartered in Allschwil (Basel), Switzerland. We provide a unique and wide portfolio
of separation and application technologies, amongst which liquid-liquid extraction.

Working Principle Fields of Application


Liquid-liquid extraction is an important the liquids are transported countercur- Liquid-liquid extraction is a complex sepa-
separation technology, with a wide range rently. The viscosity and interfacial tension ration process. An additional component
of applications in the modern process in- are additional important parameters. has to be introduced as extractant, which
dustry. The extraction process is based on makes other subsequent separation steps
In nearly all liquid-liquid extraction pro-
different solubilities of components in two necessary. Therefore, liquid-liquid extrac-
cesses one of the liquids is dispersed into
immiscible, or partially miscible, liquids. tion is mostly used when separation of
the second liquid in the form of droplets.
The components that need to be recov- components by distillation is either un-
The key for a high process performance
ered are extracted from the feed stream economical, or even impossible. Some
is an adapted droplet size and a uniform
with the help of an extractant (often called examples are:
hold-up profile throughout the column.
solvent). Both liquids have to be thorough-
This requires specially adapted equipment Simultaneous separation of various
ly contacted and subsequently separated
and in-depth know-how about two phase components with widely differing boiling
from each other again. To achieve high pu-
liquid flows. points
rities and yields, it is necessary to operate
with multiple stages and with the liquids Separation of high-boiling products or
flowing countercurrently. pollutants which are present in only low
concentrations
For successful separation by extraction, all
Separation of components with similar
components must meet certain specifica-
boiling points or components forming
tions. The main criteria for the extractant
azeotropes
are a favorable partition coefficient, a high
selectivity and an easy separation from Separation of mixtures with thermally
the extracted product. The basic condi- sensitive components
tions for the pair of liquids are a low mutual Selective separation of single compo-
solubility and a difference in density, which nents out of a multi-component mixture
is the driving force for the motion of the Separation of components from electro-
droplets. In most multistage extractors, lytic solutions

Our head offices in Allschwil, Switzerland

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Overview of Equipment

Our liquid-liquid extraction is a technically sophisticated separation technology, offering you a solution where other tech-
nologies are uneconomical or even not feasible

Extractors Classification Extractor Types


The main task of any extractor is to create A wide range of equipment for liquid-liquid You can find our equipment in almost all
optimal conditions for mass transfer be- extraction is available, which can be cat- industrial applications. Our portfolio is
tween the two phases. This includes drop- egorized as follows: based on a number of modern, efficient
let formation / dispersing, transport and Extraction columns types of extractors. The core of this range
settling of the phases. Two types of dis- is the agitated Khni column type ECR
Mixer-settlers
persion are possible. The feed can be dis- with an extremely wide field of applica-
persed into the solvent, or be continuous Centrifugal extractors tions, and the Sulzer packed column ECP.
with the solvent dispersed into it. These The extraction columns, also referred to as Mixer-settler type extractors are available
two types often show a considerably dif- extraction towers, can be further differenti- if process reasons do not favor the use of
ferent behavior. Also, the type of contact ated into three groups: columns.
between the two phases is an important,
Static without energy input Column type extractors:
equipment related aspect. In the case of
stage-wise contact, the liquids are com- Agitated Agitated Khni column ECR
pletely separated from each other in every Pulsed Sulzer packed column ECP
stage, whereas in the case of differential
Mixer-settler type extractors:
contact, the liquids are in continuous,
countercurrent contact. Both systems Mixer-settler EMS
have specific advantages affecting equip- Mixer-settler column ECMS
ment sizes and extraction efficiency.

Sulzer extraction packing Installation of an industrial ECR type column on site

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Agitated Khni Column ECR

Our flexible, multipurpose extraction column

Basic and Mechanical Design Advantages and Characteristics


The agitated Khni column is a well-prov- Based on its flexible design and our long-
en, highly efficient extractor. Its main char- standing experience, the Khni column
acteristics are the agitated compartments, ECR has a range of advantages:
arranged one on top of each other. The
Universal use
concept is simple, yet, its hydrodynamic
performance is outstanding. High flexibility for varying process para-
meters and physical properties
Turbine Mixers and Partition Reliable scale-up
Plates More than 30 theoretical stages in one
single column
Turbine agitators installed in each stage
are responsible for the formation of the Standard turndown 1 : 3
dispersion. They create a torus-shaped, Column diameter: 30 mm - 3.5m
rotary flow pattern and also mix the liquid Physical properties:
phases radially, which is an important con- Velocity [m/s]
- Density difference >40kg/m3 0.0513 0.0907 0.130 0.169 0.209 0.248 0.287 0.327
dition for safe and reliable scale-up. Perfo-
rated plates form the boundaries between - Viscosity < 500 mPas
each agitated compartment and reduce - Interfacial tension > 2 mN/m CFD analysis of an agitated extraction column
back-mixing to enhance the separation compartment
Differential phase contact
performance.
Phase ratio up to 70 : 1
The hydrodynamic conditions can be in- Materials:
fluenced by varying four geometrical pa-
- Stainless steel / higher alloys
rameters:
- Special metals, for example, titanium
Turbine diameter
- PP / PVDF / PFA
Turbine height
- Glass-lined shell
Open area of the partition plates
Height of the compartments
With this flexible geometry, it is possible to
optimize performance regarding through-
put and mass transfer, even in cases
where process parameters and physical
properties vary strongly along the length
of the column.
The agitated Khni column ECR has a
simple and robust construction. The drive
unit and the shaft are supported at the top
of the column. All common types of shaft
seals can be used (stuffing box, mechani-
cal seals). In special cases, the seal can
be replaced by a magnetic drive. Only
radial slide-bearings are necessary inside
the column, which are accessible through
hand- or manholes. The sturdy design, the
materials selected and the low rotational
speed of the agitator in industrial columns
(typically 10-70 rpm) allow a practically
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maintenance free operation.
Agitated column internals

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Packed Column ECP

Our extraction column of choice for high throughput

Basic and Mechanical Design Liquid Distributors amplitude) of 800 to 1200 mm/min. Such
pulsators are available as standard items
The ECP packed column is based on In order to create an even flow profile at and are used with our packed extraction
the current state-of-the-art extraction re- either end of the packed bed, both liquid columns.
search. The column consists of a packed phases are distributed over the whole
bed, distributors for the two liquid phases cross sectional area by suitable distribu-
and, optionally, a pulsator. tors. The design of the dispersed phase
Advantages and Characteristics
distributor requires special attention, in Based on the special design of the pack-
Packing order to achieve a narrow droplet size dis- ing and liquid distributors, the ECP col-
tribution. umn has a number of advantages:
The special Sulzer extraction packing re-
duces the back-mixing of the continuous If the column is operated without energy High specific throughput resulting in:
phase, thus providing nearly plug flow input (unpulsed), the packed extraction - Small column diameters
conditions and a narrow droplet size dis- column is a simple item of equipment
- Revamp options of existing columns to
tribution. Both are necessary to achieve without any special mechanical features
increase capacity
high throughput and high efficiency. To fur- and free of moving parts. Often, however,
ther increase the separation performance, the liquid has to be pulsed to increase Capable to deal with challenging physi-
additional dual flow plates can be inserted the separation performance and provide cal properties:
between the packing elements. a further control parameter for changing - Low density difference <50kg/m3
operating conditions. Pulsators are typi- - Low interfacial tension <2mN/m
cally specified with intensities (frequency
- Tendency to form emulsions
Reliable scale-up
Standard turndown 1 : 2
Column diameter: 50 mm - 5.6m
Physical properties:
- Density difference >30kg/m3
- Viscosity up to 100 mPas
- Interfacial tension > 1 mN/m
Materials:
- Metals
- PTFE, PVDF, PFA

Packed internals of a liquid-liquid extraction


column

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Mixer-Settler EMS and Mixer-Settler-Columns ECMS

If you need stage-wise contact but have space constraints

Conventional Mixer-Settler EMS Mixer-Settler-Column ECMS Advantages and Characteristics


Mixer-settlers operate with a purely stage- As implied by the name, the mixer-settler- Mixer-settlers EMS have a number of spe-
wise contact. After every mixer, there is a column is a series of mixer-settlers in the cific advantages and are suitable for:
settler. Mixer-settlers can be operated in a form of a column. It consists of a number
Long residence times (> 15min):
multistage, countercurrent fashion, which, of stages installed one on top of the other,
however, is associated with considerable each hydraulically separated, and each - Extraction controlled by residence time
piping and instrumentation and also re- with a mixing and settling zone. With this - Reactive extraction systems
quires large areas for installation. Because design, it is possible to eliminate some of - Long phase separation times
of these implications, mixer-settlers are the main disadvantages of conventional
Extraction controlled by pH (stage-wise
only used if process reasons dictate a mixer-settlers, whilst maintaining stage-
pH adjustment)
stage-wise contact. wise phase contact.
Batch extraction
Conventional mixer-settlers are made The mixer turbines do not need to trans-
Stage-wise phase contact
either as a box or a tubular type design. port the liquids from stage to stage, there-
The latter is also used for glass equipment fore, the rotational speed can be adjusted
Specific advantages of the mixer-settler-
and when higher design pressures are re- to achieve optimal droplet sizes. Due
columns ECMS are:
quired. to the requirement for settling of the liq-
uid phases in every stage, the specific Small footprint
The most important element of every mixer
throughput achievable in a mixer-settler- Column like design
is the pump-mix turbine. It has to create
column is considerably lower in compari-
the dispersion and the hydrostatic head Allows extreme to unlimited phase ratio
son to other extraction columns (< 10 m3/
for transport of the liquid. An additional
m2h). The mechanical design of the mixer-
agitator can be mounted on the same
settler-column is comparable to the agi-
shaft to optimize the dispersion and en-
tated Khni column ECR.
hance the efficiency.

Principle of a mixer-settler-column Examples of mixer-settlers

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Selection of Equipment

The right choice of equipment is important for a stable operation and optimal performance

Correct Selection of Equipment Criteria in favor of a packed column: uously innovate our extraction technology,
-High throughput with particular attention to the following
The correct selection of the type of extrac- two areas: miniplant and modeling.
tor is an important step in every extrac- -Limited number of stages required
tion project. Various selection aids, such -No moving parts desired
as decision trees, point score tables, and
Miniplant and Modeling
diagrams can be found in the literature. All Additional Criteria The continuous improvement of miniplant
extractors have one behavior in common: technology on the one hand, and the
the efficiency of the extraction is linked to When examining economic aspects, re- mathematical modeling of extraction col-
the specific capacity. Basically, the selec- liability is an important factor. Delayed umns with population balance or Monte-
tion of equipment should be made using commissioning, non-performance, down- Carlo methods on the other hand are
process and economic criteria. However, time due to equipment failure lead to loss merging at the same time.
this can be difficult at the beginning of of production and may bring substantial
costs to rectify. Therefore, besides pure With the help of these complex models
a project when without testing the type
technical criteria, the experience and reli- and small laboratory scale droplet experi-
and size of the extractor required are not
ability of Sulzer Chemtech as technology ments it is possible to predict the perfor-
known.
partner are important attributes. When mance of extraction columns in pilot scale
cooperating with us, you will find a part- in specific cases. This method can be
Process Related Criteria used to reduce the effort in pilot trials as
ner with outstanding test facilities and
The agitated ECR column with its inherent numerous reference applications in liquid- basis for the optimized design of an ex-
flexibility and wide operating range is the liquid-extraction in the field. Our state- traction column and therefore, reduces
most suitable extractor for the majority of of-the-art equipment and proven scale- both costs and time-to-market.
cases. Exceptions and special applica- up procedures, in combination with our Future developments are expected to
tions, which require a different type of ex- highly skilled employees will provide you extend the application of this method to
tractor, can be identified with a few criteria a process solution with guaranteed per- the scale-up of industrial size columns. It
that are easily checked: formance. would then only be necessary to establish
Necessity of stage-wise contact the model parameters, with the help of
Requirement for a residence
Outlook small laboratory measuring cells. We in-
time > 15 min tensely participate in and support this field
Research in the field of liquid-liquid extrac-
of research within our own test center and
Criteria in favor of a mixer-settler: tion continues with great effort. We contin-
by our cooperations with both industrial
- Density difference < 50kg/m3 and university partners.
Sections of pilot columns
-Interfacial tension < 2 mN/m
-Tendency to form emulsions
-Low number of theoretical stages

Feed Feed
continuous dispersed

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Feasibility Study and Trials

Your optimal process solution is guaranteed by our design based on pilot trials in our state-of-the-art test center, and our
extensive know-how on our liquid-liquid extraction technology

Optimal Process Solution Mass balance, including concentrations Rental equipment is available for tests on
Physical properties (density, interfacial your premises. If required, we can provide
In spite of considerable progress in the you assistance and training for such in-
research and development of liquid-liquid tension, viscosity)
house tests.
extraction technology, it is still not possible Liquid-liquid equilibrium data
to design an extractor from first principles. The miniplant size extractor ECR 32 is well
Therefore, a systematic test method is Lab and Pilot Trials suited for miniplant piloting of complete
very important. We offer you decades of processes including recycle streams. This
Laboratory or pilot plant trials are neces- small-scale unit proves the feasibility of
relevant experience to call upon, including
sary to secure the correct design of ex- the proposed solution and generates pre-
the necessary test methods and facilities,
traction equipment. We undertake these liminary scale-up data while requiring only
incorporating various laboratory and pilot
to establish optimal operating conditions, a minimum amount of feed material.
plant equipment.
and, depending on the extractor type, the
The design of an extractor is carried out in most favorable geometric parameters
four steps: (size and type of internals). Successful
trials allow us to safely scale-up to an in-
Execution of a feasibility study
dustrial size unit, and to provide you full
Generation of basic data process guarantees. We are capable of
Pilot trials carrying out all testing, including estab-
Scale-up and design lishing missing physical properties, in our
own test center. At this location we have
the following test extraction equipment
Feasibility Study and Basic Data
available:
The success of an extractive separation
Extraction columns:
step depends largely on finding a suitable
extractant. In many cases, based on our -Agitated columns with diameter 32, 60,
experience we are able to propose such 150 mm
Agitated liquid-liquid extraction column
a solvent. However, for new processes, a -Packed columns with diameter 50 and in pilot scale
professional and analytical screening of 150 mm
suitable solvents is required. The feasibility -Shell: glass
of the selected extraction process is then
often confirmed in a mini-plant test run. -Internals: SS316L, hastelloy, titanium,
zirconium, PP and PVDF
In the next step, basic data are estab- Mixer-settlers:
lished which are used as input for subse-
quent pilot trials and also permit a prelimi- -Tube type mixer-settlers
nary sizing of the extractor. These basic -Total volume per stage: 70 ml 15 l
data include: -Material: glass / SS316L

Sulzer test center in Allschwil, Switzerland

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Design, Fabrication and Delivery of Equipment

Our extensive experience in design and fabrication in our modern workshops ensures top quality extraction units at your
service

Design and Scale-up Manufacturing Service Installation, Commissioning and


In the field of liquid-liquid extraction, scal- Every extractor we supply is manufac- Start-up
ing-up from pilot units to industrial size tured under our complete responsibility in We have a team of highly experienced
equipment is an important and critical modern workshops equipped with state- installation supervisors, who provide con-
step. It is not at all straightforward and of-the-art manufacturing tools with certi- struction support services for site-built
simple empirical methods will normally fail. fied production processes. Column shells plants, and for the off-loading and installa-
Our extensive experience in successful are either manufactured in-house, or by tion of skid-mounted plants. These super-
scale-up is supported by our detailed un- approved and qualified sub-suppliers. The visors liaise closely with your construction
derstanding of the fundamental theories of latter approach is followed for very large manager, safety officer and mechanical
hydrodynamics and mass transfer playing columns, for glass-lined columns, or when contractor, to ensure a safe and trouble-
a role in extraction. Our Sulzer extractors special design codes are to be applied. free installation.
have often been the topic of scientific re-
GMP and CIP are requirements well- Following installation, our process engi-
search at various universities.
known to us. Design, manufacture and neers undertake plant commissioning fol-
certification of many extractors have been lowing a structured plan. The commission-
Installation of an industrial scale ECR extraction carried out in accordance with these and
column
ing team is usually headed by the process
other standards. engineer responsible for the plant design.
We deliver our extraction technology as a This phase ends with the start-up of the
basic design package with state-of-the- process unit followed by a Site Accep-
art proprietary equipment. In addition, we tance Test (SAT). Training of your opera-
have a specific long-term experience in tors may take place in parallel.
fabrication, installation and start-up of our At plant hand-over, you will be provided
solutions as skid-mounted units. with final, as-built documentation includ-
Advantages of skid-mounted, turn-key ing operating manuals, final lay-out draw-
plants are: ings and certificates. A dedicated after
sales group ensures the support for spare
Short delivery time through an integrated parts and services during the whole life-
fast track execution time of the plant, wherever you are around
Low overall investment costs the globe.
Reduced on-site erection and hook-up Right from plant start-up you can benefit
time and thus minimal site disruption from your optimal performing plant solu-
Manufacture of the complete plant under tion based on our liquid-liquid extraction
workshop conditions ensuring the high- technology.
est quality
Completion of the Factory Acceptance
Test (FAT) prior to delivery
Qualification tests prior to plant delivery

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Application and Processes

The following examples give you a taste of our collection of successful applications

Sulzer extractors are successfully applied Wet Purification of Phosphoric geometry of the extraction column inter-
in every segment of the process industry: Acid nals.
Bulk chemical industry You can find Sulzer extraction columns
Pure, food-grade phosphoric acid is cur-
Petroleum industry in several other processes for removal of
rently almost exclusively produced using
polycyclic aromatics out of oil streams, in
Fine chemical industry the so-called wet process. This process
both production and recycling.
Pharmaceutical industry includes three extraction steps with a
scrubbing stage in the middle to remove
Biotech industry
impurities. Our extensive and specific ex- Purification of Organic Acids
Food industry perience covers a multitude of large col-
Dilute aqueous carboxylic and sulphonic
Hydrometallurgy umns installed worldwide.
acids can be concentrated and purified
with the help of liquid-liquid extraction. A
Standard Processes Extraction of Aromatics classic example is the recovery of acetic
acid from streams with concentrations of
On the basis of decades of both experi- Two agitated ECR columns are used in
5-50 wt%. Higher acids are recovered by
ence and in-house development, we the IFP process for recovery of aromatics
reactive extraction with amines, which ex-
have acquired our own detailed process (benzene, toluene, xylene) from hydrocar-
tract the acid by forming reactive bonds.
know-how for many classic liquid-liquid bon mixtures. In the first column of this
An example is the extraction of lactic acid
extraction applications. As a result of this, process the extraction is carried out with
following the fermentation process.
in some specific applications, our Sulzer DMSO, combined with a backwash. The
extractors are used almost exclusively. extreme profiles of flow rate and physical
Below we give you an overview of a few properties require a high flexibility in the
typical applications where our extraction
solutions are used. Loading of a Sulzer Chemtech modular system for recovery of solvents and purification

Solvent Recovery
Many standard processes for the separa-
tion and recovery of various solvents in-
clude extraction:
Recovery of high-boiling, organic com-
ponents, in low concentrations, from in-
dustrial wastewaters (for example, DMF
and phenol)
Breaking of azeotropes (for example,
pyridine/water)
Removal of water-soluble components
from a complex solvent mixture (for ex-
ample, ethanol, methanol and IPA)

Wastewater stripper with optional decanter in-


cluding a wastewater example
(Concentration figures quoted in % by weight)
Vent

Cooling water

Condenser

Decanter

Feed (100 kg/h)


92 % Water
8% Ethyl acetate
Distillate (8 kg/h)
>9 7% Ethyla cetate
Stripping <3 % Water
column

Heat exchanger Heat input

Bottom product (92k g/h)


>9 9.99 % Water

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Application and Processes
Client Specific Applications

We jointly develop your process solution and tailor our extraction technology to your needs

Client Specific Applications Specific Case Stories Wool Wax Alcohol


Our extractors are widely used and tailor- The following case stories demonstrate Wool wax alcohol can be extracted fol-
made to your specific applications. In the the variety, complexity and attractiveness lowing the saponification of wool grease.
majority of cases the optimum process of liquid-liquid extraction when applied to Another typical application in this field is
solution was developed in close coopera- specific fields. the purification step in the manufacture of
tion with the customer and based on pilot lanolin (ingredient in cosmetics) from wool
trials. We have an extensive track record Caprolactam grease.
of numerous, highly customer specific ap-
plications based on our liquid-liquid ex- This application presents the successful
Separation Based on Polarity
traction technology. operation of the agitated Khni column
type ECR in a case with extremely low In numerous applications the separation
The following forms a summary of our ref- interfacial tensions in the range of 120 of a polar component, like an alcohol or
erence list of extracted substances. mN/m. The total product yield with our ketone, out of a non-polar matrix, for ex-
process amounts to over 98%. ample monomer or hydrocarbon, is re-
Acetic acid, acetonitrile, acetyl-para- quired. In this so-called washing step a
aminophenol, alkaloids, ammonia, Pesticides high flexibility and often extreme phase
aniline, benzoic acid, caprolactam, ratio is required.
catalysts, cresols, diacetone sorbose, Pesticides are produced in the agrochemi-
dichlorobenzene, diethylaniline, di- cal industry, where our liquid-liquid extrac-
Removal of Phenol from Indus-
methylacetamide, dimethylformamide, tion process has proven application serv-
dimethyl ketone, dimethyl sulfoxide, ing two purposes, namely, the treatment trial Wastewaters
ethanol, guaiacol, hydroquinone, iso- of wastewater and the recovery of the Our extraction process has also proven
propanol, lactone, metal ions (like Fe3+, chemical compound for re-use. its use in environmental applications. A
Na+, Pd2+, and Au3+), methanol, n- typical example in this field is formed by
methylpyrrolidone, monoacetonesor- Used Oil Recycling extraction of phenol from industrial waste-
bose, nitrobenzene, nitric acid, pesti- water with a heavy oil. The extract is sub-
Our technology has proven use in extrac-
cides, pharmaceuticals, phenol, potas- sequently used as burner fuel, thereby
tion of polycyclic aromatics from used
sium carbonate, potassium chloride, recovering energy in addition.
engine and lube oil, to improve the color
pyridine, sodium borohydride, sulfate,
index and oil quality.
sulphuric acid, sulphonic acid, tetra-
hydrofuran, triacetoneamine, vanillin,
vitamins, water, wine aroma, wool wax Triacetone Amine
alcohol, xylenol. A typical example of the application of our
extraction process is in the treatment of
industrial wastewater with 5% triacetone
amine, whereby reductions down to 5
ppm (factor 10'000) can be achieved, with
a phase ratio of 35 : 1.

Part of an extraction column on a truck Glass-lined column shell with PVDF internals

11
www.sulzer.com
Please check for your local contact

Sulzer Chemtech Ltd, a member of the Sulzer Corporation, with headquar- The activity program comprises:
ters in Winterthur, Switzerland, is active in the field of process engineering Process components such as fractionation trays, structured and ran-
and employs some 4000 persons worldwide. dom packings, liquid and gas distributors, gas-liquid separators, and
Sulzer Chemtech is represented in all important industrial countries and internals for separation columns
sets standards in the field of mass transfer and static mixing with its ad- Engineering services for separation and reaction technology such as
vanced and economical solutions. conceptual process design, feasibilities studies, plant optimizations in-
cluding process validation in the test center
Recovery of virtually any solvents used by the pharmaceutical and
chemical industry, or difficult separations requiring the combination of
special technologies, such as thin film/short-path evaporation, distilla-
tion under high vacuum, liquid-liquid extraction, membrane technology
or crystallization.
Complete separation process plants, in particular modular plants
(skids)
Advanced polymerization technology for the production of PLA and
EPS
Tower field services performing tray and packing installation, tower
maintenance, welding, and plant turnaround projects
Mixing and reaction technology with static mixers
Cartridge-based metering, mixing and dispensing systems, and dis-
posable mixers for reactive multi-component material

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Legal Notice: The information contained in this publication is believed to be accurate and reliable, but is not to be construed as implying any
28.65.06.40 - XI.14 - 20 - Printed in Switzerland warranty or guarantee of performance. Sulzer Chemtech waives any liability and indemnity for effects resulting from its application.

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