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Supercritical Fluids

Technologies and Plants

A company
of ThyssenKrupp
Technologies

Uhde High Pressure Technologies

TK

CO2

Process Engineering and Plant Construction


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High-precision machining of an HP extraction


component on a CNC-operated horizontal
boring mill

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Uhde High Pressure Technologies manufactures a broad range of components for


high pressure installations.
These products include autoclaves, reactors with rotary agitators, tubular reactors,
heat exchangers, high pressure pumps,
valves and fittings, flanges and piping,
which are used in a wide variety of high
pressure processes. Thanks to a combination of proven designs, high quality and
meticulous precision, all these products
have been found to give excellent service.
With its longstanding experience in the
design and construction of industrial
plants, Uhde is in a position to engineer
and manufacture complete pilot and industrial-scale installations for high pressure
extraction using supercritical gases.
Uhde, moreover, attaches considerable
importance to operational safety.
Extractors of a production plant with automatic quick-acting clamp closure

CAE design of plants

Assembly and installation

The process engineering for a high pressure


extraction system is based either on test
results or on customer specifications. On
the process-development side, Uhde
works in close cooperation with both
industry and research establishments.
Using the latest analysis techniques, it is
possible to assess the product yield, and
therefore the closely linked factor of process economy, at an early stage. Uhdeengineered high pressure installations may
be designed for either manual or fully automated operation, the level of automation
depending on process requirements, operational safety and customer specifications.
The range of services offered by Uhde includes the process development, design
and construction of the system in compliance with all applicable regulations,
installation and commissioning as well as
the training of the operating personnel.

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Headline
Applications of Supercritical Fluids
Subheadline

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Supercritical fluids are applied for:


Extraction of valuable substances
- From spices, herbs and other plant
material
- For the food, cosmetics and pharmaceutical industry
Upgrading of raw materials
- Decaffeination of coffee and tea
- Pesticide removal from plant raw
materials and extracts
Purification
- Binder removal from construction
components
- Solvent recovery from synthesis
products
- Removal of contaminants from soil
Cleaning
- Parts cleaning
- Wafer cleaning
- Textile cleaning
Particle generation
- Microparticles and nanoparticles for
the pharmaceutical industry with
improved properties
Coating and impregnation
- Textile dyeing
- Coating of sensitive substances in
order to improve properties
Reaction
- Improvement of reactions
- New products by novel reactions for
the chemical and pharmaceutical
industries

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Advantages of supercritical CO2


1. Gentle treatment of temperaturesensitive natural substances
2. The products obtained are free of
solvent
3. Natural substances can be separated
without losing their aroma
4. Selective separation is possible
5. The dissolving characteristics of the
solvent can be varied by alterations
in pressure and temperature
6. Simple recovery of the solvent
7. No environmental-pollution problems
8. Low-energy solvent recovery because
CO2 has a lower evaporation temperature than most organic solvents
Supercritical fluids can replace conven9. High-purity extracts can be obtained
tional solvents such as methanol, ethanol,
in just a few process steps
methylene chloride etc. Because some of 10. Further on CO2 is:
the conventional solvents are toxic, efforts
a) Physiologically completely harmless
are now being made to avoid their use.
b) Germicidal
c) Non-inflammable
An alternative to these solvents is provided
d) No process-handling problems
especially by supercritical CO2. Substances
dissolve at a much higher rate in supercritical fluids than would normally be expected at a given vapour pressure. CO2
has proven to be especially well-suited
for the extraction of natural substances.
The low critical temperature of 31C allows
particularly gentle handling of natural substances. Moreover, CO2 is not only readily
available but may also be obtained at
relatively low prices.

Advantages of CO2

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08

200

150

supercritical

P
100

Temperature / C

gaseous

50

liquid

liquid-gaseous
-50
0,6

0,7

Entropy /

0,8

0,9

1,1

1,2

1,3

kJ
kg K

High pressure extraction can be used for


the separation of both solid and liquid
raw substances, the former being fed to
the extraction vessels in batches whilst
the latter are extracted continuously in
counter-current columns.
Liquid CO2 flows from the collecting vessel
D to the pump P which compresses it to
the required extraction pressure and transfers it to the heat exchanger E 1 where it
is heated up to the extraction temperature
and transferred to the extraction vessel or
column. The substances to be extracted
are dissolved in the CO2 as they pass
through the extraction vessel or column
C. The CO2, laden with the dissolved
substances, is then fed to the separator
S. By adjusting the pressure and/or temperature, the dissolving power of the CO2
in the separator is reduced, thus causing
the extracts to be precipitated. This may
take place in several stages, thereby allowing extract fractions of different qualities
to be obtained. The gaseous CO2 from
the separator is liquefied in a refrigerated
condenser and collected in the collecting
vessel D. The use of several extraction
vessels for the extraction of substances
in the solid state permits virtually semicontinuous operation.

E2

E3

E1

E4

Process diagram of an extraction system for solid materials

E2

E3

E1

E4

Process diagram of an extraction system for liquids

Process Description of Extraction


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Applications
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Industrial equipment
for the extraction of pepper and paprika
3 extractors
(500 l each)
2 separators
(375 l each)
1 separator with
175 l
Pressure
440 bar

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Production plant for the purification of biological material


2 extractors: 6 l each, operating pressure: 350 bar

Production plant
3 extractors: 3,500 l each
operating pressure: 500 bar

Pilot plant for dyeing synthetic fibers using supercritical CO2


dyeing autoclave: 30 l, operating pressure: 300 bar

Combined system for the extraction of solid and liquid materials


extractor: 10 l, column: inner diameter 70 mm

Applications
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Automatic quick-acting segment-type closure


diameter: 1,100 mm, extractor: 3,500 l, operating pressure: 500 bar

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Plant for contract extraction and process


development. 3 extractors: 360 l each,
operating pressure: 550 bar

Extraction facility for the decaffeination of tea


3 extractors: 3,000 l each, 2 adsorbers: 3,800 l each, operating pressure: 350 bar

Pilot extraction unit


1 extractor 4 l, 1 separator 4 l, operating pressure: 525 bar
CO2 flow rate: 30 kg/h

Clamp closure with a charging lock

Extraction column
inner diameter: 800 mm, effective length: 12 m
operating pressure: 500 bar

Special Equipment
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Stirrer-type reactor with a permanent-magnetic-stirred drive


volume: 100 l, operating pressure: 300 bar

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Separator for direct extraction with an internal heating coil

View of HP ball valves installed in a unit for


the expansion of spices

Ball valves
In order to prevent incrustations and to
reduce the ensuing pressure drop in HP
extraction units, Uhde has developed
special ball valves which are suitable for
use in units for processing natural substances at operating pressures up to
500 bar.
Direct expansion
For the separation of highly viscous
extracts, a separation system was developed in order to prevent the blocking of
pipes. Extracts are directly released into
the separation vessel which is equipped
with a heating device in order to set the
correct temperature.
Stirrer-type reactor
A stirrer-type reactor which allows the
suspension of the raw-material particles
in the supercritical medium was developed
for some applications, e.g. extraction or
coating.

Process Control
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Uhde
Remote
Support

Scada
Master

Scada
Backup

Ethernet
HUB2

Printer

Ethernet
HUB1

Modem

Tele
Service

S7-400
Main Control

S7-300
Cover Control
Profibus-DP

Panel

Process automation
The measuring, control and automation
system specially matching the prevailing
plant topology allows the simple and
faultless operation of the plant. The complete operating system comprises all the
necessary field devices such as sensors
and actuators, local panels, PLC system
as well as a central-computer-based
operation and viewing system.
The field devices are designed with process connections which are suitable for
food or are hygienic according to their use.
If combustible media are used, they have
an explosion-proof design. An efficient
field-bus system links the field devices to
the PLC system via so-called remote I/Os.
Wherever local operation is required (e.g.
for the filling or discharging of an extractor), appropriate operating panels are installed. Depending on the requirements,
parts of the plant (including the operating
panels) are manufactured in a clean-room
version.
The PLC system contains the complete
plant software, including the registration
of actual values, controls, sequences, interlocks as well as motor and valve controls. It is linked to the computer system
via a plant bus, usually Industrial Ethernet.
In order to improve the availability, the
computer system may have a redundant
structure with a master computer and a
back-up computer. The plant structure is
displayed clearly on the computer screens
in a form similar to P&I diagrams. Messages and requests for data input are displayed in plain language. The system
contains extensive diagnostic functions in

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PMA
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PMA
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3.0

3.1

4.0
Panel

PMA
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5.0

12.0
Drivecom
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P214

order to guide the operator to the affected


component in the case of a fault.
Basic functions of the computer system
are:
Display of actual pressure values, temperatures and flow rates
Indication of valve positions and status
messages
Recording and trend display of relevant
process data
Recipe management, i.e. input, modification and downloading of recipes into
the PLC
Batch protocols with all relevant data
Alarm-annoucning system
Hard copies of all computer screens
Teleservice via standard telephone line

PMA
42.0

Services
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Services
In addition to the supply of plants, Uhde
offers several services connected with
supercritical fluids and their application.
Process development
In cooperation with experienced institutes
and companies, processes are developed
from the first tests to the application on a
production scale. Process development is
accompanied by economic evaluation in
order to help the customer to take his decision in favour of installing a production
plant, even in an early state of development.
Equipment and plant design
and engineering
Equipment and plants are designed and
engineered in compliance with all the relevant regulations and standards. For the
pharmaceutical industry, these include DQ,
IQ and OQ according to cGMP and GAMP
guidelines according to the regulations
from FDA, EMEA or similar organisations.
Manufacturing
The equipment such as high pressure
vessels, heat exchangers, valves etc. to
be used in the plants is manufactured in
the Uhde workshops and is accompanied
by continuous quality control. Manufacturing is only completed when the equipment
has been accepted by authorities such as
TV or Lloyds and the fulfilment of the
regulations and specifications has been
certified.
Assembly and installation
Depending on the size of the plant, it is
completely assembled in our workshops
or is installed at the customer's site. Installation is carried out either by the customer's
personnel under the supervision of the
Uhde experts or completely by the Uhde
personnel.

Start-up and commissioning


Upon completion of the installation, the
plant is started up and commissioned
under the supervision of the Uhde experts.
Assistance for production after commissioning can be offered by the Uhde experts.
Training of plant operators
and maintenance personnel
During the manufacturing phase, the customer's personnel is trained by the Uhde
experts in our offices and workshops.
Training is continued during the installation
and start-up of the plant.

High pressure extraction

Bench-scale system

Comparison with extracts obtained


by conventional methods

Calculation and optimization


of process parameters

Analyses

Quality

Scale-up

Cost estimate

Costs

Process revision and optimization

Analyses

Quality

Production of sample extracts

Market tests

Scale-up

Capacity requirement

Decision

Pilot system

Product acceptance

Process selection

Decision

Production-scale
system

Cost calculation

Costs

Uhde High Pressure Technologies


a company with ASME/ ISO certificates
These certificates prove that we at Uhde
meet the requirements of the above
standards and are thus able to respond
to all demands of our customers on an
international level.

Our fabrication and supply programme:

Uhde High Pressure Technologies GmbH


Buschmuehlenstr. 20
58093 Hagen, Germany
Tel.: +49 23 31-967-0
Fax: +49 23 31-967-370
info @uhde-hpt.com
www.uhde-hpt.com

empeer 5/ 2003,
technical modifications reserved

HP pipes and isometrics


HP valves and fittings
HP pumps and compressors up to
14,000 bar
HP reactors and process equipment
HP autoclaves with stirrer drives
Bare-tube and fin-tube heat exchangers
designed as
- Multi-tube heat exchangers
- Double-pipe heat exchangers
- Shell-and-tube heat exchangers
- Suction heaters
Cooler, heaters, condensers, deaerators
HP extraction plants
HP pasteurisation plants
HP textile dyeing plants
Laboratory and experimental installations
HP intensifiers for aqua-jet cutting units