supercritical fluids example
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Uhde High Pressure TechnologiesA company
of ThyssenKrupp
Technologies
TK
Supercritical FluidsTechnologies and Plants
CO2
Process Engineering and Plant Construction
High-precision machining of an HP extractioncomponent on a CNC-operated horizontalboring mill
02
Uhde High Pressure Technologies manu-
factures a broad range of components for
high pressure installations.
These products include autoclaves, react -
ors 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 combi-
nation 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 in -
dus trial-scale installations for high pressure
extraction using supercritical gases.
Uhde, moreover, attaches consider able
im portance to operational safety.
Extractors of a production plant with automatic quick-acting clamp closure
03
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 pro-
cess economy, at an early stage. Uhde-
engineered high pressure installations may
be designed for either manual or fully auto -
mated operation, the level of automation
depending onprocess requirements, ope rat -
ional safety and customer specifications.
The range of services offered by Uhde in -
cludes the process development, design
and construction of the system in compli-
ance with all applicable regulations,
installation and commissioning as well as
the training of the operating personnel.
Assembly and installation
CAE design of plants
HeadlineSubheadline
Applications of Supercritical Fluids04
05
Supercritical fluids are applied for:• Extraction of valuable substances
- From spices, herbs and other plant
material
- For the food, cosmetics and pharma-
ceutical 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
06
Advantages of supercritical CO2
1. Gentle treatment of temperature-
sensitive 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
CO
2
has a lower evaporation tempera -
ture than most organic solvents
9. High-purity extracts can be obtained
in just a few process steps
10. Further on CO
2
is:
a) Physiologically completely harmless
b) Germicidal
c) Non-inflammable
d) No process-handling problems
Supercritical fluids can replace conven-
tional solvents such as methanol, ethanol,
methylene chloride etc. Because some of
the conventional solvents are toxic, efforts
are now being made to avoid their use.
An alternative to these solvents is provided
especially by supercritical CO
2
. Substances
dissolve at a much higher rate in super-
critical fluids than would normally be ex -
pected at a given vapour pressure. CO
2
has proven to be especially well-suited
for the extraction of natural substances.
The low critical temperature of 31°C allows
particularly gentle handling of natural sub -
stances. Moreover, CO
2
is not only readily
available but may also be obtained at
relatively low prices.
07
Advantages of CO2
08
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 CO
2
flows from the collecting vessel
D to the pump P which compresses it to
the required extraction pressure and trans -
fers 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 CO
2
as they pass
through the extraction vessel or column
C. The CO
2
, laden with the dissolved
substances, is then fed to the separator
S. By adjusting the pressure and/or tem-
perature, the dissolving power of the CO
2
in the separator is reduced, thus causing
the extracts to be precipitated. This may
take place in several stages, thereby allow -
ing extract fractions of different qualities
to be obtained. The gaseous CO
2
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 semi-
continuous operation.
E2
E1 P E4
E3
C S D
E2
E1 P E4
E3
C S D
Process diagram of an extraction system for solid materials
Process diagram of an extraction system for liquids
Tem
pera
ture
/°C
0,6 0,7 0,8 0,9 1 1,1 1,2 1,3
liquid-gaseous
liquid
supercritical
gaseous
P
-50
0
50
100
150
200
D
S
C
Entropy / kJkg K
09
Process Description of Extraction
Applications
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
10
11
Production plant for the purification of biological material
2 extractors: 6 l each, operating pressure: 350 bar
Pilot plant for dyeing synthetic fibers using supercritical CO
2
dyeing autoclave: 30 l, operating pressure: 300 bar
Production plant
3 extractors: 3,500 l each
operating pressure: 500 bar
Combined system for the extraction of solid and liquid materials
extractor: 10 l, column: inner diameter 70 mm
12
Applications
Automatic quick-acting segment-type closure
diameter: 1,100 mm, extractor: 3,500 l, operating pressure: 500 bar
13
Extraction facility for the decaffeination of tea
3 extractors: 3,000 l each, 2 adsorbers: 3,800 l each, operating pressure: 350 bar
Plant for contract extraction and process
development. 3 extractors: 360 l each,
operating pressure: 550 bar
Pilot extraction unit
1 extractor 4 l, 1 separator 4 l, operating pressure: 525 bar
CO
2
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 Equipment14
Stirrer-type reactor with a permanent-magnetic-stirred drive
volume: 100 l, operating pressure: 300 bar
15
Ball valvesIn order to prevent incrustations and to
reduce the ensuing pressure drop in HP
extraction units, Uhde has developed
spe c ial ball valves which are suitable for
use in units for processing natural sub -
stances at operating pressures up to
500 bar.
Direct expansionFor the separation of highly viscous
extracts, a separation system was devel -
oped 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 reactorA 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.
View of HP ball valves installed in a unit for
the expansion of spices
Separator for direct extraction with an internal heating coil
16
Process Control
HUB2
Ethernet
HUB1
Ethernet
S7-400Main Control
Printer
ScadaMaster
ScadaBackup
TeleService
Modem
UhdeRemoteSupport
Profibus-DP
S7-300Cover Control
Panel
2.0
Panel
3.0 3.1
4.0
5.0
11.0 11.1
12.0
14.0 14.1 14.2
Drivecom13.0
P214
PMA11.0
PMA12.0
PMA41.0
PMA42.0
1.0
17
Process automationThe measuring, control and automation
system specially matching the prevailing
plant topology allows the simple and
faultless operation of the plant. The com-
plete 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 pro-
cess 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 extract -
or), appropriate operating panels are in -
stalled. 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, in -
terlocks as well as motor and valve con-
trols. 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. Mess -
ages and requests for data input are dis -
played in plain language. The system
contains extensive diagnostic functions in
order to guide the operator to the affect ed
component in the case of a fault.
Basic functions of the computer system
are:
• Display of actual pressure values, tem-
peratures and flow rates
• Indication of valve positions and status
messages
• Recording and trend display of relevant
process data
• Recipe management, i.e. input, modifi-
cation 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
18
Services
19
ServicesIn addition to the supply of plants, Uhde
offers several services connected with
supercritical fluids and their application.
Process developmentIn 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 de -
cision in favour of installing a production
plant, even in an early state of develop-
ment.
Equipment and plant design and engineeringEquipment and plants are designed and
engineered in compliance with all the re -
levant 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.
ManufacturingThe equipment such as high pressure
vessels, heat exchangers, valves etc. to
be used in the plants is manufactured in
the Uhde workshops and is ac companied
by continuous quality control. Manufactur -
ing is only completed when the equipment
has been accepted by authori ties such as
TÜV or Lloyds and the fulfilment of the
regulations and specifica tions has been
certified.
Assembly and installationDepending on the size of the plant, it is
completely assembled in our workshops
or is installed at the customer's site. Instal l -
ation 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 commissioningUpon completion of the installation, the
plant is started up and commissioned
under the supervision of the Uhde experts.
Assistance for production after commis sion -
ing can be offered by the Uhde experts.
Training of plant operators and maintenance personnelDuring the manufacturing phase, the cus t -
omer'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 Comparison with extracts obtainedby conventional methods
Bench-scale system
Calculation and optimization
of process parameters
Analyses Quality
Decision
Pilot system
Process revision and optimization
Production of sample extracts
Analyses
Market tests
Scale-up
Capacity requirement
Product acceptance
Process selection Cost calculation
Costs
Decision
Production-scale
system
Quality
CostsCost estimate
Scale-up
Uhde High Pressure Technologies GmbHBuschmuehlenstr. 20
58093 Hagen, Germany
Tel.: +49 2331-967-0
Fax: +49 2331-967-370
info
@
uhde-hpt.com
www.uhde-hpt.com
empeer 5/2003,
technical modifications reserved
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:
• 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
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