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