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Auto Lab

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Auto Lab

Uploaded by

pssvasan108
Copyright
© © All Rights Reserved
Available Formats
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AUTOMATED BENCH &

PILOT SCALE REACTORS


TAILOR-MADE DESIGNS

AUTO-LAB™
Hazard Evaluation Laboratory
The features you want... the way you want them. Automated Chemical Reactions
AUTO-LAB™ is a turnkey solution to synthetic
chemistry automation, consisting of commonly
used laboratory equipment (such as reactors,
pumps, heaters, valves...), assembled to
perform important process R&D tasks,
controlled and monitored by dedicated
software running from a standard PC. The
primary applications are for bench and pilot
scale chemical reactors (volume ~ 0.25 to 100
litres) in the fine chemical and related
industries.

Whether you are looking for increased


productivity by having unattended round the
clock operation, operator independent
reproducibility or permanent recorded data
from your chemical process, the AUTO-LAB™
provides you with a turnkey dedicated solution.

Applications are virtually unlimited, and to date


we have supplied systems for hydrogenation,
polymerisation, cascade, continuous flow and
even solid phase reactors.

Each AUTO-LAB™ system is assembled


specifically for the application in question. The
reactor, the heater/chiller, the reagent feeds
and even the sensors are all selected to exactly
suit the chemistry in question.

The equipment is interfaced with winISO, our


in-house developed Windows NT/98 software
that provides powerful yet simple to operate
interface.

Better Processes - Faster


Every chemical process is different and each
user is unique, yet winISO allows recipe
programming in seconds with minimal training.
All control loops can automatically be set up
without user programming or tuning unless
required.

All data is automatically logged, all the time, and


displayed on-line as well as being available for
off-line analysis and archiving.

Our unique and modular electronics allows the


creation of a system designed for your process
as it stands today. However, as your research
demands grow, so the AUTO-LAB’s capabilities
are expanded with additional sensors, probes,
reagent feeds. Reactors can be changed and
even calorimetry is available as an upgrade.

2 3

What AUTO-LAB can’t do, can’t be done!
List of
Mimic with experimental
display of steps
Numerical data display
Reactors Software key data

Whether you wish to use an “off-the shelf” Working under Windows 98 or NT, winISO

reactor, or you want us to develop a geometry
specific for your application, the options on
WHY AUTO-LAB ? software is designed to allow even untrained
operators to develop an experimental plan
reactors are almost endless. quickly.
▲ INCREASED PRODUCTIVITY: A plan consists of a series of steps, in the form of
This includes atmospheric and mid-pressure glass menu cards, in which the user enters the
Complete control of all
reactors, stainless steel, specialist alloy and even controls for each equipment item (heater, pump,
glass lined stainless steel reactors. Pressure variables allows for totally stirrer, etc.). Progress through the next steps
capabilities come in a series of steps of 20, 60, may be based on time or a sensor value.
unattended operation. Complex logic statements may also be used to
100, 200 and even up to 350 bar maximum.
terminate steps. Moreover, it is possible to jump Real-time Set of controls
interactive of step being
steps and even loop back to previous ones.
▲ IMPROVED SAFETY: graphics executed

Above: High pressure reactor.


Operating Range
Every variable is Above: The winISO software package, makes
operation simple.
Below: Pump and balance (liquid dosing). Temperatures from -80°C to 350°C (500 °C monitored and can be set Modification Of Tests
optional) and pressures from vacuum to 350 bar. Below: Graphical overview of winCALC.
with user-defined alarms, A plan can be modified while a test is running.
Steps can be deleted, new ones added or just
terminations and shut control conditions changed. All changes are fully
Feeds
down conditions. documented by winISO.
Gas, liquid and solid feeds are all available with
full computer control. Liquid and solid addition is
normally based on weight loss off a balance,
▲ UNLIMITED POSSIBILITIES: Multiple Reactor Control
while gas is added using a mass flow sensor From the ground up this
Any number of totally independent or related
and/or reactor pressure. The software can
control feeds to be constant over the reaction
is your system, from systems can be controlled from the same PC.
This could for example be a series of separate
time, to be event determined or even linked with reactor volumes and vessels, to save space and cost, or a cascaded
a sensor to control a parameter such as pH,
pressure, temperature etc.
chemical resistance to reactor system.

interdependent cascade
reaction systems. Data Obtained
Controls & Sensors
The user can choose to view and record any
▲ Temperature (heat, cool, isothermal) using ▲ FLEXIBILITY: number of available sensor values as well as
circulating oil or electrical heating derived parameters (such as rates of change,
Assemble a system that controller outputs, set points). WinCALC
▲ Pressure (vacuum or overpressure)
exactly matches your software is provided for off-line calculations,
▲ Mass flow (gas) sensors graphical output, polynomial fitting, etc.
requirements safe in the Above: Reflux condenser and distillation column
▲ Pumps (peristaltic, diaphragm, syringe)
(vacuum jacketed and silvered with reflux control).
▲ Solids feed
knowledge that additional
Safety
▲ Control valves (liquid, gas)
feeds, reactors and
▲ Electric motors (e.g. stirrers, pumps, valves)
sensors can be added at An essential feature of any unsupervised system
Above: Solids feeder (on balance).
is the safety measures. The AUTO-LAB™
▲ Liquid level any time. allows you to monitor and set alarm conditions
Right: on any of the sensors, allowing you to shut
High pressure ▲ pH, conductivity, turbidity...
down the system or to demand operator
pH probe.
▲ Gas addition and gas evolution meters DON'T CONFIGURE YOUR supervision. In the event of any loss of
communication the system automatically reverts
Left: ▲ 4-20mA, 0-10 volts and serial communications CHEMISTRY TO SUIT YOUR to your predetermined safe state - for example
FTIR probe. ambient temperature without feeds, but with
EQUIPMENT - SELECT THE agitation. Above: Various stirrers.

AUTO-LAB TO SUIT YOUR

4
CHEMISTRY. 5
Challenge Us: Describe Your Process & We’ll Automate It.....
Crystallisation Research EACH REACTOR Cascade Reaction System
pH CONTROL 5 LITRE, DOUBLE JACKETED
A INDEPENDENT CONTROL OF;
pH
PH,
For the investigation of crystal formation and polymorphism a B TEMP, A client wished to research his process using a cascade
LEVEL,
client required an automated 2 litre reactor with precise AGITATION, reaction system, which presented us with a number of
temperature control and a number of different in-situ FLOW. challenges. To allow full control of the system, the two
monitors. L pH
reactors needed totally independent temperature control
LEVEL and level sensors to operate under aggressive environments.
These monitors, including pH, turbidity, and FTIR and all L

outputs are displayed live on the screen during operation, and The reagent feed into the upper reactor, the flow between
FLOW
can be used as a control function for liquor feeds, agitation or LEVEL CONTROL
CONTROL the reactors and the product draw-off are all monitored and
any other control parameter. In addition a series of sampling controlled by the software to enable detailed study of control
ports were incorporated in the reactor to allow the sample parameters effecting product yields and quality.
to be removed and analysed on an XRD spectrometer. HIGH T PUMP

Each of the reactors can also be run in batch or semi-batch


mode.

STIRRER
REAGENT A
Solid Phase Chemistry Polymer Chemistry

A customer was working with an active substrate bonded on A pilot plant for value added polymers, with a varied and
pH

LEVEL
the surface of polymer beads. They turned to us to reduce complex recipe was required. This included two separate gas
SOLVENT PUMP
L
both reaction steps and flushing whilst minimising the amount additions and six different liquid feeds of different volumes
SOLVENT of expensive reagents used. and precision.
SELECTION
MANIFOLD REAGENT B
T
We developed a reactor with an inbuilt sintered filter, The 20 litre metal reactor, with an electrical lifting jack, was
automatic bottom outlet valve, a level sensor/controller and fully automated, together with alarms and sensors for
WASH SOLVENTS
UV-VIS custom geometry to minimise reagent volume. flammable gas leaks, high temperatures and high pressure.
Other features included solvent leak sensors, torque
The customer can now complete all chemistry and sample measurement on the agitator and emergency venting
washing without supervision and with a reduced quantity of procedures.
WASTE RECYCLE
high value reagents.
Fast feeds with minimum overshoot; precise feed rate and
Several 1 to 10 litre units have now been supplied. temperature profiles; pumping of volatile and pyrophoric
liquids were some of the more unusual features.

Plug Flow Reactors (Flow Through) Semi-Batch Process - General Purpose

GAS FEED CONTROL


AUTO-LAB™ is easily adapted to catalyst research and This is the most typical version of AUTO-LAB™ : a batch
H2 Air N2
FIXED BED
CATALYTIC P
PRESSURE CONTROL other investigations of continuous plug flow reactions. or semi-batch reaction process in a jacketed, stirred vessel.
PREHEATER
REACTOR
COOLER SAMPLE The stirrer speed is controlled and motor current (or torque)
TO GC
This elaborate unit, operating up to 100 bar and 400°C logged to permit semi-quantitative monitoring of viscosity
TEMPERATURE
PRODUCT included simultaneous addition of three gases and two liquids. change.
LIQUID FEED
CONTROL The mixed stream was preheated and then passed over fixed
CONTROL
BALANCE bed catalysts in stainless steel and titanium reactors. The Most units are equipped with liquid dosing by weight loss
product was cooled, vapour and liquid separated and the feed-back from a balance, sometimes multiple pumps. pH
sample collected for GC analysis. control by one of the pumps is an option. Occasionally
automatic powder addition has been included. Operation
under reflux is common as is fractional distillation with
control of reflux ratio. For best results, glassware can be
supplied silver coated and jacketed.

Complete units inclusive of heater/chiller to suit required


operating range completes a typical specification.

6 7
Hazard Evaluation Laboratory
HEL offer a comprehensive range of products and services for the modern process chemistry
and process safety laboratory. Our computer controlled reactor systems and
calorimeters are designed for the safe and efficient development and
optimisation of chemical processes. The acknowledged technical
strengths of HEL are complimented by Consultancy
Services that include specialist testing and
advice on a confidential basis.

Consultancy & Testing Services


Process & Reaction Hazard Evaluation
Process Research and Development
Reactor Relief Systems/Vent Sizing
Fire & Explosion Testing
Continuing Education

Other Products
Miniature Multiple Reactor System
(auto-MATE™)

Automated Batch Reactors


(AUTO-LAB junior™)

Reaction Calorimetry
(SIMULAR™)

Adiabatic Calorimetry
(PHI-TEC™)

Thermal Screening Unit


(TS U)

www.helgroup.co.uk
[email protected]

Hazard Evaluation Laboratory Limited Hazard Evaluation Laboratories Inc.

50 Moxon Street, Barnet, Princeton Corporate Plaza,


Hertfordshire, EN5 5TS. 1 Deer Park Drive, Suite L,
England. Monmouth Junction,
New Jersey 08852-1921, USA.
TEL: +44 (0) 20 8441 6778
FAX: +44 (0) 20 8441 6754 TEL: +1 732-329-3090
E-MAIL:[email protected] FAX: +1 732-329-3023
WEB:www.helgroup.co.uk E-MAIL:[email protected]

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