Recipe control of automated reactors in R+D labs

Recipe control is a must for efficient process control and easy handling of batch operations in R+D but manual operations must be feasible at the same time

The automation of reaction plants is a prerequisite for a safe and reproducible operation and data from automated research reactors is applicable for the scaling up of processes.

Automated laboratory equipment has to be adaptable to the specific needs and capabilities of any particular laboratory.

Firstly, in many instances laboratory staff have no specific knowledge of or experience in process automation.

Secondly, R+D needs a high degree of flexibility in the handling of the system.

Automation systems designed for production do not offer this flexibility.

The paper NA27 of Namur recommends that parameters and even the configuration of the process in research and development are changeable during operations and that staff without expertise in automation are able to perform these modifications.

Recipe editor.

The demands for easy handling and high flexibility are satisfied by a recipe control system for batch operations.

The control is realised by a sequence of so-called unit operations according to the Namur recommendation NE33.

Unit operations are basic laboratory operations, like dosing, tempering, stirring, distillation, crystallisation and others.

These unit operations are combined in series or parallel with a graphic editor.

Connected to build a recipe they represent and document a distinct reaction process.

Thus laboratory staff are able to program a complex synthesis procedure in a few minutes.

Unit operations may be used several times in one recipe.

After compiling, the desired values of temperatures, heating rates, dosing rates, pressures and so on are assigned to the recipe.

Recipe and parameters are stored independently from each other.

So, different sets of parameters may be stored for each recipe.

Decisions, conditional branches or counter loops are also realized with graphic elements.

A unit operation library fits all the requirements of the daily work in the laboratory.

Customised unit operations may be programmed if required and incorporated in the library.

Plant visualisation.

The progress of the recipe may be monitored in the recipe plan or on the plant operation console.

This user interface is designed for manual control, eg, when starting the plant, and to monitor the actual plant status and measured values.

On parallel reactor systems a recipe can be assigned to different reactors.

Each reactor may work with different reaction parameters or with different recipes at one time.

The process control hardware is the HiTec-Zang Lab-manager.

The Lab-manager is a standalone automation device with high reliability.

The compact device contains the electronics of a control cabinet and may be mounted near to the reactor and even in the fume hood.

The Lab-manager is developed in close collaboration with R+D laboratories according to the recommendations of Namur NE28.

Connections to laboratory equipment are realized by standardised plug connectors.

Nearly every sensor, actuator or laboratory device may be connected with these plugs.

For the visualisation and handling, for data storage and analysis , a PC with Windows XP and LabVision process control software is supplied.

This split-up of tasks combines the performance of the PC with the reliability of automation systems.

The LabVison software module KalDas supports reaction calorimetry.

Heat flow or heat balance calculations are possible.

Reaction calorimeters based on LabVision are not constricted to calorific experiments, they have all the potential of a automated laboratory reactor.

Additional instrumentation.

HiTec-Zang offers a wide range of laboratory equipment for laboratory reactors.

Unique is the gravimetric liquids dosing system GraviDos.

It consist of a sample vessel suspended on a load cell and a solenoid valve.

Due to its simple setup it is inexpensive and robust compared to a system composed of balance and pump.

ViskoPakt is a series of measurement stirrers with maximum torque values between 10 and 110Ncm.

The precision torque measurement stirrers ViskoPakt rheo features a high torque resolution - even fractions of the water viscosity are measured.

Both series are distinguished by very small dimensions - the space used at the top of the reactor can be critical.

The reliable and precise dosing of solids is one of the most challenging problems in the laboratory.

SoliDos solids dosing device doses powders and granulates reliably even in condensing atmospheres.

The isolation of liquid phases, e.g when draining the reactor, is possible with the aid of the PhaDec phase interface detector.

PhaDec discriminates following the heat conductance of the liquids.

Hence the phases need not be conductive or transparent.

Dosing of small volumes or automatic sampling from the reactor is possible with the AutoSam liquid handling system.

AutoSam is available for sample volumes between 1 and 2000ml.

Other options enable the construction of complex automatic laboratory or pilot plants, including the whole range of plants for R+D.

These options also include sample preparation, in-situ molecule spectroscopy and product work-up.

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