The ICES kilo laboratory supports work in scale-up and process innovation. There are two main processing areas: one for chemical processing and one for solids processing. These share a control room which houses the control systems and meeting room for staff. There is also a well equipped development laboratory.

The processing areas are suitable for operation in explosion-proof mode so that flammable materials can be handled. The area operates under mild negative pressure and contained addition/discharge is possible (as well as a range of PPE) to allow handling of toxic materials. All processing is rigorously assessed before implementation through both laboratory testing (calorimetry) and process studies such as HAZOP. Access control prevents unauthorised entry to the processing areas.

A core range of utilities and services are available: one for chemical processing and one for solids processing. These share a control room which houses the control systems and meeting room for staff. There is also a well equipped development laboratory. 

Chemical processing

In the chemicals processing area we have a 60L scale batch processing facility comprising three 60L and one 30L Hastelloy vessels. The system is primarily manually operated for flexibility with some automated capabilities and the capability to add extra automatic control if required. The system is readily reconfigurable to accommodate a range of chemical processing operations, and has the following capabilities:

• Heating and cooling capability - heating to 120^oC and cooling to -20^oC using recirculating temperature - controlled heat transfer fluid;
• SCADA-controlled loss in weight addition and temperature profiling/control;
• Overhead condensation, phase separation and reflux;
• Agitation using angle-bladed turbines;
• Flexible installment of various diplegs and blowlegs;
• Nitrogen blanket;
• Pressure range full vacuum to 5 barg;
• Easy deployment of a variety of in situ PAT devices - Raman, FTIR, PVM, FBRM and other devices can be deployed. 

The chemicals processing area also houses ICES' innovative multipurpose continuous processing facility. This has a plug-and-play design, with a range of processing skids design to carry our different tasks. The systems are built for a nominal flow of up to 20L/hour so as to give comparable processing capability to the batch system. The skids can rapidly be configured to deliver a wide range of chemical processing. These continuous systems are computer-controlled, and also have access to the same range of PAT devices. We have several skids operational and others under construction:

• Feed skids to control the flow of several materials, combined with mixing capabilities;
• Oscillatory baffled reactor (Nitech);
• Wiped film evaporator (Pope);
• Heat transfer skid;
• 5L stirred tank.

The continuous and batch systems can also be operated together as a hybrid processing system.

Solids processing and formulation

The solids hall houses a variety of processing and formulation equipment for the growing activity in secondary and formulation processing.

• A Rosenmund filter-dryer complements the batch reactor system;
• DEC solids transfer systems to allow hygienic/contained transfer of solids;
• A twin screw extruder;
• A Consigma (GEA) twin screw granulator (from July 2011);
• A 5L scale homogeniser.

Development laboratory

The development laboratory not only houses a wide range of process development equipment but also the analytical equipment to support process operation in the Kilo Lab. Calorimetry (Mettler RC1 and APTAC) provide the basis for thermal safety assessment as well as kinetic studies. 

We have a range of glass reactors up to 10L in volume that can be used for development as well as a Mettler Multimax that allows rapid process development and optimisation through multiple parallel experiments. We also have equipment suitable for laboratory scale flow processing.

The PAT equipment from the processing areas can also be deployed in the development laboratory both for process development and to test the potential value of the measurements for process operation. The normal analytical equipment (GC-MS, HPLC, Karl Fischer and a VLE still) is available in the laboratory while the exceptional analytical capabilities of ICEs are available nearby.

Control and process understanding

The Kilo Lab has a variety of connected control and PAT equipment that provides a platform for development of new approaches to process monitoring and control. The data management is overseen by a Siemens Sipat system which captures data from both of the control systems and any PAT devices. Chemometrics can be carried out on-line or data can be sent for more complex analysis elsewhere in ICES. 

The Kilo Lab and its associated control and software systems give us an outstanding environment to be able to demonstrate process monitoring and control on real systems, but in a safe and cost-effective way.