Lab scale Systems

Case Studies

Customer: University of Cambridge, UK

Project: NMR/MRI Catalyst Testing System

Project Description:

In 2011, Zeton was invited by the University of Cambridge's Department of Chemical Engineering and Biotechnology to discuss and review the options for using Magnetic Resonance techniques in a lab scale catalyst testing system. The ultimate objective was to develop magnetic resonance techniques that can be used to spatially map chemical composition, concentration gradients, temperature, and gas and liquid flow profiles within a working reactor. The system was to be capable of testing scaled-down industrial reactors as well as microchannel reactors across a range of sizes and scales.

The catalyst testing system consists of a traditional trickle bed reactor design with three gas feed systems, each equipped with parallel mass flow meters for a high rangeability in gas feedrate. The liquid feed is delivered by a HPLC pump under mass flow control. The system design allows for connections to a wide range of different gas and liquid feeds. The reactor is operated at elevated temperatures and pressures in either up or down flow mode. A gas/liquid separator and product collection vessel are installed downstream of the reactor.

A unique design characteristic of the NMR/MRI catalyst testing system is in the way the Magnetic Resonance Magnet is integrated into the pilot plant. This required a special non-metallic reactor section operating at high pressures and temperatures, with localized heating.

Design and Build Summary

The University of Cambridge invited Zeton to participate in early stage discussions. In Phase I of the project, both parties worked collaboratively to develop the P&IDs based on a preliminary PFD and process description provided by the University. While the design of the feed, separation and the product collection sections was relatively straightforward, an extra degree of attention was required to solve the reactor design challenges presented by this project.

When integrating a reactor section into a NMR spectrometer, several design criteria have to be met. Firstly, there is the temperature difference between the NMR spectrometer and the process area. For kinetic experiments, it is essential to accurately control this temperature difference. The second, and more difficult challenge, is the non-metallic/non-magnetic requirements in the near vicinity of the NMR magnet. Only through the close and innovative collaboration between the University of Cambridge, Zeton and several key equipment suppliers were these challenging design criteria met.

To minimize the interference between the process section and the magnet, the process system was built separately from the reactor section, with the two being connected via a "pipe bridge". Non-magnetic stainless steel tubing and tracing was used as far as possible into the NMR magnet. However, the center of the magnet had more stringent restrictions, requiring both non-metallic and non-magnetic materials. After an intensive study of alternatives, the team designed and built a special ceramic reactor for use under high pressure and high temperature conditions. This is the first time that the University of Cambridge or Zeton has implemented this type of reactor design in a lab scale system.

Once the reactor fabrication technology to be used in the project had been agreed, the NMR/MRI catalyst testing system was completed using Zeton's fast-track project execution methodology.

"This is a very exciting development in our collaboration with Cambridge. For the first time we can use NMR techniques to follow a catalytic reaction under real operating conditions, and gather information on catalyst performance across a range of length scales", Dr. Andrew York, Johnson Matthey Technology Centre.

Technical Specifictions:

  • A wide range of gas and liquid feeds
  • Liquid feed flow rate 2.5 - 125 ml/h
  • LHSV Max/min 10 - 0.2
  • GHSV Max/min 5000 - 5
  • Design pressure 30 barg
  • Design temperature 350 °C
  • Control system is LabVIEW from National Instruments

Customer Quote:

"We have really appreciated the interactive nature of the design and development for this unit and the novel solutions that Zeton has used when facing very difficult challenges. We have ended up with an excellent piece of integrated equipment that has exceeded expectations on the design and control front. Zeton has built this research equipment to specification and in a challenging and unique way", Andy Sederman, Project Manager, University of Cambridge.