The Vapourtec High temperature fixed bed reactor has a stainless-steel column (Hastelloy as an option) contained within a thermally insulated manifold. The catalysts or reagents are packed into the stainless steel or Hastelloy column by the user. The packing materials are constrained within the column by frits.
The reactor is heated by either an R-Series or E-Series flow chemistry system. A temperature sensor accurately controls the outside temperature of the steel column in the range ambient to 250 °C.
In a typical application, the working fluid will be preheated in a tubular reactor before entering the high temperature fixed bed reactor and contacting the catalyst or reagents within the column. A cooling coil is supplied with the high temperature reactor to ensure the reactants exiting the reactor are reduced in temperature sufficiently before depressurising through a back pressure regulator.
Application examples for the High temperature fixed bed reactor
- Post cracking work-up of high value petroleum products
- Continuous flow hydrogenation
- Continuous flow hydration over a fixed bed
- Direct alkylation of N-heterocycles and amines
- α-Methylation of pyridines
- Click chemistry
- Heterogeneous or homogeneous reactions using Dowtherm solvents. E.g. https://pubs.rsc.org/en/content/articlelanding/2024/ob/d4ob00078a/unauth .
- Gould-Jacobsen reaction. E.g. https://www.sciencedirect.com/topics/chemistry/gould-jacobs-reaction
- Oxidations using manganese oxide. However extreme care should be taken to avoid strongly exothermic conditions.
High temperature fixed bed reactor – features
- Precise temperature control, ambient to 250 °C
- Pressure up to 50 bar
- The reactor volume is 3.8 ml. If a smaller volume is required for the active packed bed then celite can be used to fill the remaining void volume.
- “Post Cooling” tube to return products to a safe temperature before re-entering PFA tubing.
- Ideal for immobilised catalysts at high temperature conditions
- Precise temperature control
- Materials of construction for the fixed bed reactor are stainless steel 316 L, (Hastelloy® C276 also available upon request)
Safety
There are a few safety considerations when using these high temperatures. Vapourtec takes safety extremely seriously.
Firstly, reaction products exiting the system at 250 °C can present a hazard so is recommended that
- Either the cooling coil or another metal tube reactor set at a lower temperature is used after the column reactor as a cooling stage before products are depressurised and leave the system.
- Online quenching using a solvent is used immediately after the main reaction to reduce the temperature
Useful references (examples of possible applications)
https://www.mdpi.com/1420-3049/20/9/15797
https://pubs.acs.org/doi/10.1021/ol1026848 using Cu tubing, not column
https://pubs.acs.org/doi/10.1021/acs.joc.3c01788
https://pubs.acs.org/doi/10.1021/acs.oprd.3c00144
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