Design and Synthesis

We are fully equipped for the design and preparation of heterogeneous catalyst using conventional wet impregnation, incipient wetness and precipitation techniques. Following impregnation or precipitation our suite of synthesis facilities enable material calcination/conditioning, ball milling, sieving and reduction. Additional capabilities include the preparation of materials via microwave calcination and the separation using centrifugation.

Heterogeneous Catalyst Preparation

Impregnation:

The initial stages of impregnation and controlled drying are performed by rotary evaporation using a series of temperature and pressure controlled Bucchi Rotovapor R‑210 systems. Calcination: The calcination step, involving fixing of the metal precursor to the support by thermal activation, is perfomed via fluidisation in vertical quartz tubes. We have two custom designed facilities comprising both lenton and carbolite tubular furnaces. These units are all housed in vented hoods allowing material calcination/treatment to be carried out using toxic and flammable gases including H₂, CO and NO. Several additional tube and chamber furnaces (Carbolite CWF 1100 and Carbolite RHF1500) provide heating capacity up to 1200 °C

Precipitation:

Precipitaion: Our Mettler Toledo LabMax automatic lab reactor provides a route to heterogeneous catalysts via precipitation methods. Computer control can be used for developing and optimising bench scale preparations, allowing reaction data to be collected in real time. The LabMax functions as a continuously stirred tank reactor and can be used with a jacketed 0.6 L or 1 L glass vessel. Different stirrer options for the agitator motor (stirrer options include glass anchor/Hastelloy anchor / pitch blade stirrer) are possible, depending on the preparation requirements. Control can be achieved by temperature or pH via separate feed pumps

Microwave Synthesis:

Our CEM Discover S-Class microwave reactor can be used to carry out synthesis under pressurized (accommodates 10 mL, 35 mL and 80 mL pressure vials) and atmospheric conditions (accommodates up to 125 mL round-bottom flask). The system can operate up to a maximum temperature of 300 °C with a power output of 300 W. The reactor is equipped with an in situ camera and has automated pressure control. Affording faster reaction times compared to conventional heating methods the reactor has been used in the preparation of metal oxide nanoparticles (synthesis reduced to 30 minutes from 3 days) and the calcination of supported metal precursors (calcination time reduced from 10 hours to 5 minutes).

Centrifugation:

For the separation of precipitated solids we have a Sigma 2-16P Centrifuge that holds 6 × 50 mL/15 mL tubes in a fixed angle rotor operating up to 7800 rpm and a Minispin Eppendorf micro-centrifuge that holds 12 eppendorfs in a fixed angle rotor with a maximum speed of 13,400 rpm. Both units have digital speed and time control

Ball Milling:

A Fritsch planetary ball mill, Pulverisette 6, and a Fritsch vibratory sieve shaker, Analysette 3 Pro, are available for the control of solid particle size. An array of sieves permits separation of solid material into a range of size fractions from 2 μm to 2 mm.

Synthesis and handling of air sensitive materials:

Our extensive capabilities for the preparation and handling of air sensitive materials include three MBraun glove boxes (Unilab and Labmaster DP), fitted with freezer compartments for chemical storage, multiple Schlenk lines and a Radleys parallel reaction station. One of our glove boxes is also fitted with a gate valve that is used for the inert atmosphere transfer of solid materials directly to XPS and TEM instruments. For the synthesis of air sensitive materials using solution based chemistry, such as phosphines and organometallic complexes, dry and degassed solvents are generated by two solvent purification systems (MBraun).

Homogeneous Catalyst preparation

We are perfectly equipped to carry out the synthesis and characterisation of ligands and metal complexes, including the manipulation of very air and moisture sensitive compounds and pyrophoric reagents.

Our laboratories contain all the glovebox and vacuum line facilities required for the safe and efficient handling of ligands and metal complexes. We have multiple facilities for automated solvent purification as well as the ability to link synthesis and characterisation facilities without compromising the integrity of the samples.

Computational capabilities:

The wealth of experimental techniques at the St Andrews facility is complemented by state-of-the-art computational methodologies using a compute cluster (9×BL460c G7 blades with 2×6-core i7 CPU’s). We apply a wide spectrum of sophisticated computational techniques including various flavours of DFT, time-dependent DFT, many-body perturbation theory (MPn), methods based on random-phase approximation (RPA), highly correlated coupled cluster methods, like CCSD(T), but also COSMO-RS for the adequate simulation of bulk solvent effects and to predict fluid thermodynamic data. Our expertise in the skilful application of these theoretical methods broadly covers theory-based rational catalyst improvement & design, computational spectroscopic characterisation of reactive intermediates and computational fluid thermodynamics.

Distillation:

Our Fisher Technology Spaltröhr HMS 500 AC rig is a fully automated distillation apparatus capable of processing volumes from 50500 mL. The operating conditions span from atmospheric pressure down to 1 mbar over the temperature range RT to 400 °C. The unit is fully heat traced to allow distillation of heavy products, which are solids at RT. Fraction collection volumes can be adjusted between 160 mL and collection is fully automated.