Scale Up

In many scenarios, single reaction volumes of more than 100 ml are required. Although these volumes and beyond can easily be accommodated in reflux glassware, open to atmospheric pressure conditions, there are many distinct advantages to performing reactions in a closed vessel. These advantages derive from the ability to operate at temperatures significantly above the normal boiling point of the the reaction mixtures, and to accommodate safely the corresponding elevated vapor pressures.

Milestone's Batch Reactor, designed to work with the MicroSYNTH Labstation, is inserted into the multimode cavity through the top of the labstation. It offers the following features and benefits:

• The batch reactor supports closed-vessel operating pressures to 14 bar (203 psig). This can facilitate reaction temperatures significantly above the normal boiling point of the reaction mixture without loss of solvent or volatile fractions through evaporation.

Reactor Material	Liner: PTFE-TFM Cold finger: stainless steel
Reactor Volume	Total: 300 mL With cold finger: 250 mL
Max. Temperature	230 °C
Max. Pressure	30 bar  (435 psi)

• The batch reactor design provides valved access into the reactor, resulting in safe access to the reaction mixture to add or remove materials.
• Reaction temperature and pressure monitoring is integral to the batch reactor platform. Reaction temperatures are monitored using an immersed thermocouple, while vapor pressures over the reaction mixture are monitored with a pressure transducer. Accurate monitoring and precise temperature/pressure feedback control is achieved using the easyWAVE software, resulting in reproducible reaction temperature conditions, ± 1 °C precision, and ± 0.1 bar pressure conditions.
• Controlled reaction temperatures to 200 °C, and controlled reaction pressures up to 14 bar (203 psig) are possible.
• The batch reactor design incorporates a fluid-cooled vapor phase cooling device, to allow efficient quenching of completed reactions.
• A variety of reactor volumes and vessel materials are available. These are interchangeable and reusable, providing maximum flexibility.
• Stirring ensures homogeneous reaction mixtures, even bi-phasic mixtures of liquids and slurries. Ordinary magnetic stir bars can be used in the batch reactors, in conjunction with the variable speed stirring available in every Ethos MicroSYNTH Labstation, or a paddle stirrer can be accommodated for viscous mixtures.
• Milestone's unique Weflon buttons and stir bars, when introduced in the batch reactor, facilitate microwave heating, even of non-microwave-absorbing reaction mixtures.
• The facility to create a controlled-intensity mercury vapor spectrum, to induce photochemical reactions in the batch reactor, can be achieved by substituting an electrodeless plasma lamp for the cold finger.

 

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