Batch Autoclave Reactor Systems

In addition to continuous systems used primarily for moderate-pressure liquid-phase reactions, the EERC also houses a number of batch autoclave systems ranging in size from 250 cm³ up to 2 gallons. These reactors are used when very high pressures are required or when the feed is a solid or slurry. The reactors ranging in size from 250 cm³ to 1 liter can be used at pressures and temperatures up to 5000 psig and 932°F (500°C). The 1-gallon autoclave is rated to 5100 psig and 950°F (510°C), and the 2-gallon autoclave is rated to 5500 psig and 650°F (340°C).

The 250-, 500-, and 1000-cm³ reactors are all equipped with magnetically driven mixing impellers and baffles; diptubes for gas inlet or liquid sampling; PID (proportional-integral-derivative)-controlled water cooling; headspace ports for gas venting and liquid addition; thermocouples for monitoring the heater, liquid, and gas temperatures; condensers; and inline vent traps for bubbling product gas through liquid scrubbing solutions. The 1-liter reactor is also equipped with a bottom drain for removing liquid without opening or lifting the reactor. All gas and liquid feed can be metered into the reactors manually or by computer control from behind a blast wall. Gas can be automatically metered into the reactor to maintain a pressure set point when constant pressure is required in a gas-consuming reaction.

The 1- and 2-gallon reactors are equipped with heaters, gas fill and vent lines, and a vacuum pump to assist in venting or to run reactions at below atmospheric pressure. Vent lines run to a water-cooled condenser for collecting volatile product. The 2-gallon autoclave is heated in four separate bands to help maintain constant temperature throughout. This reactor is stirred by a belt-driven water-cooled mixer with two propellers and an impeller along the shaft length. The 1-gallon autoclave is heated by a single-zone heater. The 1-gallon reactor can be run with or without a mixer and is equipped with a bottom drain for liquid removal. Both reactors are equipped with thermocouples at top and bottom for monitoring the temperature of both the vapor and liquid phases.

Several systems are available, ranging in volume from 100 mL to 2 gallons, with pressure ratings to 6000 psi, automated heatup and cooldown, constant hydrogen pressure regulation, and computer control and recording of runs.

Available Systems

• 2-gallon stirred autoclave system fully instrumented for temperature and pressure monitoring.
• Computer-controlled Parr autoclave system includes 250-mL, 500-mL, and 1-L reactors, with stirring capability and temperature and pressure monitoring.
• Several pressure vessels ranging in size from 100 mL to 4 L, that can be configured to accommodate a variety of batch or continuously stirred tank operations.