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Figure
1
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Figure
2
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Reactions needing
pressures between 100 and 1500 psig are run in one of the stainless steel
autoclaves shown in Figure 1. These reactors are run at constant pressure
using the standard reservoir system described above. Reaction temperatures
are maintained by external temperature controllers. A computer is interfaced
with all three of the autoclaves to monitor reactor and reservoir pressures
and the reaction temperature for each reactor. The stirring rates are also
monitored throughout the reaction. The progress of the reaction is shown
on the computer screen as the drop in reservoir pressure with time (Figure
2).
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Figure
3
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We also have
the capability with these high pressure reactors to introduce the substrate
after pre-treatment of the catalyst without opening the reactor using the
modification shown in Figure 3. Here the catalyst and some solvent are placed
in the reactor and the substrate, either as a liquid or in solution, is
placed in the pressure cylinder (A) through the septum port (B). After the
pre-treatment of the catalyst, the cylinder, A, is pressurized to a value
somewhat higher than the pressure in the reactor. The valves (C) connecting
the cylinder with the reactor are opened and the substrate is blown into
the reactor. These valves are then closed and the reaction initiated. The
pressure in the cylinder can be vented through the septum port.
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