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The
Center for Applied Catalysis is well equipped to undertake catalyst evaluations
and optimization of catalytic reactions in either a batch process or a continuous
mode. Various pieces of equipment are available for use in reactions run
from atmospheric pressure to 1500 psig (100 bar). These reactors range in
size from 40 mL to 300 mL These small scale reactors provide an economy
of scale important when a large number of reactions are being run.
In order to properly evaluate a catalytic process the reactor system must
be able to measure and record all of the pertinent reaction data. To accomplish
this, all of the reactors in the Center have computerized monitoring and
data acquisition systems capable of measuring and recording reaction temperature
and pressure and the rate of gas uptake, where appropriate, over the course
of the reaction. With some reactors, the rate of agitation throughout the
reaction is also recorded. All of the batch reactors operate in a constant
volume - constant pressure mode.
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Figure
2
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Figure
1
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A common
method used to determine the rate of gas uptake while keeping the pressure
in the reactor constant is shown in Figure 1. The reaction gas is initially
charged into the reservoir (A) at a pressure significantly higher than
the pressure needed for the reaction. A gas regulator (R) is used to maintain
the pressure in the reactor while a pressure transducer (B) measures the
pressure drop in the reservoir. A second pressure transducer (C) is used
to monitor the pressure inside the reactor. The regulator (R') controls
the pressure in the reactor during the purging step before the actual
reaction.
Figure 2 shows a close-up of such an arrangement in one of the low pressure
reactor systems in the Center. Since the maximum pressure in the reservoir
is fixed by the pressure rating of the cylinder and other safety considerations,
the best way of using such a system for larger scale reactions is to change
the size of the reservoir. A facile method for changing the reservoir
size is shown in this Figure with different sized reservoirs connected
to a selection valve.
In addition, the Center is well equipped for the analysis of the reaction
products formed in our studies. We have GC-MS, several automated GC and
HPLC instruments with a number of chiral and achiral columns as well as
diffuse reflectance FTIR with which surface compositions can be measured
during a gas phase reaction. Also available are the various instruments
in the Department of Chemistry and Biochemistry which includes both 200
MHz and 500 MHz nmr's, a digital polarimeter and a Super CRC reaction
calorimeter.
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