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Synthesis of a Catalyst Using Excess Wetness Impregnation

Morgan Walli
WRD 204 001, Dan Shumer, University of Kentucky, 6 September 2018

1. INTRODUCTION poured through. The pans can be gently

In the effort to establish electrical energy as tapped until the smaller particles have
a norm in transportation, eighteen wheelers filtered through the one-hundred-and-fifty
and planes present a challenge. More micron mesh into the solid pan. Ten to
difficult to switch over to electric power, twelve grams of the sized support must then
their sustainability timeline is behind that of be measured into the flask.
smaller vehicles. Today, biofuels research is 2.3 Precursor Preparation After the
working to ease the transition from support has been added, the proper amount
traditional fuels to clean energy by of each precursor must be calculated using
providing a greener interim method of dimensional analysis to obtain the desired
powering these vehicles. Catalysts are at the catalyst composition. The precursors are
heart of this research, making their chemical compounds containing the metals
preparation central to the process. that will form the catalyst and attach to the
Wet impregnation is a common method support. An example calculation is shown in
of catalyst preparation. As Narallah Deraz the figure below.
summarized, “in wet impregnation an excess
of solution is used. After a certain time the
solid is separated and the excess solvent is
removed by drying.”1 The Center for
Applied Energy Research in Lexington, KY
uses wet impregnation to prepare alumina
supported nickel catalysts for the synthesis
of biodiesel from hemp oil.2 Their method is
discussed here.

2.1 Equipment Preparation The wet
impregnation process begins with equipment
preparation. A flat-bottomed round-flask, a Figure 1. Example calculations for a 20%
ceramic drying pan, and a metal stir bar Ni - 5% Cu/Al2O3 Catalyst
must be obtained, in addition to a clean one-
hundred-and-fifty micron pan and a solid After calculations are complete, each
filter pan. substance must be measured out directly into
2.2 Support Preparation Next, the the flask. The precursors are added directly
powdered support, a high surface area to the flask for the sake of accuracy because,
molecule that serves as a bed for the if using a filter paper, some of the material
catalyst, must be selected and sized to one- may remain on the paper. The powdered
hundred-and-fifty microns. The filter pans contents of the flask must then be gently
used to do this must be set up in the fume swirled in order to mix them.
hood so that the powdered support can be
After all the dry substances have been
added, it is time to begin wet impregnation.
To do so, the flask must be placed on the
mixing plate with a metal stir bar and a
small amount of water (just a few milliliters)
must be added using a long Pasteur Pipette.
The mixer must be turned on relatively low
speed and allowed to mix, with additional
water being added as necessary.
Because this is wet impregnation, just
enough water to create a slurry – not more –
should be added. Once the slurry has
formed, the start time and the amount of
water added should be recorded and the Figure 3. Catalyst Precursors After Wet
flask must be left on the mixer at four- Impregnation
hundred-and-fifty rpm mixing speed for two
to three hours.
4.1 Rotovaping With impregnation
complete, the water must then be evaporated
from the catalyst. This will be accomplished
using the Rotovap. Dry ice must be obtained
and added to the isopropyl alcohol chamber.
The flask containing the catalyst must be
attached and lowered into the medium-hot
heating bath. The Rotovap and the
associated vacuum must then be turned on
and the rotation adjusted to one hundred
rpm. The flask must then be observed as the
water evaporates. The end result should
appear dry.

Figure 2. Catalyst Precursor Prior to Wet


Figure 4. The Rotovap

4.2 Vacuum Oven After initial drying,
the contents of the flask must be scraped REFERENCES
into a ceramic drying pan and placed in the 1. Deraz, N. The comparative
vacuum oven overnight to dry further. The jurisprudence of catalysts preparation
pan must be covered with a filter paper to methods: I. precipitation and impregnation
prevent possible cross contamination with methods. Industrial Environmental
other catalysts in the oven. Chemistry. 2018, 2, 19-212
5. CALCINATION comparative-jurisprudence-of-catalysts-
After at least 12 hours in the vacuum oven, preparation-methods-i-precipitation-and-
the catalyst must be removed and transferred impregnation-methods.pdf (Accessed Aug
to the baking oven. Here, it must be run 30, 2018).
under the following program: 1) five-minute 2. Santillan-Jimenez, E.; Loe, R.;
ramp up to 500ºC, 2) hold for 3 hours at Garrett, M.; Morgan, T.; Crocker, M. Effect
500ºC, 3) five-minute ramp down to 35ºC, of Cu promotion on cracking and
4) hold at 35ºC until cool. After the methanation during theNi-catalyzed
calcination has finished, the catalyst must be deoxygenation of waste lipids and hemp
stored in properly labeled scintillation vials. seed oil tofuel-like hydrocarbons. Catalysis
The prepared catalyst can then be used in Today. 2018, 302, 261-271.
reactions and analysis.

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