Page 270 - Principles of Catalyst Development

LABORATORY RECIPES 261
Continue the drying until the gel pieces are translucent. Calcine 10-15 hr
at 550°C.

2.2. Nickel Oxide Alumina (Hydrogenation and Methanation)

Dissolve 454 g of AI( N0 3 h9H 20 in 3000 em' of H 20 and cool to
5-1O°C. Dissolve 200 g of NaOH in 1000 cm of H 20 and cool to 5-IO°C.
3
Add the soldium hydroxide solution to the aluminum nitrate solution
dropwise while stirring vigorously over a period of 1-2 hr. Dissolve 100 g
of Ni(NO)h6H 20 in 600 em) of H 20, add 45 cm of concentrated HNO
3
and cool to 5-10 0c. Add the nickel nitrate solutions to the sodium aluminate
solution with vigorous stirring over a period of 0.5-1 hr. Filter the light
green precipitate in a Buchner funnel and suspend the filtrate in 2000 cm 3
of H 20 for 15 min while stirring. Repeat the washing procedure six times.
Cut the filtrate into cubes, place in an evaporating dish, and dry in an air
oven for 16 hr at 105°C. Crush the catalyst to 8-12 mesh.
Before use, the required amount of catalyst is reduced in a stream of
hydrogen (30-80 cm min ') for 16 hr at 350°C. The furnace temperature is
3
raised to the reduction temperature over a period of 3 hr.

3. DISPERSED OXIDES

3.1. Chromia Alumina (Dehydrogenation)

Place 175 g of activated alumina of the desired mesh size in a 500-cm 3
filter flask. Attach a dropping funnel through a one-hole stopper. At some
point between the stopcock of the funnel and the rubber stopper, make a
flexible tubing connection that may be clamped shut. Attach the side arm
of the flask to a vacuum pump. Dissolve 31.6 g of Cr0 2 in sufficient water
to make 65 cm of solution and place the solution in the dropping funnel.
3
Evacuate the flask and admit the chromium solution while shaking the
catalyst to ensure uniform absorption of the liquid. When all the solution
has been added and the catalyst is uniformly impregnated, remove the
catalyst from the flask, dry at 1500C, and calcine in hydrogen at 550°C.

3.2. Fischer-Tropsch (Hydrocarbon Synthesis)

Dissolve 246 g of Co( N0 3h 6H 2 and 6.3 g of Th(NO))44H20 in
1300 em] of H2 0. Heat to boiling and add 100 g of kieselguhr and 6 g of
MgO in 500 cm] of H2 0, maintaining the boiling. Dissolve 92 g of sodium
carbonate in 500 em' of H:,O and heat to boiling. Add the boiling slurry of