Page 268 - Principles of Catalyst Development
P. 268

APPENDIX  6


           Laboratory Recipes







           1.  SINGLE  OXIDES


           1.1.  Alumina Gel (A Support and  Dehydration Catalyst)

           Dissolve 1000 g ofCP AICI 3  6H 20  in 10,000 cm of H 20. Prepare an aqueous
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           ammonia solution by adding 840 cm of concentrated ammonia hydroxide
                                             3
           (about 30%  NH 3 )  to 1450 cm of H 20. Add the ammoniacal solution to the
                                      3
           AICh solution until  the  pH  is  about 8.  Allow the precipitate to settle and
           filter with a  Buchner funnel.  Wash five  times by decantation with 5 cm of
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           concentrated ammonia in  5000 cm of H 20. Allow the precipitate to settle
                                           3
           and filter with a Buchner funnel. By the end of the fifth wash, the precipitate
           is  very  difficult  to  settle  since  it  has  started  to  peptize.  If a  water  wash
           containing  no  ammonia  is  used,  peptization  begins  even  during  the  first
           wash.
               Dry the washed filtrate in an oven for several hours at 100-150°C. Then
           calcine overnight at about 550°C  in a  muffle furnace.


           1.2.  Silica Gel (A Support)
               Prepare  two  solutions.  Solution  A  is  500 cm 3   of  water  glass
           (Si02/Na20 = 3.22) in  1000 cm of H2 0. Solution B is 245 cm of 4  N  HCI
                                        3
                                                                    3
           plus 300 em) of H2 0. Cool both solutions to about 5°C, then add solution
           A to  solution  B with  vigorous  mechanical  agitation.  Pour into  a  flat  tray.
               The resulting sol  has a  pH of about 6 and a gel time of 2 miri. The gel
           will  be stiff enough to cut into cubes within 30-60 min. Transfer the cubes
           to a  Buchner funnel  as soon as  possible. Treat immediately with  1 N  HCI
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