Preparation Of Catalyst

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Preparation of Catalyst.-Metallic nickel was used almost exclusively. Pure nickel nitrate is calcined at a dull red heat for an hour, cooled, and very finely ground. It may be heated again to a red heat to insure complete decomposition of the nitrate. The powdered nickel oxide is then reduced in a stream of hydrogen at 250' for several hours. It is allowed to cool overnight in an atmosphere of hydrogen and is placed in a tightly stoppered flask until used, This catalyst used in the proportion of one part catalyst to 10 of substance remains in an active state for 5 or 6 reductions. If the reduction is proceeding too slowly it is best to replace the old by fresh unused nickel.

Baeyerl prepared this substance by the oxidation of cyclohexanol with Beckman's chromic acid mixture and proved its identity with the ketohexamethylene obtained by Perkin, Jr., from calcium pimelate. Baeyer used a proportion of 2 g. of cyclohexanol to 27 g. of the chromic acid mixture. The method used by us is essentiaily the same, modified slightly to keep the volumes down when dealing with roo-g. portions.
One hundred g. of cyclohexanol and 150cc. of water are placed in a one-liter flask and cooled in ice water. To this is added gradually 35 ce. of conc. sulfuric acid. One hundred g. of sodium dichromate (Na&rzOi- z&O) is dissolved in a solution of 35 cc. of conc. sulfuric acid in 150 ec. of mater. The chromic acid solution is added to th cyclohexanol mixture in IO cc. portions over a period of 2 hours, and the solution is shaken well after each addition. To complete the reaction the mixture is heated in a water-bath for z hours, cooled, and ether extracted, the extract dried with potassium carbonate and the ether distilled off. The cyclohexanone boils constantly ai. 155". Yield, 83 g. or 85%.

Hazards: concentrated sulfuric acid: hazardous in case of skin/eye contact, ingestion & inhalation; may produce burns with skin contact; non-flammable; may be combustible at high temps; reacts violently with

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