Hydrogen peroxide-calcium chloride

FERRIC OXIDE (1309-37-1) FcjO, Violent reactions with powdered aluminum (thermite reaction), hydrogen peroxide, calcium disilicide (thermite reaction), ethylene oxide (may cause explosive polymerization), calcium hypochlorite, hydrazine, hydrogen trisulfide, powdered magnesium. Contact with carbon monoxide may cause fire or explosion. Incompatible with calcium carbide (powdered), chlorides, guanidinium perchlorate, metal acetylides. Contact with the explosive hydrazinium diperchlorate or ammonium perchlorate can increase heat-, mechanical shock-, or friction sensitivity. Incompatible with aluminum-magnesium-zinc alloys. Spent material... 

Organoperoxysulfonic acids and their salts have been prepared by the reaction of arenesulfonyl chlorides with calcium, silver, or sodium peroxide treatment of metal salts of organosulfonic acids with hydrogen peroxide hydrolysis of di(organosulfonyl) peroxides, RS(0)2—OO—S(02)R, with hydrogen peroxide and sulfoxidation of saturated, non aromatic hydrocarbons, eg, cyclohexane (44,181). 

A 300-ml. three-necked flask equipped with a Trubore stirrer, dropping funnel, and reflux condenser protected with a calcium chloride drying tube is charged with 100 ml. of methylene chloride (Note 1). To this solvent is added without stirring 5.4 ml. (0.20 mole) of 90% hydrogen peroxide (Notes 2, 3, 4, 5). The hydrogen peroxide is not miscible with the solvent and separates as the lower layer at the bottom of the flask. The flask is then cooled in an ice bath, and the stirrer is started. To this cold solution over a 20-minute period is added 34.0 ml. (0.24 mole) of trifluoroacetic anhydride. After addition is complete, the ice bath is removed and the solution is stirred at room temperature for 30 minutes. 

In an excess of concentrated (30 per cent) hydrogen peroxide to which a little sulfuric acid has been added to insure acidity, dissolve the potassium metavanadate, observing that the color changes to an intense yellow. To this solution, well cooled, add 95 per cent alcohol until the pervanadate has been precipitated as a microcrystalline powder. Filter off the product, wash with alcohol, and dry in a desiccator over calcium chloride. 

Oxalic Acid. — The solution of 2 cc. of hydrogen peroxide in 10 cc. of water should not become turbid on the addition of calcium chloride solution. 

To prepare the 8-hydrate, llg of calcium chloride 6-hydrate are dissolved in 5ml of water and treated with 50ml of fresh 3% hydrogen peroxide and then with 7ml of concentrated ammonia solution in 100ml of water. If this procedure is carried out at 55°C, or if only 30ml of water are used for the ammonia at 20°C, the four-tenths hydrate is obtained. Palmer may be consulted for more details. 

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