Oxalic Acid → HCID 178526027, compound

Participants

Reaction Conditions

Reaction Steps

Approximately 1,000 g of deionized water and oxalic acid dihydrate (381.9 g, 99% 3.0 moles), were charged to a 5-liter flask that was maintained under a nitrogen atmosphere. The resultant slurry was cooled to about 5 to 10 degrees C. and approximately 569.1 g (3.0 moles) of titanium tetrachloride were added dropwise over about 2 hours to the aqueous slurry containing oxalic acid. Deionized water, 1,082 g, was added rapidly over about 3 minutes to the slurry at temperatures from about 9 to 24 degrees C. The slurry was warmed to a temperature of about 30 degrees C. for about 10 minutes to provide a clear solution. Concentrated ammonium hydroxide solution was added dropwise over about 2 hours at a temperature from about 25 to 30 degrees C. to provide a white slurry with a pH of about 9.0. The slurry was stirred for about 30 minutes while the pH was maintained at about 9.0 by the addition of small amounts of ammonium hydroxide. The total amount of concentrated ammonium hydroxide (about 29.5% NH3) consumed was approximately 1,336 g (about 22.7 moles). The white slurry was filtered and the wet cake washed with six 645 ml displacement washes of 2% ammonium hydroxide solution. The wet cake, which weighed about 1,327.6 g, was dried in a vacuum oven at about 120 degrees C. to provide about 550.5 g of amino titanium oxalate. The dry amino titanium oxalate was shown by ignition at 750 degrees C. for 3 hours to remove the volatiles to have a titanium dioxide content of about 43.27%. This represents a 99% by wt. yield.

Provenance & Evidence