Oxalic Acid → HCID 178526027, compound

Participants

Reaction Conditions

Reaction Steps

A titanium oxychloride solution (about 383.2 g, 12.5% by weight titanium 1.0 mole), was prepared and was added rapidly to the oxalic acid slurry with stirring at a temperature of from about 40 to about 60 degrees C. The resulting clear solution was cooled to about 25 degrees C. Concentrated ammonium hydroxide solution was added dropwise over a period of about 40 minutes at a temperature of from 25 to 30 degrees C. to provide a white slurry with a pH of about 9. The slurry was stirred for 30 minutes while the pH was maintained at about 9.0 by the addition of small increments of ammonium hydroxide. The total amount of concentrated ammonium hydroxide (29.5% NH3) consumed was about 410.9 g (7.12 moles). The white slurry was filtered and the filter cake washed with six 400 ml displacement washes of 2% ammonium hydroxide. The wet cake was dried at about 120 degrees C. in a vacuum oven to provide approximately 156.5 g of amino titanium oxalate.

Provenance & Evidence