1-Butanol → Titanium tetrabutoxide

Participants

Reaction Conditions

Reaction Steps

The reaction apparatus consisted of a heated enameled vessel of two cubic meters capacity, equipped with three feed tubes, a stirrer, and a glass condenser operated with water and connected to a 4 square meter Hastelloy C brine cooler (-45° C.). 670 liters of hexane were placed in it and refluxed. The temperature below the water condenser amounted to 69° C. Over a period of 2 hours 380 kg of titanium chloride (2 kmol) and 444 kg of n-butanol (6 kmol) were put in at such a rate that the molar ratio of titanium chloride to n-butanol amounted always to about 1:3. Immediately at the start of the addition a vigorous evolution of hydrogen chloride began. The temperature below the water condenser dropped to 60° C. and rose toward the end of the reaction back to 64° C. After the reaction another 155.4 kg of n-butanol (2.1 kmol) was added with stirring. A sample had a chlorine content of 11.6%. This meant that 47.5% of the chlorine present had been removed in the form of hydrogen chloride. After cooling to about 30° C., the mixture was first diluted with 200 liters of hexane, and then ammonia was fed through the third feed tube for a period of 2 hours. The suspension obtained was centrifuged to separate the precipitated ammonium chloride. First the hexane was distilled out of the filtrate; then, at a vacuum of less than 1 mbar and at a head temperature of about 155° C., the butyl titanate was purified by distillation. 619 kg of butyl titanate was obtained.

Provenance & Evidence