反应详情

温度

30 °C

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.

1. customThe reaction apparatus consisted of a heated enameled vessel of two cubic meters capacity
2. customequipped with three feed tubes, a stirrer, and a glass condenser
3. temperaturerefluxed
4. customamounted to 69° C
5. customrose toward the end of the reaction back to 64° C
6. additionwas added
7. custompresent had been removed in the form of hydrogen chloride
8. additionthe mixture was first diluted with 200 liters of hexane
9. customThe suspension obtained
10. customto separate the precipitated ammonium chloride
11. distillationFirst the hexane was distilled out of the filtrate
12. distillationthen, at a vacuum of less than 1 mbar and at a head temperature of about 155° C., the butyl titanate was purified by distillation