Reaktion #792587

Reaktionsgleichung

phenol

TIPT

tetraisopropoxy titanium

→

Tetraphenoxy Titanium

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.DISTILLATIONTo the bottom of an Oldershaw type reaction-distillation column (
2. 2
   workup.DISTILLATIONhereinafter referred to as “reaction-distillation column for synthesizing a catalyst”)
3. 3
   Sonstigeequipped with a bottom flask
4. 4
   workup.ADDITIONwas charged 300 ml of phenol
5. 5
   Temperaturheated by an oil bath
6. 6
   TemperaturWhile maintaining the whole refluxing state
7. 7
   workup.DISTILLATIONafter stabilization of the temperature distribution in the reaction-distillation column
8. 8
   Sonstigefor synthesizing a catalyst, phenol
9. 9
   Temperaturwhile maintaining the reflux ratio of 5
10. 10
    workup.DISTILLATIONWith regard to the bottom, the liquid was continuously taken out from the bottom portion of the reaction-distillation column for synthesizing a catalyst so that the liquid surface
11. 11
    Temperaturmaintained 330 ml
12. 12
    TemperaturWith this state, it was maintained until the system
13. 13
    Sonstigewas 190° C.
14. 14
    Sonstigewas 164° C
15. 15
    SonstigeThe reaction conditions

Vorschrift

To the bottom of an Oldershaw type reaction-distillation column (hereinafter referred to as “reaction-distillation column for synthesizing a catalyst”) having an inner diameter of 32 mm and equipped with a bottom flask having a volume of 1L was charged 300 ml of phenol, and heated by an oil bath. While maintaining the whole refluxing state, and after stabilization of the temperature distribution in the reaction-distillation column for synthesizing a catalyst, phenol was fed with a flow amount of 342.4 g/h, and tetraisopropoxy titanium (TIPT) with 21.6 g/h. The ratio of the molar number of the phenol fed and the molar number of of the Ti atom in TIPT (phenol/Ti) was 48. The distilled liquid from the top was taken out while maintaining the reflux ratio of 5. With regard to the bottom, the liquid was continuously taken out from the bottom portion of the reaction-distillation column for synthesizing a catalyst so that the liquid surface maintained 330 ml. With this state, it was maintained until the system became a steady state, and when the bottom liquid was analyzed, 10.8% by weight of tetraphenoxy titanium (TPT), 89.2% by weight of phenol and 114 ppm of isopropanol (IPA) were detected. Also, the composition of the distillate was 71.8% by weight of phenol and 28.2% by weight of isopropanol. The taken out amounts at that time were the bottom liquid of 295.4 g/h and the top distillate of 68.6 g/h. Also, the bottom temperature was 190° C., and the top temperature was 164° C. As a result, the conversion of TIPT to TPT (TPT yield) was 99.8%. The reaction conditions and the results are shown in Table 1.

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