Reaktion #594904

Reaktionsgleichung

tris(2,4-Di-tert.butylphenyl)phosphite

isopropanol

→

Tris(2,4-di-tert.butylphenyl)phosphate

Lösungsmittel

Water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwhile maintaining
2. 2
   Sonstigethe pot temperature (reaction is exothermic)
3. 3
   Temperaturthe mixture is maintained for 1 hour at 60° C
4. 4
   Sonstigethe completeness of reaction
5. 5
   Sonstigecrystallization
6. 6
   TemperaturCooling slowly in 2 steps to 45° C.
7. 7
   Sonstigeto 20° C.
8. 8
   Sonstigecrystallization
9. 9
   FiltrationThe product is filtered (25μ screen)
10. 10
    Sonstigedried at 70° C. under full vacuum with a nitrogen sweep

Vorschrift

tris(2,4-Di-tert.butylphenyl)phosphite (5146 g; Irgafos® 168, Ciba Specialty Chemicals) and isopropanol (IPA, 7890 g) are mixed in a reaction vessel and heated to 55-60° C. At this point the mixture is a slurry of approximately 39.0% solids. The peroxide (549 g, 50 weight-% solution of H2O2 in water, 1 equivalent) is added for 2-3 hours while maintaining the pot temperature (reaction is exothermic). After the peroxide addition, the mixture is maintained for 1 hour at 60° C. The reaction mass is homogeneous and the completeness of reaction is checked by LC (>97.0% conversion). Water (1355 g) is added, and the reaction mass is seeded to induce crystallization. Cooling slowly in 2 steps to 45° C. and then to 20° C. completes crystallization. The product is filtered (25μ screen), then dried at 70° C. under full vacuum with a nitrogen sweep.

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