Reaktion #311921

Reaktionsgleichung

γ-chloropropyltriethoxysilane

ammonia

ammonia

→

γ-chloropropyltriethoxysilane

γ-aminopropyltriethoxysilane

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigethe reactor was sealed
2. 2
   workup.STIRRINGthen stirring
3. 3
   workup.WAITwas continued for 8 hours at 75° C
4. 4
   Sonstigethe ammonia was removed
5. 5
   SonstigeAfter the removal of ammonium chloride
6. 6
   Filtrationby filtration
7. 7
   workup.DISTILLATIONthe remaining raw product was purified by vacuum distillation

Vorschrift

Into a ten-liter steel autoclave with stirrer, 3400 g (200 moles) of liquid ammonia was poured, and the reactor was sealed. Then the ammonia was heated to 75° C., causing a pressure of 36 bars to be established. After this temperature was reached, γ-chloropropyltriethoxysilane was fed in, with stirring at 183 rpm, for a period of one hour, in the amount of 2.67 moles; then stirring was continued for 8 hours at 75° C. Then the pressure was let off and the ammonia was removed. After the removal of ammonium chloride by filtration, the remaining raw product was purified by vacuum distillation. From the 642 grams of γ-chloropropyltriethoxysilane, 486 g of γ-aminopropyltriethoxysilane was obtained (82.4% of the theoretical yield) plus 98.3 g of byproducts (secondary and tertiary amines).

Quelle