Reaktion #319164

Reaktionsgleichung

acryloyl chloride

diethylenetriamine

→

4-N-acryloyl-diethylenetriamine

Lösungsmittel

hexane

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONby slowly adding, at 23° C.
2. 2
   workup.DISTILLATIONhad been purified by vacuum distillation
3. 3
   workup.ADDITIONThe reaction product was oligomerized by the addition of 200 ml of a 4.1 wt% solution of isophthaloyl chloride in dichloromethane at 20° C. with mechanical stirring
4. 4
   SonstigeThe composite membrane was then air-dried at room temperature for 30 minutes

Vorschrift

4-N-acryloyl-diethylenetriamine was prepared by slowly adding, at 23° C., 200 ml of a solution of acryloyl chloride in a mixture of hexane and dichloromethane (C6H14 :C2Cl2 =3:1) at a concentration of 3.6 wt% (0.4 mEq/ml) to 600 ml of 1.4 wt% (0.4 mEq/ml) diethylenetriamine which had been purified by vacuum distillation. The reaction product was oligomerized by the addition of 200 ml of a 4.1 wt% solution of isophthaloyl chloride in dichloromethane at 20° C. with mechanical stirring. An asymmetric microporous polysulfone support flat sheet membrane 4 mils thick was immersed in a 2 wt% aqueous solution of 4-N-acryloyl-diethylenetriamine oligomer, drained of excess solution, then immersed in a 0.5 wt% solution of trimesoyl chloride at 20° C. for 30 seconds. The composite membrane was then air-dried at room temperature for 30 minutes and subjected to heat treatment at 105° C. for 10 minutes.

Quelle