Reaktion #171127

Reaktionsgleichung

triallyl amine

α-methylene-γ-valerolactone

acrylic acid

water

sodium dodecyl sulfate

sodium hydroxide

sodium persulfate

water

sodium dodecyl sulfate

→

α-methylene-γ-valerolactone triallyl amine acrylic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo a 150 mL round bottom flask equipped with a magnetic stir bar
2. 2
   workup.ADDITIONis added dropwise over 120 minutes
3. 3
   workup.ADDITIONAfter 5 minutes of monomer mixture addition
4. 4
   workup.ADDITIONis also added dropwise over 120 minutes
5. 5
   workup.ADDITIONAfter addition of both the monomer and aqueous mixtures
6. 6
   Temperaturafter which the reaction is cooled to room temperature
7. 7
   Sonstigethe polymer can be dried under vacuum for isolation

Vorschrift

To a 150 mL round bottom flask equipped with a magnetic stir bar is added 10.00 g (0.555 mol) water and 0.115 g (3.99×10−4 mol) sodium dodecyl sulfate (20% aqueous solution). The mixture is pre-heated under flowing nitrogen to 75° C., at which time a monomer mixture consisting of 4.725 g (4.18×10−2 mol) α-methylene-γ-valerolactone, 0.250 g (4.16×10−3 mol) acrylic acid, and 0.036 g (2.62×10−4 mol) triallyl amine is added dropwise over 120 minutes. After 5 minutes of monomer mixture addition, an aqueous mixture consisting of 18.937 g (1.05 mol) water, 0.300 g (1.04×10−3 mol) sodium dodecyl sulfate (20% aqueous solution), 0.033 g (1.39×10−4 mol) sodium persulfate, and 0.037 g of a 20% aqueous sodium hydroxide solution is also added dropwise over 120 minutes. After addition of both the monomer and aqueous mixtures are complete, the emulsion stirs for an additional 60 minutes, after which the reaction is cooled to room temperature and the polymer can be dried under vacuum for isolation.

Quelle