Reaktion #171124

Reaktionsgleichung

acrylic acid

α-methylene-γ-valerolactone

water

sodium dodecyl sulfate

sodium hydroxide

sodium persulfate

water

sodium dodecyl sulfate

→

α-methylene-γ-valerolactone acrylic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo a 50 mL round bottom flask equipped with a magnetic stir bar
2. 2
   workup.ADDITIONwas added via syringe pump over 115 minutes
3. 3
   workup.ADDITIONAfter 10 minutes of monomer mixture addition
4. 4
   workup.ADDITIONwas also added via syringe pump over 120 minutes
5. 5
   workup.ADDITIONAfter both the monomer and aqueous mixtures were added completely
6. 6
   Temperaturafter which the reaction was cooled to room temperature
7. 7
   Sonstigedried under vacuum at 100° C
8. 8
   Sonstigeat 210° C
9. 9
   SonstigeSize exclusion chromatography yielded a molecular weight of 931 kDa

Vorschrift

To a 50 mL round bottom flask equipped with a magnetic stir bar was added 7.3769 g (0.343 mol) water and 0.084 g (2.70×10−4 mol) sodium dodecyl sulfate. (20% aqueous solution). The mixture was heated under flowing nitrogen to 73° C., at which point a monomer mixture consisting of 3.4691 g (2.58×10−2 mol) α-methylene-γ-valerolactone and 0.184 g (2.56×10−3 mol) acrylic acid was added via syringe pump over 115 minutes. After 10 minutes of monomer mixture addition, an aqueous mixture consisting of 13.9194 g (0.649 mol) water, 0.2360 g (6.87×10−4 mol) sodium dodecyl sulfate (20% aqueous solution), 0.0201 g (1.68×10−5 mol) sodium persulfate, and 0.0376 g of a 20% aqueous sodium hydroxide solution was also added via syringe pump over 120 minutes. After both the monomer and aqueous mixtures were added completely, the emulsion was allowed to stir for an additional 60 minutes, after which the reaction was cooled to room temperature and dried under vacuum at 100° C. Analysis of the polymer by DSC showed a single Tg at 210° C. Size exclusion chromatography yielded a molecular weight of 931 kDa and a PDI of 2.00.

Quelle