Reaktion #171130

Reaktionsgleichung

acrylic acid

α-methylene-γ-butyrolactone

styrene

water

water

sodium dodecyl sulfate

sodium hydroxide

sodium persulfate

sodium dodecyl sulfate

→

α-methylene-γ-butyrolactone styrene-acrylic acid

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeTo a 100 mL round bottom flask equipped with a magnetic stir bar
2. 2
   workup.ADDITIONwas added via syringe pump over 130 minutes
3. 3
   workup.ADDITIONAfter 10 minutes of monomer mixture addition
4. 4
   workup.ADDITIONwas added via syringe pump over 130 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 under vacuum at 90° C. overnight
8. 8
   SonstigeSize exclusion chromatography yielded a monomodal peak with a weight average molecular weight of 104 kDa
9. 9
   Sonstigeat approximately 167° C.

Vorschrift

To a 100 mL round bottom flask equipped with a magnetic stir bar was added 8.825 g (0.490 mol) water and 0.117 g (4.06×10−4 mol) sodium dodecyl sulfate (20% aqueous solution). The mixture was heated under flowing nitrogen to 73° C., at which time a monomer mixture consisting of 3.079 g (3.14×10−2 mol) α-methylene-γ-butyrolactone, 1.082 g styrene (1.04×10−2 mol) and 0.220 g (3.66×10−3 mol) acrylic acid was added via syringe pump over 130 minutes. After 10 minutes of monomer mixture addition, an aqueous mixture consisting of 16.694 g (0.927 mol) water, 0.269 g (9.33×10−4 mol) sodium dodecyl sulfate (20% aqueous solution), 0.033 g (1.39×10−4 mol) sodium persulfate, and 0.041 g of a 20% aqueous sodium hydroxide solution was added via syringe pump over 130 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 under vacuum at 90° C. overnight. Size exclusion chromatography yielded a monomodal peak with a weight average molecular weight of 104 kDa and a polydispersity of 1.96, relative to polystyrene standards. Differential scanning calorimetry showed a single first order transition at approximately 167° C.

Quelle