Water → alpha-Methylene-gamma-Valerolactone Acrylic Acid

HRID 83942

Reaktionsgleichung

Reaktionsgleichung von HRID 83942
O.S([O-])(OCCCCCCCCCCCC)(=O)=O.[Na+].[CH2:20]=[C:21]1[CH2:26][CH:25]([CH3:27])[O:24][C:22]1=[O:23].[C:28]([OH:32])(=[O:31])[CH:29]=[CH2:30].S(OOS([O-])(=O)=O)([O-])(=O)=O.[Na+].[Na+].[OH-].[Na+]>>[CH2:20]=[C:21]1[CH2:26][CH:25]([CH3:27])[O:24][C:22]1=[O:23].[C:28]([OH:32])(=[O:31])[CH:29]=[CH2:30]

Komponenten

7

Edukt 6

HCID 962Water2×HCID 6581Acrylic AcidHCID 14798Sodium HydroxideHCID 62655Sodium PersulfateHCID 99939gamma-Methyl-alpha-methylene-gamma-butyrolactoneHCID 3423265Sodium Lauryl Sulfate2×

Produkt 1

HCID 86664974alpha-Methylene-gamma-Valerolactone Acrylic Acid

Reaktionsbedingungen

Temperatur
73 °C

Versuchsvorschrift

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.

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-814aae88dde047788853e27ef440edc9
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846817B2

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