Reaktion #171118

ord-40aa735a4fc642b2855ba315df9fa102

Reaktionsgleichung

CCCCCCCCCCCCOS(=O)(=O)[O-].[Na+]
sodium dodecyl sulfate
[Na+].[OH-]
sodium hydroxide
C=C1CCOC1=O
α-methylene-γ-butyrolactone
C=CC(=O)O
acrylic acid
C=CCOCC(CO)(CO)CO
pentaerythritol allyl ether
O=S(=O)([O-])OOS(=O)(=O)[O-].[Na+].[Na+]
sodium persulfate
C=C1CCOC1=O
α-methylene-γ-butyrolactone
C=CC(=O)O
acrylic acid
C=CCOCC(CO)(CO)CO
pentaerythritol allyl ether
CCCCCCCCCCCCOS(=O)(=O)[O-].[Na+]
sodium dodecylsulfate
→
C=C1CCOC1=O.C=CC(=O)O.C=CCOCC(CO)(CO)CO
α-methylene-γ-butyrolactone acrylic acid pentaerythritol allyl ether

Edukte

—
solution
CCCCCCCCCCCCOS(=O)(=O)[O-].[Na+]
sodium dodecyl sulfate
[Na+].[OH-]
sodium hydroxide
C=C1CCOC1=O
α-methylene-γ-butyrolactone
C=CC(=O)O
acrylic acid
C=CCOCC(CO)(CO)CO
pentaerythritol allyl ether
O=S(=O)([O-])OOS(=O)(=O)[O-].[Na+].[Na+]
sodium persulfate
C=C1CCOC1=O
α-methylene-γ-butyrolactone
C=CC(=O)O
acrylic acid
C=CCOCC(CO)(CO)CO
pentaerythritol allyl ether
CCCCCCCCCCCCOS(=O)(=O)[O-].[Na+]
sodium dodecylsulfate

Reagenzien

Keine

Lösungsmittel

O
water
O
water

Reaktionsbedingungen

Temperatur
75°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeTo a four neck round bottom glass flask, equipped with a mechanical stirrer
  2. 2
    workup.ADDITIONa thermocouple with a nitrogen inlet at the side of the inlet-tube and two dropping funnels was added the
  3. 3
    workup.ADDITIONwere added
  4. 4
    workup.ADDITIONwere added
  5. 5
    workup.ADDITIONThe initial charge
  6. 6
    workup.ADDITIONdropwise addition of the monomer
  7. 7
    workup.ADDITIONDropwise addition of the aqueous mixture
  8. 8
    workup.WAITThe monomer feed ended 120 minutes
  9. 9
    workup.ADDITIONafter the start of monomer addition
  10. 10
    workup.WAITthe aqueous stream ended 5 minutes
  11. 11
    TemperaturAfter a cook-down time of one hour, the reaction mixture was cooled to room temperature

Vorschrift

The crosslinked polymer poly(α-methylene-γ-butyrolactone-acrylic acid-pentaerythritol allyl ether) was prepared by emulsion polymerization of α-methylene-γ-butyrolactone and acrylic acid with the crosslinking monomer pentaerythritol allyl ether. To a four neck round bottom glass flask, equipped with a mechanical stirrer and a thermocouple with a nitrogen inlet at the side of the inlet-tube and two dropping funnels was added the initial charge of 44.03 g of water and 0.51 g of a 20% solution of sodium dodecyl sulfate surfactant. Into the monomer dropping funnel a mixture of 20.8 g of α-methylene-γ-butyrolactone, 1.1 g of acrylic acid and 0.16 g of pentaerythritol allyl ether were added. Into the second dropping funnel the aqueous mixture consisting of 83.43 g water, 1.32 g 20% sodium dodecylsulfate, 0.14 g sodium persulfate and 0.17 g 20% sodium hydroxide solution were added. The initial charge was heated to 75° C. dropwise addition of the monomer was started. Dropwise addition of the aqueous mixture started 5 minutes later. The monomer feed ended 120 minutes after the start of monomer addition, and the aqueous stream ended 5 minutes after the monomer stream ended. After a cook-down time of one hour, the reaction mixture was cooled to room temperature.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08846817B2uspto-grants-2014_09