Reaktion #467420

ord-b69be9f814fd424f84270f41a341ff6a

Reaktionsbedingungen

Temperatur
70°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.ADDITIONTo the solution was dropwise added
  2. 2
    workup.STIRRINGby stirring for 2 hours
  3. 3
    Temperaturthe mixture was heated to temperature of 75° C.
  4. 4
    workup.STIRRINGby stirring for 3 hours
  5. 5
    Temperaturthe mixture was heated to temperature of 80° C.
  6. 6
    workup.STIRRINGby stirring for 3 hours
  7. 7
    TemperaturThe temperature of the reaction mixture was raised to 100° C.
  8. 8
    workup.STIRRINGby stirring under a reduced pressure of 200 mmHg for 2 hours
  9. 9
    workup.DISTILLATIONdistilling off the unreacted monomers
  10. 10
    TemperaturAfter cooling the reaction mixture, it

Vorschrift

A mixed solution of 10 g of Resin for Dispersion Stabilization (P-1) shown below and 280 g of Isopar G was heated to temperature of 70° C. with stirring under a nitrogen gas stream. To the solution was dropwise added a mixture of 30 g of methyl methacrylate, 61 g of methyl acrylate, 9 g of 2-(N,N-dimethylamino)ethyl methacrylate and 1.5 g of 2,2′-azobis(isovaleronitrile) (abbreviated as AIVN) over a period of one hour, followed by stirring for 2 hours. Then, 1.0 g of AIVN was added to the reaction mixture and the mixture was heated to temperature of 75° C., followed by stirring for 3 hours. Then, 0.8 g of 2,2′-azc)bis(isobutyronitrile) (abbreviated as AIBN) was added to the mixture and the mixture was heated to temperature of 80° C., followed by stirring for 3 hours. The temperature of the reaction mixture was raised to 100° C., followed by stirring under a reduced pressure of 200 mmHg for 2 hours, thereby distilling off the unreacted monomers. After cooling the reaction mixture, it was passed through a nylon cloth of 200 mesh. The resulting white dispersion was a latex having a polymerization rate of 99% and an average particle size of 0.35 μm. The particle size was measured by CAPA-500 manufactured by Horiba Ltd. (hereinafter the same).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06302537B1uspto-grants-2001_10