Reacción #163425

ord-8e81e160058e42609982d2effd7110fc

Disolventes

Condiciones de reacción

Temperatura
-70°CELSIUS
Condiciones detalladas
See reaction.notes.procedure_details.

Tratamiento posterior

  1. 1
    OtroIn a 2 L reaction vessel
  2. 2
    Otroequipped with a stirrer
  3. 3
    Otrothe solution was reacted for 2.0 hours
  4. 4
    Otrothe reaction was terminated
  5. 5
    workup.ADDITIONby adding a large amount of methanol
  6. 6
    OtroAfter removing the solvent from the reaction solution
  7. 7
    workup.DISSOLUTIONa polymer was dissolved in toluene
  8. 8
    Lavadowashed twice with water
  9. 9
    workup.ADDITIONThis toluene solution was added to the methanol mixture
  10. 10
    Otroprecipitating a polymer
  11. 11
    Secadothe resultant polymer was dried at 60° C. for 24 hours

Procedimiento

In a 2 L reaction vessel equipped with a stirrer, 589 mL of methylcyclohexane (dried over molecular sieves), 613 mL of n-butyl chloride (dried over molecular sieves) and 0.550 g of cumyl chloride were added. After cooling the reaction vessel to −70° C., 0.35 mL of α-picoline(2-methylpyridine) and 179 mL of isobutylene were added. Furthermore, 9.4 mL of titanium tetrachloride was added and the polymerization was initiated, and then the solution was reacted for 2.0 hours while stirring at −70° C. Next, 59 mL of styrene was added to the reaction vessel and the reaction was continued for 60 minutes, and then the reaction was terminated by adding a large amount of methanol. After removing the solvent from the reaction solution, a polymer was dissolved in toluene and washed twice with water. This toluene solution was added to the methanol mixture, thereby precipitating a polymer, and the resultant polymer was dried at 60° C. for 24 hours to obtain a styrene-isobutylene diblock copolymer.

Fuente

DOI: 10.6084/m9.figshare.5104873.v1Patente: US08835557B2uspto-grants-2014_09