Реакция #657250

ord-e0aa23279017416eaf788c7de7c92fde

Уравнение реакции

C=Cc1ccccc1
styrene
C=CC(=O)OCCCC
butyl acrylate
CCCCCCCCCCCCS
1-dodecanethiol
C=CC(=O)OCCCC.C=Cc1ccccc1
Styrene n-Butyl Acrylate

Реагенты

Нет

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеSeparately the monomer emulsion was prepared in the following manner
  2. 2
    Другоеto form an emulsion
  3. 3
    workup.ADDITIONcontaining the aqueous surfactant phase at 80° C.
  4. 4
    Другоеto form the “seeds”
  5. 5
    Другоеwhile being purged with nitrogen
  6. 6
    workup.ADDITIONThe initiator solution was then slowly charged into the reactor and after 10 minutes the rest of the emulsion
  7. 7
    workup.ADDITIONhalf of the monomer emulsion had been added to the reactor
  8. 8
    ТемператураAlso at this time the reactor stirrer was increased to 350 RPM
  9. 9
    workup.ADDITIONOnce all the monomer emulsion was charged into the main reactor
  10. 10
    workup.WAITthe temperature was held at 80° C. for an additional 2 hours
  11. 11
    Другоеthe reaction
  12. 12
    ТемператураFull cooling
  13. 13
    Другоеwas reduced to 35° C
  14. 14
    ДругоеThe product was collected into a holding tank
  15. 15
    ДругоеAfter drying the latex the molecular properties

Методика

Separately the monomer emulsion was prepared in the following manner. 323 kg of styrene, 83 kg of butyl acrylate and 12.21 kg of β-CEA, 2.85 kg of 1-dodecanethiol, 1.42 kg of ADOD, 8.04 kg of Dowfax 2A1 (anionic surfactant), and 193 kg of deionized water were mixed to form an emulsion. 1% of the above emulsion was then slowly fed into the reactor containing the aqueous surfactant phase at 80° C. to form the “seeds” while being purged with nitrogen. The initiator solution was then slowly charged into the reactor and after 10 minutes the rest of the emulsion was continuously fed using a metering pump at a rate of 0.5%/min. After 100 minutes, half of the monomer emulsion had been added to the reactor. At this time, 3.42 kilograms of 1-dodecanethiol was stirred into the monomer emulsion, and the emulsion was continuously fed in at a rate of 0.5%/min. Also at this time the reactor stirrer was increased to 350 RPM. Once all the monomer emulsion was charged into the main reactor, the temperature was held at 80° C. for an additional 2 hours to complete the reaction. Full cooling was then applied and the reactor temperature was reduced to 35° C. The product was collected into a holding tank. The particle size was calculated to be 180 nanometers. After drying the latex the molecular properties were Mw=37,500 Mn=10,900 g/mol and the onset Tg was 55.0° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09022546B1uspto-grants-2015_05