反応 #75424

ord-c7fdaf5d8aa948d0843521d00fdf498b

溶媒

反応条件

温度
60°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他Into a clean, dry
  2. 2
    その他nitrogen-purged
  3. 3
    workup.ADDITIONthree liter, four neck, round bottom flask was charged 272.7 g of polybutadiene latex (Polysar PL-662) (55% polybutadiene)
  4. 4
    その他The flask was fitted with a stirrer
  5. 5
    温度thermometer, reflux
  6. 6
    workup.ADDITIONcondenser and 1000 ml addition funnel
  7. 7
    その他A solution was prepared
  8. 8
    その他was obtained
  9. 9
    workup.ADDITIONThis solution was then charged into the reaction flask
  10. 10
    その他was prepared
  11. 11
    workup.STIRRINGWith stirring
  12. 12
    その他controlled at 60° C.
  13. 13
    workup.ADDITIONmonomer addition
  14. 14
    温度maintained at 0.5%/min
  15. 15
    workup.ADDITIONAfter all the monomer had been added
  16. 16
    その他polymerization
  17. 17
    workup.ALIQUOTThe latex was sampled
  18. 18
    workup.ADDITIONAntioxidant was added to the latex in the form of 42 g of an 18% emulsion
  19. 19
    workup.ADDITIONcontaining 2/1

実験手順

Into a clean, dry, nitrogen-purged, three liter, four neck, round bottom flask was charged 272.7 g of polybutadiene latex (Polysar PL-662) (55% polybutadiene). The flask was fitted with a stirrer, thermometer, reflux condenser and 1000 ml addition funnel. A solution was prepared by mixing 12.0 g sodium stearate, 0.9 g sodium bicarbonate, 1.5 g sodium hydroxide, 3.0 g potassium persulfate and 1322 g deionized water. The mixture was heated to 60° C. while stirring until a clear, homogeneous solution was obtained. This solution was then charged into the reaction flask to dilute the stirred polybutadiene latex. A solution containing 435.6 g of the mixture of Example 1, 164.4 g acrylonitrile and 2.7 g tert-dodecyl mercaptan was prepared and placed in the addition funnel. With stirring and the charge temperature controlled at 60° C., monomer addition was started and maintained at 0.5%/min. After all the monomer had been added, polymerization was allowed to proceed for one additional hour. The latex was sampled to determine conversion by measuring total solids content. Antioxidant was added to the latex in the form of 42 g of an 18% emulsion containing 2/1--TNPP/Irganox 1076.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04176144uspto-grants-1979_11