반응 #75424

ord-c7fdaf5d8aa948d0843521d00fdf498b

용매

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Into a clean, dry
  2. 2
    기타nitrogen-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
    기타The flask was fitted with a stirrer
  5. 5
    온도thermometer, reflux
  6. 6
    workup.ADDITIONcondenser and 1000 ml addition funnel
  7. 7
    기타A solution was prepared
  8. 8
    기타was obtained
  9. 9
    workup.ADDITIONThis solution was then charged into the reaction flask
  10. 10
    기타was prepared
  11. 11
    workup.STIRRINGWith stirring
  12. 12
    기타controlled at 60° C.
  13. 13
    workup.ADDITIONmonomer addition
  14. 14
    온도maintained at 0.5%/min
  15. 15
    workup.ADDITIONAfter all the monomer had been added
  16. 16
    기타polymerization
  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

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04176144uspto-grants-1979_11