Reaction #75424

ord-c7fdaf5d8aa948d0843521d00fdf498b

Solvents

Conditions

Temperature
60°CELSIUS
Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    OtherInto a clean, dry
  2. 2
    Othernitrogen-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
    OtherThe flask was fitted with a stirrer
  5. 5
    Temperaturethermometer, reflux
  6. 6
    workup.ADDITIONcondenser and 1000 ml addition funnel
  7. 7
    OtherA solution was prepared
  8. 8
    Otherwas obtained
  9. 9
    workup.ADDITIONThis solution was then charged into the reaction flask
  10. 10
    Otherwas prepared
  11. 11
    workup.STIRRINGWith stirring
  12. 12
    Othercontrolled at 60° C.
  13. 13
    workup.ADDITIONmonomer addition
  14. 14
    Temperaturemaintained at 0.5%/min
  15. 15
    workup.ADDITIONAfter all the monomer had been added
  16. 16
    Otherpolymerization
  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

Procedure

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.

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04176144uspto-grants-1979_11