Water → Prop-2-enenitrile--ethenylbenzene (1/1)

Temperature

65 °C

168.7 Parts of demineralized water were added to a reactor. The reactor was sealed and purged with nitrogen. To a separate container were added 26.9 parts of demineralized water, 1.5 parts GAFAC RE-610 and 0.02 part citric acid monohydrate, and the components were mixed until dispersed. To a third container were added 21.6 parts styrene and 67 parts acrylonitrile and the components were mixed for 10 minutes. The aqueous solution of GAFAC RE-610 and citric acid were then added to the reactor by vacuum and the contents of the reactor heated with agitation. 15.2 Parts of elastomer were then added by vacuum followed by 20.3 parts demineralized rinse water. While heating, the reactor was purged with nitrogen. A mixture of monomer precharge consisting of 0.4 part styrene and 8.43 parts of acrylonitrile were added to the reactor by vacuum, and this was followed by the addition of 20.3 parts of demineralized water. The nitrogen purge was again repeated, and the final pressure in the reactor was maintained at a vacuum of 10 inches of Hg. After the temperature of the reactor was stabilized at 60°C, 0.1 part of Vazo 52 dissolved in 1.0 part acrylonitrile was added to the reactor with vacuum, followed by 0.33 part acrylonitrile as a rinse. 0.75 Part of water was then used to rinse the acrylonitrile into the reactor, and reaction time was measured subsequent to this point. After fifteen minutes of reaction time, the balance of the monomer mixture and the t-butyl mercaptan were pumped into the reactor through separate lines over a period of 360 minutes. At 165 minutes of reaction time, 0.3 parts of Vazo 52 dissolved in 0.33 parts of acrylonitrile were added to the reaction mixture by means of a vacuum, and this was followed by 0.33 parts of acrylonitrile and 0.75 parts of water. At 285 minutes of reaction time, the above addition of Vazo 52 and acrylonitrile was repeated, and the temperature was then raised to 65°C after 315 minutes. After all the monomers and the mercaptan had been added, the lines were purged with 0.75 part demineralized water and the temperature was maintained at 65°C for an additional 30 minutes.

1. customThe reactor was sealed
2. custompurged with nitrogen
3. additionTo a separate container were added 26.9 parts of demineralized water, 1.5 parts GAFAC RE-610 and 0.02 part citric acid monohydrate
4. additionthe components were mixed
5. additionuntil dispersed
6. additionTo a third container were added 21.6 parts styrene and 67 parts acrylonitrile
7. additionthe components were mixed for 10 minutes
8. additionThe aqueous solution of GAFAC RE-610 and citric acid were then added to the reactor by vacuum
9. temperaturethe contents of the reactor heated with agitation
10. addition15.2 Parts of elastomer were then added by vacuum
11. washdemineralized rinse water
12. temperatureWhile heating
13. customthe reactor was purged with nitrogen
14. additionA mixture of monomer precharge
15. additionwere added to the reactor by vacuum
16. additionthis was followed by the addition of 20.3 parts of demineralized water
17. customThe nitrogen purge
18. temperaturethe final pressure in the reactor was maintained at a vacuum of 10 inches of Hg
19. customwas stabilized at 60°C
20. dissolution0.1 part of Vazo 52 dissolved in 1.0 part acrylonitrile
21. additionwas added to the reactor with vacuum
22. washto rinse the acrylonitrile
23. custominto the reactor, and reaction time
24. customAfter fifteen minutes of reaction time
25. customthrough separate lines over a period of 360 minutes
26. customAt 165 minutes of reaction time, 0.3 parts of Vazo 52
27. additionwere added to the reaction mixture by means of a vacuum
28. customAt 285 minutes of reaction time
29. customthe lines were purged with 0.75 part
30. temperaturethe temperature was maintained at 65°C for an additional 30 minutes

ORD record

ord-7f2abe344b53409eae2a74dafa9886f8

Source dataset

uspto-grants-1976_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US03954913