反应详情

温度

65 °C

The polymerization of N-vinyl-2-pyrrolidone (VP), dimethylaminopropyl methacrylamide (DMAPMA), and m-TMI-ME carbamate-thiocarbamate (produced in Example 1) in 82:17:1 molar ratio involved the following steps: A 0.5-L, four-neck reaction kettle was equipped with a nitrogen purge, a condenser, a mechanical stirrer, and an oil bath. A monomer solution was prepared by dissolving 5.0 g of m-TMI-ME carbamate-thiocarbamate (from Example 1) in 76.0 g of N-vinyl-2-pyrrolidone and 19.0 g of DMAPMA. Then, 160.0 g of 2-propanol (IPA) was added to the reaction vessel, stirring was started, the vessel was purged with nitrogen and heated to 65° C. over the course of 1 hour. At t=0, 0.2 g of the initiator tert-butylperoxypivalate (Trigonox® 25-C75, Akzo Nobel) dissolved in 10.0 g of IPA were charged into the reaction kettle. Simultaneously, the monomer solution was fed to the kettle, and was completed in the course of 1 hour. At t=1 hour, 0.2 g of the initiator was dissolved in 10.0 g of IPA and added to the reaction kettle, which was held for 1 hour. At t=2 hours, 0.2 g of the initiator was dissolved in 10.0 g of IPA and added to the reaction kettle, which was held for 2 hours. At t=4 hours, 0.4 g of the initiator was dissolved in 10.0 g of IPA and added to the reaction kettle, which was held for 2 hours. Then, starting at t=6 hours, 0.1 g of the intiator dissolved in 1.0 g of IPA was added to the reactor and held for 1 hour. This step was repeated 6 times. Afterward, at t=12 hours, the solvent was exchanged with 200.0 g of deionized water, completed over 1 hour. Simultaneously, three redox system initiator solutions were prepared. Solution A contained 0.01 g of ferrous ammonium sulfate dissolved in 99.99 g of deionized water. Solution B contained 2.52 g of sodium metabisulfite dissolved in 36 g of deionized water. Solution C contained 3.78 g of tert-butyl hydroperoxide 70 (Brand name, manufacturer) dissolved in 18.0 g of deionized water. From t=13 to 24 hours, a charge of 12.0 g of Solution A was added over 10 seconds and then reaction conditions held for 10 minutes. Then, 6.42 g of Solution B were added over 10 seconds, and held for 10 minutes. Finally, 3.63 g of Solution C were added over 10 seconds. At t=24 hours the reaction was stopped and the contents of the kettle were discharged.

1. customwas equipped with a nitrogen
2. custompurge
3. customA monomer solution was prepared
4. customthe vessel was purged with nitrogen
5. dissolutionAt t=0, 0.2 g of the initiator tert-butylperoxypivalate (Trigonox® 25-C75, Akzo Nobel) dissolved in 10.0 g of IPA
6. additionwere charged into the reaction kettle
7. customwas completed in the course of 1 hour
8. dissolutionAt t=1 hour, 0.2 g of the initiator was dissolved in 10.0 g of IPA
9. additionadded to the reaction kettle, which
10. dissolutionAt t=2 hours, 0.2 g of the initiator was dissolved in 10.0 g of IPA
11. additionadded to the reaction kettle, which
12. waitwas held for 2 hours
13. dissolutionAt t=4 hours, 0.4 g of the initiator was dissolved in 10.0 g of IPA
14. additionadded to the reaction kettle, which
15. waitwas held for 2 hours
16. customstarting at t=6 hours, 0.1 g of the intiator
17. dissolutiondissolved in 1.0 g of IPA
18. additionwas added to the reactor
19. waitheld for 1 hour
20. customat t=12 hours
21. waitcompleted over 1 hour
22. customSimultaneously, three redox system initiator solutions were prepared
23. additionwas added over 10 seconds
24. customreaction conditions
25. waitheld for 10 minutes
26. waitheld for 10 minutes
27. customAt t=24 hours