반응 #2275724
ord-3e5897952e8846fcb6c5303b2704b3fa
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후처리
- 1기타To a reaction vessel equipped with a stirrer
- 2온도the content was heated to 75 C
- 3기타over 3.5 hours
- 4workup.ADDITIONAfter the dropwise addition
- 5workup.STIRRINGthe reaction mixture was stirred at 75 C for 5 hours
- 6workup.DISTILLATIONwas distilled off until isopropyl alcohol could not
실험 절차
To a reaction vessel equipped with a stirrer and temperature controller were added 300 parts of isopropyl alcohol and 100 parts of ultrapure water. After replacing the atmosphere with nitrogen, the content was heated to 75 C. Under stirring, to the reaction vessel were simultaneously added dropwise 436 parts of a 70% aqueous monomer solution, comprising 227 parts of acrylamide-2-methylpropanesulfonic acid, 78 parts of acrylic acid, and 131 parts of ultrapure water, and 95 parts of a 15% isopropyl alcohol solution of dimethyl-2,2′-azobisisobutyrate over 3.5 hours. After the dropwise addition was complete, the reaction mixture was stirred at 75 C for 5 hours. Thereafter, while adding ultrapure water intermittently so that the content would not solidify, a mixture of water and isopropyl alcohol was distilled off until isopropyl alcohol could not be detected. To the aqueous solution of acrylamide-2-methylpropanesulfonic acid/acrylic acid copolymer obtained, DBU was gradually added while controlling the temperature at 25 C to adjust the pH to 6.5 (ca. 280 parts of DBU was used). By adjusting the concentration with ultrapure water, there was obtained a 40% aqueous solution of a DBU salt of acrylamide-2-methylpropanesulfonic acid/acrylic acid copolymer (B-3), a polymeric anionic surfactant. In addition, the Mw of (B-3) was 8,000