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Chemistry Letters
Volumn 36, Issue 9, 2007, Pages 1114-1115
Block copolymerization of methyl methacrylate from fluorine-contained polyimide macroinitiator by atom-transfer radical polymerization
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EID: 34948813998     PISSN: 03667022     EISSN: None     Source Type: Journal    
DOI: 10.1246/cl.2007.1114     Document Type: Article
Times cited : (16)
References (17)
  • 11
    • 34948893752 scopus 로고    scopus 로고
    • 4,4'-Diaminodiphenyl ether (1.13 g, 5.63 mmol) and 4-aminophenethyl alcohol (0.31 g, 2.25 mmol) were dissolved in 15 mL of N-methyl-2-pyrrolidinone (NMP, and then 6FDA (3.00g, 6.75 mmol) was added into the solution. After the reaction mixture was stirred under a nitrogen atmosphere at room temperature for 12 h, 3mL of p-xylene was added into the yellow viscous polyamic acid solution, and it was refluxed for thermal imidization at 180° C for 6 h. The resulting product was poured slowly into a large amount of methanol to precipitate the polyimide solid. It was then purified by repeating reprecipitation using NMP and methanol, and then was dried overnight at 80°C in a vacuum oven to obtain the linear fluorine-contained polyimide with two terminal OH groups PI-OH, 3.48 g, 83% yield based on the weight, The Mn and Mw/Mn of the polyimide were 6000g/mol and 1.60, respectively
    • n of the polyimide were 6000g/mol and 1.60, respectively.
  • 13
    • 34948879419 scopus 로고    scopus 로고
    • Distilled MMA (1.07g, 10.7mmol) and (-)-sparteine (0.10g, 0.43 mmol) in anisole (10 mL) were added to a dry 100-mL flask with a magnetic stirrer. After being degassed by three freeze-pump-thaw cycles, the polyimide macroinitiator (0.64 g, 0.10 mmol) and CuBr (0.03 g, 0.21 mmol) were charged. The reaction mixture was stirred under a nitrogen atmosphere at 100°C for 24 h. The polymerization was terminated by the addition of THF. After which, the resulting solution was poured slowly into a large amount of methanol to precipitate the polymer solid. It was purified by repeating reprecipitation using THF and methanol, and was made to dry overnight at 80°C in a vacuum oven to obtain MMA-b-PI-b-MMA (1.34 g, 79% yield based on the weight).
    • Distilled MMA (1.07g, 10.7mmol) and (-)-sparteine (0.10g, 0.43 mmol) in anisole (10 mL) were added to a dry 100-mL flask with a magnetic stirrer. After being degassed by three freeze-pump-thaw cycles, the polyimide macroinitiator (0.64 g, 0.10 mmol) and CuBr (0.03 g, 0.21 mmol) were charged. The reaction mixture was stirred under a nitrogen atmosphere at 100°C for 24 h. The polymerization was terminated by the addition of THF. After which, the resulting solution was poured slowly into a large amount of methanol to precipitate the polymer solid. It was purified by repeating reprecipitation using THF and methanol, and was made to dry overnight at 80°C in a vacuum oven to obtain MMA-b-PI-b-MMA (1.34 g, 79% yield based on the weight).
  • 14
    • 34948815895 scopus 로고    scopus 로고
    • In the estimation of contents of the MMA units by 1HNMR (CDCl 3, 500MHz, the signals at δ 3.60, O-CH3 of MMA block) and 4.55, CH2-O- of polyimide macroinitiator) were used
    • 3 of MMA block) and 4.55 (-CH2-O- of polyimide macroinitiator) were used.
  • 15
    • 34948878406 scopus 로고    scopus 로고
    • The TGA of the powder samples (ca. 2 mg) was measured from 40 to 600°C at a heating range of 10°C/min in air (100 mL/ min).
    • The TGA of the powder samples (ca. 2 mg) was measured from 40 to 600°C at a heating range of 10°C/min in air (100 mL/ min).
  • 16
    • 34948867539 scopus 로고    scopus 로고
    • n: 1.04) was purchased from Polymer Laboratories Co., Ltd.
    • n: 1.04) was purchased from Polymer Laboratories Co., Ltd.

* 이 정보는 Elsevier사의 SCOPUS DB에서 KISTI가 분석하여 추출한 것입니다.