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Synthesis and characterization of N-acryloylcarbazole/methyl methacrylate copolymers

机译:N-丙烯酰基咔唑/甲基丙烯酸甲酯共​​聚物的合成与表征

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Copolymers of N-acryloylcarbazole (A) and methyl methacrylate (M) were synthesized in different infeed ratios. The composition of the copolymer was determined by the help of H-1 NMR spectrum. The comonomer reactivity ratios determined by Kelen-Tudos (KT) and non-linear error-in-variables methods were r(A) = 1.12 +/- 0.16, r(M) = 0.94 +/- 0.14, and r(A) = 1.05, r(M) = 0.90, respectively. Complete spectral assignments of the H-1 and C-13 H-1 NMR spectra of the copolymers were done by the help of distortionless enhancement by polarization transfer (DEPT) and two-dimensional NMR techniques, such as heteronuclear single quantum coherence (HSQC), total correlation spectroscopy (TOCSY), and heteronuclear multiple bond correlation (HMBC). The methine, alpha-methyl, and carbonyl carbon resonances were found to be sequence sensitive. The signals obtained were broad because of the restricted rotation of bulky carbazole group and the quadrupolar effect of nitrogen present in carbazole moiety. Glass transition temperatures (T-g) were determined by differential scanning calorimetry and were found to be characteristic of copolymer composition. As the N-acryloylcarbazole content increases, the T-g increases from 378.3 K for poly(methyl methacrylate) to 430.4 K for poly(N-acryloylcarbazole). Variation in T-g with the copolymer composition were found to be in good agreement with theoretical values obtained from Johnston and Barton equations. (c) 2006 Wiley Periodicals, Inc.
机译:以不同的进料比合成了N-丙烯酰基咔唑(A)和甲基丙烯酸甲酯(M)的共聚物。借助H-1NMR光谱确定共聚物的组成。通过Kelen-Tudos(KT)和非线性变量误差法确定的共聚单体反应率是r(A)= 1.12 +/- 0.16,r(M)= 0.94 +/- 0.14和r(A) = 1.05,r(M)= 0.90。借助极化转移(DEPT)和二维NMR技术(例如异核单量子相干性(HSQC))进行无畸变增强,完成了共聚物的H-1和C-13 H-1 NMR光谱的完全光谱分配。 ,总相关光谱(TOCSY)和异核多键相关(HMBC)。发现次甲基,α-甲基和羰基碳共振是序列敏感的。由于笨重的咔唑基团的旋转受限以及咔唑部分中存在的氮的四极效应,获得的信号较宽。通过差示扫描量热法测定玻璃化转变温度(T-g),发现其是共聚物组成的特征。随着N-丙烯酰基咔唑含量的增加,T-g从聚甲基丙烯酸甲酯的378.3 K增加到聚N-丙烯酰基咔唑的430.4K。发现T-g随共聚物组成的变化与从Johnston和Barton方程获得的理论值高度吻合。 (c)2006年Wiley Periodicals,Inc.

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