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Polymer characterization The FT-IR spectra of all polymers showed absorptions around 3380 cm-1 (N–H),1774 cm-1 (C=O asymmetric, imide), 1712 cm-1 (C=O symmetric, imide),1660 cm-1 (C=O, amide). All these PAs exhibited absorption at 1380 cm-1 (C–N, imide) that reveal the presence of the imide heterocycle in these polymers. The PA10d showed characteristic absorptions at 1250 and 1150 cm-1 due to the sulfone moiety (SO2 stretching). In the 1H-NMR spectra of PA10a and PA10d, appearances of the N–H protons of amide groups at 9.98 and 10.35 ppm as two singlet peaks, respectively, indicate amide groups in the polymer’s side chain and main chain. The resonance of aromatic protons appeared in the range of 7.00– 8.16 ppm. The proton of the chiral center appeared as distorted doublet of doublet at 4.42–4.43 ppm. The resonance of the CH2 protons of PA10a appeared as a singlet peak at 4.16 ppm. The bridge protons are unequivalent according to the lack of plane or center of symmetry and appeared at 3.20, 3.40, 4.80, and 4.89 ppm, respectively. The results of elemental analysis of polymers were in good agreement with the calculated values. FTIR, 1H-NMR, and elemental analysis data of the resulting polymers are listed in Table 3. Figure 1 shows the X-ray scattering patterns for PA10b and PA10d. The results demonstrate that all the PAs are amorphous. According to the X-ray patterns and solubility data, the bulky anthracenic pendant moieties, which prevent polymer chains from packing well, should be responsible for the amorphous and good solubility characteristics of the synthesized PAs. Method II: polymerization of diacid 8 with diamines 9a–9g using NMP/Py/TPP/CaCl2 as condensing agent The PAs were prepared by the following general procedure: as an example for the preparation of PA10aII, 0.10 g (1.70 9 10-4 mol) of diacid 8, 0.0338 g (1.70 9 10-4 mol) of diamine 9a, 0.06 g of CaCl2 and 0.11 mL (4.26 9 10-4 mol) of TPP were placed in a porcelain dish, and the mixture was ground completely, then 0.15 mL of Py, and 0.25 mL of NMP was added and the mixture was ground for 3 min. The reaction mixture was irradiated in the microwave oven for 3 min on 100% (900 W) power of microwave apparatus. The resulting viscous solution was poured into 30 mL of methanol with constant stirring, and the precipitate was washed thoroughly with methanol and hot water, filtered, dried under vacuum to give 0.124 g (93%) of PA10aII. The other PAs, PA10b–PA10g were prepared with analogous procedures. |
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jiangguofeng
金虫 (著名写手)
- 翻译EPI: 248
- 应助: 41 (小学生)
- 金币: 25668.4
- 红花: 25
- 帖子: 2050
- 在线: 566.7小时
- 虫号: 72410
- 注册: 2005-06-04
- 专业: 合成药物化学
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大四写论文: 金币+60, 翻译EPI+1, ★★★很有帮助 2015-04-08 08:40:36
大四写论文: 金币+60, 翻译EPI+1, ★★★很有帮助 2015-04-08 08:40:36
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聚合物表征 所有聚合物的FT-IR光谱在3380cm-1(N-H)、1774cm-1(C=O不对称的,酰亚胺）、1712cm-1(C=O对称的,酰亚胺）、1660cm-1（C=O,氨化物）周围显示吸收峰。所有这些PA在1380cm-1(C-N,酰亚胺）显示出吸收峰表明在这些聚合物中存在酰亚胺杂环。 由于砜基团(SO2伸缩）PA10d在1250和1150cm-1处显示特征吸收峰。在PA10a和PA10d的1H-NMR光谱中，分别在9.98和10.35 ppm作为两个单峰出现的酰胺基的N-H质子指示出聚合物的侧链和主链中的酰胺基。芳族质子的共振出现在7.00-8.16 ppm的范围内。手性中心的质子表现为在4.42-4.43 ppm处的扭曲的双组双重峰。PA10a的CH2质子的共振表现在4.16 ppm处的一个单峰。根据平面或对称中心的缺乏桥质子是不等价的并分别出现在3.20、3.40、4.80和4.89 ppm处。聚合物元素分析的结果与计算值有良好的一致性。生成的聚合物的FTIR、1H - NMR和元素分析数据列于表3。图１显示PA10b和PA10d的X射线散射特性曲线。结果表明所有的PA都是非晶形的。根据 X射线图和溶解度数据,大的蒽侧基部分防止了聚合物链被压紧,这是合成的PA具有非晶形的和良好溶解度特性的原因。 方法II：使用NMP/Py/TPP/CaCl2作为冷凝剂，二酸8与二胺9a-9g进行聚合 通过下列一般方法制备PA： 制备PA10aII的一个实例, 0.10 g ( 1.70 9 10 - 4 mol)的二酸8、0.0338 g ( 1.70 9 10 - 4 mol)的二胺9a、0.06 g的CaCl2和0.11 mL ( 4.26 9 10 - 4 mol)的TPP放进一个瓷皿里,将混合物彻底地打粉,然后将0.15 mL的Py和0.25 mL的NMP加进并且混合物打粉3分钟。微波炉中在100%（900 W）功率的微波器上照射反应混合物３分钟。不断的搅拌下，将形成的粘稠溶液注入30 mL的甲醇中,用甲醇和热水彻底地洗涤沉淀物,过滤,真空干燥得到0.124g(93%)的PA10aII。其他PA，PA10b-PA10g用类似的方法制备。 |
2楼2015-04-07 11:19:34