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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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大四寫(xiě)論文: 金幣+60, 翻譯EPI+1, ★★★很有幫助 2015-04-08 08:40:36

聚合物表征

所有聚合物的FT-IR光譜在3380cm-1(N-H)、1774cm-1(C=O不對(duì)稱(chēng)的,酰亞胺）、1712cm-1(C=O對(duì)稱(chēng)的,酰亞胺）、1660cm-1（C=O,氨化物）周?chē)@示吸收峰。所有這些PA在1380cm-1(C-N,酰亞胺）顯示出吸收峰表明在這些聚合物中存在酰亞胺雜環(huán)。由于砜基團(tuán)(SO2伸縮）PA10d在1250和1150cm-1處顯示特征吸收峰。在PA10a和PA10d的1H-NMR光譜中，分別在9.98和10.35 ppm作為兩個(gè)單峰出現(xiàn)的酰胺基的N-H質(zhì)子指示出聚合物的側(cè)鏈和主鏈中的酰胺基。芳族質(zhì)子的共振出現(xiàn)在7.00-8.16 ppm的范圍內(nèi)。手性中心的質(zhì)子表現(xiàn)為在4.42-4.43 ppm處的扭曲的雙組雙重峰。PA10a的CH2質(zhì)子的共振表現(xiàn)在4.16 ppm處的一個(gè)單峰。根據(jù)平面或?qū)ΨQ(chēng)中心的缺乏橋質(zhì)子是不等價(jià)的并分別出現(xiàn)在3.20、3.40、4.80和4.89 ppm處。聚合物元素分析的結(jié)果與計(jì)算值有良好的一致性。生成的聚合物的FTIR、1H - NMR和元素分析數(shù)據(jù)列于表3。圖１顯示PA10b和PA10d的X射線散射特性曲線。結(jié)果表明所有的PA都是非晶形的。根據(jù) X射線圖和溶解度數(shù)據(jù),大的蒽側(cè)基部分防止了聚合物鏈被壓緊,這是合成的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作為冷凝劑，二酸8與二胺9a-9g進(jìn)行聚合
通過(guò)下列一般方法制備PA：
制備PA10aII的一個(gè)實(shí)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放進(jìn)一個(gè)瓷皿里,將混合物徹底地打粉,然后將0.15 mL的Py和0.25 mL的NMP加進(jìn)并且混合物打粉3分鐘。微波爐中在100%（900 W）功率的微波器上照射反應(yīng)混合物３分鐘。不斷的攪拌下，將形成的粘稠溶液注入30 mL的甲醇中,用甲醇和熱水徹底地洗滌沉淀物,過(guò)濾,真空干燥得到0.124g(93%)的PA10aII。其他PA，PA10b-PA10g用類(lèi)似的方法制備。

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