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Techniques The apparatus used for the polycondensation was a Samsung microwave oven(2450 MHz, 900 W). Proton nuclear magnetic resonance (1H-NMR, 500 MHz) spectra were recorded in DMSO-d6 solution using a Bruker (Germany) Avance 500 instrument at Sharif University of Technology, Tehran, Iran. Proton resonances are designated as singlet (s), doublet (d), doublet of doublet (dd), and multiplet (m). FT-IR spectra were recorded on (Jasco-680, Japan) spectrophotometer. The spectra of solids were obtained using KBr pellets. The vibrational transition frequencies are reported in wavenumbers (cm-1). Band intensities are assigned as weak (w), medium (m), strong (s), and broad (br). Inherent viscosities were measured by using a Cannon–Fenske Routine Viscometer (Germany) at concentration of 0.5 g dL-1 at 25 C. Specific rotations were measured by a Jasco Polarimeter (Japan). Quantitative solubility was determined using 0.05 g of the polymer in 1 mL of solvent. Thermal gravimetric analysis (TGA) data for polymers were taken on V5.1A DuPont 2000 at a heating rate of 10 C min-1 under N2 atmosphere. Differential scanning calorimetry (DSC) data were recorded on a DSC-PL-1200 instrument at a heating rate of 20 C min-1 under nitrogen atmosphere by the Research Institute of Polymer and Petrochemical of Iran. Glass transition temperatures (Tg) were read at the middle of the transition in the heat capacity taken from the heating DSC traces. Elemental analyses were also performed by Tarbit Moalem University,Tehran, Iran. Monomer synthesis 5-[3-Phenyl-2-(9,10-dihydro-9,10-ethanoanthracene-11,12-dicarboximido)propanoylamino] isophthalic acid (8) was prepared (Scheme 1) according to our previous works [10, 20]. Polymer synthesis Method I: polymerization of diacid 8 with diamines 9a–9g in [1,3-(pr)2im]Br/TPP as condensing agent |
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金虫 (著名写手)
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大四写论文: 金币+50, 翻译EPI+1, ★★★很有帮助 2015-04-07 08:26:12
大四写论文: 金币+50, 翻译EPI+1, ★★★很有帮助 2015-04-07 08:26:12
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技术装备 缩聚反应所用的装置是三星牌微波炉( 2450 MHz, 900 W)。质子核磁共振(1H NMR, 500 MHz)波谱是在二甲亚砜- d6溶液中使用Avance 500核磁共振仪布鲁克公司（德国）在伊朗,德黑兰,Sharif技术大学记录的。 质子共振指定为单峰(s)、双峰(d)、双重双峰和多重峰(m)。FT-IR光谱是用(日本, Jasco - 680）分光光度计记录的。固体光谱是使用KBr压片法获得的r。振动跃迁频率是以波数（cm-1）报告的。谱带强度是以弱(w)、中(m)、强(s)和宽( br)的方式分配的。特性粘度是通过使用坎农-芬斯克常规粘度仪（德国）于0.5 g dL-dL-1的浓度和25℃温度下测定的。比旋光率是通过Jasco偏振光仪（日本）测定的。定量溶解度是通过使用0.05 g聚合物在1mL溶剂中进行测定的。聚合物的热解重量分析(TGA)数据是通过使用V5.1A杜邦2000，以10℃min-1的加热速度，在N2氛围下采取的。差示扫描量热法( DSC)数据是由伊朗的聚合物和石油化学品研究所通过使用DSC-PL-1200仪器以20℃min-1的加热速度，在氮气氛围中记录的。玻璃态转化温度(Tg)是在取自热DSC曲线的热容量中转移的中间段读取的。元素分析也是由伊朗,德黑兰的Tarbit Moalem大学完成的。 单体的合成 5-[3-苯基-2-(9,10-二氢-9,10-桥亚乙基-蒽-11,12-二甲酰亚胺基)丙酰氨基]间苯二甲酸(8)是依据我们以前的研究[10, 20]而制备的(图1)。聚合物的合成方法I :二酸8与二胺9a-9g在[ 1,3-(pr)2im]Br/TPP冷凝剂中进行聚合 |
2楼2015-04-06 20:22:19
