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Polymers synthesis
Polymerization under oil bath heating in RTIL as a reaction medium The PAs were prepared by the following general procedure: as an example for the preparation of PA5cI, 0.100 g (0.244 mmol) of diacid 1 and 0.061 g (0.244 mmol) of diamine 2c were dissolved in 0.150 g of 1,3-diisopropylimidazolium bromide (1,3-(isopr)2im]Br), then 0.13 mL (0.488 mmol) of TPP was added. The whole solution was heated at 110 C for 2.5 h. The solution becomes more viscous by progress of the polymerization reaction. The resulting product was dissolved in 1 mL of DMF and was poured into a beaker containing 30 mL of methanol (ethanol), or methanol (ethanol) was directly added to the reaction vessel without using DMF. The obtained solid was filtered off and dried under vacuum to give 0.146 g (94%) of PA5cI.
Polymerization under oil bath heating in NMP as a reaction medium The PAs were prepared by the following general procedure. Taking PA5cII as an example, a mixture of 0.06 g (0.244 mmol) of diamine 2c, 0.10 g (0.244 mmol) of diacid 1, 0.060 g of CaCl2, 0.15 mL of pyridine, 0.14 mL of TPP, and 0.5 mL of NMP was placed into the flask equipped with a mechanical stirrer and a condenser. The mixture blanketed by nitrogen was stirred and refluxed for 5 h. At the end of the reaction, the obtained polymer solution was trickled into 20 mL of stirred methanol or ethanol. The white-stringy polymer was washed thoroughly with hot water and methanol, collected by filtration and dried at 100 C under reduced pressure to give 0.138 g (82%) of PA5cII.

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聚合物的合成
在反應(yīng)介質(zhì)RTIL中油浴加熱進(jìn)行聚合反應(yīng)，通過下列一般方法制備PA：作為PA5cI制備實例, 0.100 g ( 0.244 mmol)的二酸1和0.061 g ( 0.244 mmol)的二胺2c溶于0.150 g 溴化1,3 -二異丙基咪唑溴( 1,3 - ( isopr) 2im] Br),然后將0.13 mL ( 0.488 mmol)的TPP加進(jìn)。全部溶液加熱110℃2.5小時。由于聚合反應(yīng)的發(fā)展溶液變得更為黏稠。生成的產(chǎn)物溶于1 mL的二甲基甲酰胺中然后傾入裝有30 mL甲醇（乙醇)的燒杯中,或者將甲醇（乙醇）直接加到?jīng)]使用二甲基甲酰胺的反應(yīng)容器中。濾出得到的固形物然后真空干燥，得到0.146 g (94%)的PA5cI。
在反應(yīng)介質(zhì)NMP中油浴加熱進(jìn)行聚合反應(yīng)，通過下列一般方法制備PA：作為PA5cII制備實例, 0.06 g ( 0.244 mmol)二胺2c、0.10 g ( 0.244 mmol)二酸1、0.060 g的CaCl2、0.15 mL吡啶、0.14 mL的TPP和0.5 mL的NMP組成的混合物投入配有機(jī)械攪拌器和冷凝器的燒瓶中。氮?dú)獗Ｗo(hù)下混合物攪拌并回流５小時。反應(yīng)結(jié)束時，將得到的聚合物溶液一滴滴注入攪拌下的20 mL甲醇或者乙醇中。這種白色粘稠的聚合物用熱水和甲醇徹底地洗滌,過濾收集，減壓下在100℃干燥，得到0.138 g ( 82%)的PA5cII。

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2樓2015-04-08 09:36:26