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以偶氮二异丁腈、十二胺为主要原料,通过Pinner反应制备了一种两端各带有12个碳烷基链的水溶性偶氮引发剂——2,2’-偶氮二异丁基十二脒盐酸盐AIBL.采用核磁氢谱、元素分析及液相色谱对AIBL进行了结构及纯度表征,采用TGA、DSC和紫外分光光度计研究了其热分解现象和热分解动力学,采用表面张力仪对其表面活性进行了测定.结果表明,所合成的引发剂AIBL具有预想的结构和较高的纯度,其热分解反应属于一级反应,热分解活化能为134.80 k J/mol,70℃下水中的半衰期约为4 h;AIBL在水溶液中具有表面活性,其临界胶束浓度为0.13 g/L,对应的表面张力为33.57 m N/m.以丙烯酰胺为单体、AIBL为引发剂制备了水溶性端基疏水聚合物SPAM.采用溴化法研究其转化率,应用乌氏黏度法、零切黏度法以及荧光探针对其缔合作用进行了研究.结果表明,AIBL具有良好的引发丙烯酰胺聚合的能力;相对于不带疏水长链的引发剂所合成的聚合物PAM,SPAM具有明显的疏水缔合效应,这说明AIBL成功地将疏水长链引入到聚合物的端基中,从而形成端基疏水聚合物.
Using azobisisobutyronitrile and dodecylamine as the main raw materials, a kind of water-soluble azo initiator with 12 alkyl chains at both ends, 2,2’-azobis The isobutyldodecenamidine hydrochloride AIBL was characterized by means of 1H NMR, elemental analysis and liquid chromatography. The thermal decomposition and thermal decomposition kinetics of AIBL were studied by TGA, DSC and UV spectrophotometer. The surface activity of the synthesized initiator AIBL was determined by surface tensiometer.The results showed that AIBL had the expected structure and high purity, and the thermal decomposition reaction was of the first order with the thermal decomposition activation energy of 134.80 kJ / mol, the half-life in water at 70 ℃ is about 4 h; AIBL has surface activity in aqueous solution with a critical micelle concentration of 0.13 g / L and a corresponding surface tension of 33.57 m N / m. With acrylamide as the monomer , AIBL was used as initiator to prepare water-soluble terminal hydrophobic polymer SPAM. The conversion rate was studied by bromination method, and its association was studied by Ubbelohde viscosity method, zero-shear viscosity method and fluorescent probe. , AIBL has a good ability to initiate acrylamide polymerization; relative The polymers PAM and SPAM synthesized by the initiator without hydrophobic long chain have obvious hydrophobically associating effect, which indicates that AIBL successfully introduced the hydrophobic long chain into the terminal of the polymer to form the terminal hydrophobic polymer .