化工进展

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偶氮二异丁脒盐酸盐的合成新方法

胡志勇,程 原,李 蕾,张巧玲   

  1. 中北大学化工与环境学院
  • 出版日期:2007-12-25 发布日期:2007-12-25

New method for synthesizing azobis(isobutylamidine hydrochloride)

HU Zhiyong,CHENG Yuan,LI Lei,ZHANG Qiaoling   

  1. School of Chemical Engineering and Environment,North University of China
  • Online:2007-12-25 Published:2007-12-25

摘要: 以偶氮二异丁腈为原料,通过碱催化法合成了一种水溶性偶氮引发剂——偶氮二异丁脒盐酸盐,讨论了偶氮二异丁腈甲醇溶液的浓度、甲醇钠用量、氯化铵用量、第一和第二反应时间对终产物产率的影响。研究了其热分解反应动力学,并通过红外光谱法和核磁共振法对其结构进行了表征,最后将此引发剂用于乙酸乙烯酯乳液聚合制得了聚乙酸乙烯酯,并用凝胶渗透色谱仪对聚乙酸乙烯酯的相对分子质量进行了表征。结果表明:偶氮二异丁脒盐酸盐分解反应级数符合一级反应动力学规律,测定其热分解反应活化能Ea为67.39kJ/mol,制得的聚乙酸乙烯酯聚合度为4949。

Abstract: The water soluble azo initiator—azobis(isobutylamidine hydrochloride)(AIBA) was synthesized using ABIN as material by base catalysis method. The effects of the preparation conditions,such as the concentration of ABIN-methanol solution,sodium methoxide dosage,ammonium chloride dosage,the effect of the first and second step reaction time on the yield of end product was investigated. Thermal decomposition reaction kinetics of AIBA was measured. The chemical structure of azobis(isobutylamidine hydrochloride) was characterized by Flourier-infrared spectra(FTIR) and 1HNMR.Finally,poly(vinyl acetate)(PVAc) was prepared using AIBA as initiator by emulsion polymerization. Meanwhile the relative molar mass of PVAc was tested by Gel Permission Chromatography(GPC). The experimental results indicate that:the thermal decomposition reaction grade of AIBA is 1,the decomposition activity energy is 67.39kJ/mol and the of PVAc reached 4949.

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