癸二酸合成高纯度癸二腈的工艺研究

The sebacic acid synthesis of high-purity Sebaconitrile

摘要:

本论文以癸二酸和氨气为原料采用一步法合成癸二腈，详细地探讨了催化剂组成，反应温区和反应时间等因素对收率的影响。并得到了最佳合成条件：将反应分为高低两个温区，低温区酰胺化反应温度为140～210 oC，8小时；高温区脱水温度为210～265 oC，5小时；复合型催化剂ZnO/Al2O3显示最好的催化效果，相应的质量分数为6%，收率83%。癸二腈粗产物已经过核磁氢谱验证，同时气质色谱检测显示纯度为92%，具有工业化价值。

Abstract:

In this paper, sebaconirile had been successfully prepared using sebacic and ammonia as raw materials under the condition of catalysts. The effects of catalysts with different compositions, reaction temperature and time were studied. The results showed that the optimal synthesis condition as follows: the lower temperature region (140-210 oC) were favorable for amidition reaction and the corresponding reaction time is 8h, however the dehydration reaction is very effective under the higher temperature region (210-265 oC) and the corresponding dehydration time is 5h. ZnO/Al2O3 catalysis with mass faction of 6% revealed the yield of 83%. The crude product had been characterized by HNMR and the purity of prepared sebaconitrile was 92% via temperament chromatograph , which indicated that the sebaconitrile synthesized in this paper would have the good value of industrialization