摘要
该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℃，8h；高温区脱水温度为210—265℃，5h；复合型催化剂ZnO／AI2O3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共振氢谱验证，同时气质色谱检测显示纯度为92％，具有工业化价值。
In this paper, sebaconitrile was successfully prepared using sebacic acid 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 show that the optimal synthesis conditions are as follows：the lower temperature region （140 -210 ℃ ） are favorable to the amidation reaction and the corresponding reaction time is 8 h;however the dehydration reaction is very effective within the higher temperature region （210 -265 ℃ ） and the corresponding dehydration time is 5 h. ZnO/A12 03 catalysis with a mass fraction of 6% gave a yield of 83%. The crude product was characterized by means of 1HNMR and the purity of the prepared sebaconitrile was 92% via GC-MS detection, which indicates that the sebaconitrile synthesized in this paper holds out a oromisin potential for industrialization.
出处
《精细化工》
EI
CAS
CSCD
北大核心
2013年第11期1284-1286,1302,共4页
Fine Chemicals
基金
山西省自然科学青年基金(2012021007-5)~~
关键词
癸二酸
癸二酰胺
癸二腈
氨化
催化
精细化工中间体
sebacic acid
decanediamide
sebaconitrile
ammoniation
catalysis
fine chemicalintermediates
