Abstract Co-ZSM-5 zeolite has high catalytic activity in aldehyde-ammonia condensation reaction. Co-ZSM-5 zeolite catalyst has the main characteristies moderate reaction condition, high shape selectivity and little byproduct. Aldehyde-ammonia condensation reaction is one of the typical routes to manufacture alkylpyridine. By means of SEM, FT-IR, XRD, NMR, TG/TGA, BET techniques, the effects of calcinations on the structure of Co-ZSM-5 zeolite catalyst were studied. The Co-ZSM-5 zeolite calcinated at different temperature had been used to manufacture alkylpyridine from aldehydes and ammonia. Experimental results showed that catalyst calcinated at 530°C had a considerably surface image. The Co-ZSM-5 zeolite catalyst had three phases of weight loss. The framework of zeolite was very sensitive to the FT-IR spectra at ～1225、～1102、～953、～803、～553cm^-1. The framework of zeolite calcinated at temperature higher than 600°C would suffer dealumination. The framework of zeolite calcinated at temperature higher than 750°C would suffer severe destruction. Using Co-ZSM-5 zeolite calcinated at 450～600°C, alkylpyridine could be obtained in higher yield.
Key words Calcination temperature, Co-ZSM-5, Aldehyde-ammonia condensation, Alkylpyridine

焙烧温度对Co-ZSM-5分子筛催化剂上醛氨缩合的影响

蒋劼 毛东森^# 杨为民^# 卢冠忠^*
(华东理工大学化学与制药学院 上海 200237 ^#上海石油化工研究院 上海 201208)

摘要 Co-ZSM-5分子筛催化剂是一种具有较强催化活性的醛氨缩合催化剂，其主要特点是反应条件温和、择形选择性高、副产物较少等。醛氨缩合反应是制备烷基吡啶最具代表性的反应路线之一。本文用SEM、XRD、IR、TG/TGA、NMR和BET等技术考察了焙烧温度对Co-ZSM-5分子筛的物理化学特性的影响，并将不同焙烧温度下制备的Co-ZSM-5分子筛用于醛氨缩合合成烷基吡啶的反应。研究表明，在530°C焙烧制得的催化剂具有较好的表面形貌特征；Co-ZSM-5分子筛有三段失重过程；～1225、～1102、～953、～803、～553cm^-1谱带对分子筛的骨架结构变化十分敏感；当焙烧温度高于600°C后，分子筛骨架脱铝明显；焙烧温度高于750°C后，分子筛骨架结构随焙烧温度的升高而遭到破坏。采用焙烧温度在450～600°C范围制得的Co-ZSM-5分子筛催化剂合成烷基吡啶可达较高的产率。
关键词 焙烧温度 Co-ZSM-5 醛氨缩合 烷基砒啶

蒋劼 男，28岁，硕士生，现从事精细化学品的研究与开发。 *联系人
中国石油化工股份有限公司基金资助项目(200021)

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