【作者】 杨浩；

【导师】 肖国民；

【作者基本信息】 东南大学 ， 化学工艺， 2004， 硕士

【摘要】 吡啶氯化物都是重要的化工原料,以吡啶直接氯化生产吡啶氯化物尤其是深度氯化物的研究多年来一直是化工行业的一个热点,也一度被誉为世界性难题。本文在调研了大量文献的基础上,设计了吡啶氯化反应系统,筛选了不同的催化剂载体和催化剂活性组分,并且优化了反应的工艺条件,获得了比较好的结果,为以后工业化生产奠定了基础。根据实际情况,计算了氯气、氮气和吡啶所需要的预热器换热面积,设计并加工了切实可行的蛇管式沙浴预热装置,设计并加工了固定床直管式吡啶反应器、撞击流气体混合器。经过调试能够正常运转。结果表明催化剂(20%CoCl2、80%LaCl3/C)是一种催化活性比较高的吡啶氯化催化剂,对于该催化剂,最优的反应条件是原料配比值为nCl2:nPyridine = 8:1左右,适宜的反应温度为330～340℃,最佳的吡啶流量为280ml/h左右。并且在此条件下,吡啶的转化率可以达到90%以上,目的产物五氯吡啶收率可以达到80%左右(纯度95%)。该催化剂在最优条件下经过系统正常运转42h后仍然有较好的活性和选择性,证明此反应系统设计合理,经济上可行,能够为以后的中试和工业化生产提供参考。进行了合理的工业化概念设计——年产1000吨五氯吡啶工业装置设计,经过经济性核算,五氯吡啶成本(不计算固定资产和能耗)为1.912万元/吨,远低于市场价格。更多还原

【Abstract】 Pyridine and chloro-pyridines are very useful chemical materials,chemical intermediate, medical and pesticide intermediates. In recent years, it has been a hotspot in chemical field that chloro-pyridines are produced directly from pyridine, especially the poly-chloro-pyridine. So, it has been considered as a hard question world widely.In this paper, according to a great deal of references, the system of pyridine-chlorination was built. Several catalyst carrier and active component were tested. The optimal technologic conditions were found, which reached in a better result. A foundation was built for industrialization latter.According to the practical instance, the warm-up areas of nitrogen, chlorine, and pyridine warm-uppers were calculated. Three spiral-piping warm-uppers warmed by sand and upright fixed bed reactor for pyridine chlorination were designed and machined. They worked naturally after debugged.The result showed the catalyst (20%CoCl280%LaCl3) was a high active one for pyridine chlorination. About this catalyst the optimum react conditions are the ratio of material: nCl2:nPyridine = 8:1, the fitting react temperature: 330～340℃, the optimal flux of pyridine: 280ml/h or so.Under this condition, the conversation of pyridine reached over 90%, the yield of pentachloropyridine reached about 80%(95% pure). The catalyst has good activity and selectivity after continuous working naturally. A notional industrial design of pentachloropyridine with annual production 1000 tons was built. After economical calculation, the cost of pentachloropyridine (except fixed capital and energy sources) is far below the price on the market. It proved that this reaction system is reasonably designed and feasible economically and could be used for the magnified test and industrialization.更多还原