有机胺分解氯化铵工艺设计

近年来，纯碱的需求量快速增长。中国纯碱企业多采用联碱法生产纯碱，联碱法生产纯碱工艺每生产1t纯碱就会副产物氯化铵。而全球范围内氯化铵的年总消耗量并不高，其生产主要集中在中国。

本文旨在研究氯化按分解制氨气和氯化氢气体的关键技术，采用有机胺介质法分解氯化按的工艺方法，对有机胺分解氯化按技术进行了系统的研究，分别采用了四种有机胺对氯化按分解释放氨气和有机胺盐酸盐分解释放氯化氢气体两个反应过程进行了对比研究。

在利用有机胺介质法分解氯化按释放氨气实验过程中，通过对三己胺、三(2-乙基己基)胺、三辛胺、三月桂胺四种有机胺的反应温度、反应时间、异戊醇有机溶剂与氯化按的进料摩尔比、有机胺与氯化按摩尔比进料、氮气流量等影响因素的对比考察，发现与其他有机胺相比，三己胺具有反应时间更短，氨气收率更高的优势，氨气收率可达到97.5%。

在有机胺盐酸盐分解释放氯化氢的实验过程中，通过对三己胺盐酸盐、三(2-应温度、反应时间、非极性有机溶剂、氮气流量等影响因素的对比考察，发现采用三己胺盐酸盐的有机胺盐酸盐分解反应具有所需反应时间最短，所需非极性有机溶剂和氮气流量更少，氯化氢收率更高的优势，氯化氢收率可达到94.65%。

关键词：有机胺法；氯化铰；热分解；三己胺

In recent years, the demand for soda has increased rapidly. The Chinese soda enterprises mostly use the combined alkali process to produce the soda, which is a by-product of ammonium chloride for every 1 ton of soda soda produced by the combined alkali production process. However, the total annual consumption of ammonium chloride worldwide is not high, and its production is mainly concentrated in China.

In this paper, the key technology of chlorination to produce ammonia and hydrogen chloride gas by chlorination is studied. The decomposition and chlorination of organic amine by organic amine medium is studied systematically. Four kinds of organic amines were used to study the process of chlorination releasing ammonia according to decomposition and organic amine hydrochloride decomposing and releasing hydrogen chloride respectively.

In the process of decomposing chlorination with organic amine medium according to ammonia release, the reaction temperature and reaction time of four organic amines, namely, trihexylamine, triethylhexyl) amine, trioctylamine and lauryl amine, were studied. Compared with other organic amines, the reaction time of trihexylamine was shorter than that of other organic amines, such as the molar ratio of organic solvents to chlorination, the molar ratio of organic amines to chlorination, the flow rate of nitrogen and so on, and compared with other organic amines, the reaction time of trihexylamine was shorter than that of other organic amines. The higher yield of ammonia gas is, the yield of ammonia gas can reach 97.5%.

In the process of decomposition and release of hydrogen chloride from organic amine hydrochloride, the influence factors such as trihexylamine hydrochloride, trihexylamine hydrochloride, reaction time, nonpolar organic solvent, nitrogen flow rate and so on were investigated. It is found that the decomposition reaction of organic amine hydrochloride with trihexylamine hydrochloride has the advantages of the shortest reaction time, less non-polar organic solvent and nitrogen flow rate, and higher yield of hydrogen chloride. The yield of hydrogen chloride can reach 94.65%.

Keywords: organic amine method; chlorination hinge; thermal decomposition; trihexylamine

1.绪论1

1. 1研究背景1

1. 2氯化铵分离回收技术2

1. 2. 1电化学方法2

1. 2.2催化分解法3

1. 2.3无机酸盐法3

1. 2.4金属氧化物法5

1. 2.5有机胺法7

1.3选题依据和主要内容7

2实验部分8

2. 1实验原料和试剂8

2. 2实验装置和操作步骤8

2.2.1实验装置8

2.2.2回收氨气操作步骤10

2. 2. 3异丙醇蒸馏装置10

2. 2. 4回收氯化氢操作步骤10

2.3分析方法确定10

2.3.1分析原理10

2.3.2分析仪器11

2.3.3分析操作步骤11

2. 3. 4分析数据的处理11

2.4有机胺法分解氯化铵实验可行性研究12

2. 4. 1氨气初步回收率12

2. 4. 2氯化氢气体初步回收率12

2. 4. 3实验循环可行性研究12

2. 5有机胺法分解氯化铵制备氨气的工艺考察16

2. 5. 1温度对反应的影响16

2.5.2三辛胺与氯化铵的摩尔比对反应的影响17

2. 5. 3异丙醇与三辛胺摩尔比对反应的影响17

2. 5. 4氮气流量对反应的影响18

2.5.5反应时间对反应的影响19

结论20

致谢21

参考文献22

1.氮气钢瓶2.缓冲瓶3.转子流量计4.油浴锅5.水银温度计6.填料柱

7.二口连接管8.注射器9.球形冷凝管10.吸收瓶

图3氯化铵分解回收氯化氢装置图