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3-甲氧基丙胺的合成研究

Study on Chemial Process of3-Methoxypropan-1-amine

【作者】 张新军

【导师】 朱为宏; 卢中杰;

【作者基本信息】 华东理工大学 , 轻工技术与工程, 2012, 硕士

【摘要】 3-甲氧基丙胺,别名:Y-甲氧基丙胺,在染料和水处理剂及缓蚀剂方面的应用广泛。根据文献分析,对3-甲氧基丙胺的两种合成路线进行综合对比,创新地提出了一种全新的合成工艺路线,即以甲醇与丙烯腈为原料,先制得3-甲氧基丙腈,然后通过连续法催化剂加氢来制得3-甲氧基丙胺。本文主要以甲醇与丙烯腈为原料制备3-甲氧基丙腈,然后以3-甲氧基丙腈为原料,连续加氢制备3-甲氧基丙胺的工艺进行了研究。当反应温度40-45℃,用30%NaOH为催化剂,甲醇:丙烯腈(摩尔比)=1.1:1时,丙烯腈的转化率接近100%。将粗品3-甲氧基丙腈进行甲醇脱除,得到的甲醇套用做3-甲氧基丙腈,得到的纯3-甲氧基丙腈作为加氢原料。在加氢过程中,确定了合适的工艺条件:在加氢釜中加入纯的3-甲氧基丙胺和催化剂、抑制剂,通入氢气,控制反应温度90℃,反应压力2.5MPa,用计量泵将纯3-甲氧基丙腈打入加氢釜中。在此种条件下,3-甲氧基丙胺的收率≥99%。

【Abstract】 3-Methoxypropan-l-amine (MOPA), also named y-methoxy propane-1-amine, is a widely used raw chemical material and fine chemical intermediate. In this dissertation, we compared two preparation processes of MOPA, and proposed a new chemical process to synthesize MOPA with great potential in industrialisation.The process includes two steps:i)3-methoxy propionitrile is prepared with methanol and acrylonitrile as raw materials; ii) MOPA is prepared by continuous hydrogenation of3-methoxypropionitrile. In the first step, the optimized conversion of acrylonitrile is nearly100%under the reaction temperature range from40to45C, using30%NaOH as catalyst, and1.1:1molar ratio of methanol:acrylonitrile. After distilled excess methanol, pure3-Methoxy propionitrile is obtained. The recycled methanol is used for the next batch. In the second step, MOPA is obtained with catalytic hydrogenation, with a yield higher than99%, keeping the reaction temperature at90C, and pressure at2.5MPa.

  • 【分类号】TQ226.3
  • 【下载频次】112
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