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化工学报  2015 

牛磺酸合成工艺的改进

DOI: 10.11949/j.issn.0438-1157.20141023, PP. 171-178

Keywords: 牛磺酸,亚硫酸铵,脱盐,结晶,化学过程

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Abstract:

乙醇胺酯化-磺化法制备牛磺酸工艺分为酯化反应和磺化反应两部分,用亚硫酸铵代替亚硫酸钠作为磺化反应的原料,在含氨气体存在下与2-氨基乙醇硫酸酯进行磺化反应,得到的优化条件为:反应温度为98℃,反应时间为12h,物料配比(n亚硫酸铵:n酯)为1.65,分4批加料,2-氨基乙醇硫酸酯的转化率可以达到76.43%。对磺化反应后的混合溶液的分离提纯进行研究。首先用化学沉淀法除去其中的无机盐(NH4)2SO4,滤出沉淀物硫酸盐后稍微加热母液,生成的NH3·H2O分解放出的氨气用于磺化反应过程,此过程的除盐率达到98%以上。采用溶剂结晶法对含有牛磺酸、未反应完的2-氨基乙醇硫酸酯和不到2%的滤液物系进行分离。用均匀实验设计法考察了结晶温度、结晶时间、降温速率和搅拌速率对牛磺酸结晶过程的影响,并用软件对实验结果进行回归分析,得到溶剂结晶较优的工艺条件为:结晶温度为13.9℃,结晶时间为1h,搅拌速率为低速搅拌(350~450r·min-1),降温速率为0.5℃·min-1。在此条件下,牛磺酸的一次结晶率可达到67.94%,纯度接近100%。

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