匹可硫酸钠的合成工艺改进
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篇名: 匹可硫酸钠的合成工艺改进
TITLE:
摘要: 目的:改进匹可硫酸钠的合成工艺。方法:通过改变反应溶剂、加料方式、精制方法和形成结晶水等方法对匹可硫酸钠的合成工艺进行改进。以苯酚为起始原料,与2-吡啶甲醛缩合制得4,4′ -(吡啶-2-基亚甲基)双苯酚,并考察其收率;然后经酯化、成盐,形成结晶水得到匹可硫酸钠,再考察其纯度。结果:关键中间体4,4′ -(吡啶-2-基亚甲基)双苯酚的收率达88%以上,精制后的产品纯度达99.5%以上。匹可硫酸钠一水合物稳定,单一杂质含量小于0.1%。结论:改进后的工艺简单、条件温和,适合大规模生产。
ABSTRACT: OBJECTIVE: To improve the synthesis technology of sodium picosulfate. METHODS: The synthesis technology of sodium picosulfate was improved by changing reaction solvent, charging sequence, refined method and formation of crystal water. Using phenol as raw material, it was condensed with 2-pyridinecarboxaldehyde to achieve 4,4′ -(pyridin-2-ylmethylene) diphenol, and its yield rate was investigated. Sodium picosulfate was obtained after esterification, salification, formation of crystal water, and then its purity was determined. RESULTS: The yield rate of key intermediate 4,4′ -(pyridin-2-ylmethylene) diphenol reached above 88%, and the purity of refined products reached over 99.5%. Sodium picosulfate monohydrate was stable, and the content of single impurity was less than 0.1%. CONCLUSIONS: The improved technology is simple with mild conditions, and suitable for large-scale production.
期刊: 2017年第28卷第31期
作者: 孙晋瑞,李丹,王洪臣,邓玉晓,杨利
AUTHORS: SUN Jinrui,LI Dan,WANG Hongchen,DENG Yuxiao,YANG Li
关键字: 匹可硫酸钠;合成工艺;4,4′ -(吡啶-2-基亚甲基)双苯酚;改进
KEYWORDS: Sodium picosulfate; Synthesis technology; 4,4′ -(pyridin-2-ylmethylene) diphenol; Improvement
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