氯化亚砜法合成水杨腈工艺研究

Study on the synthesis process of salicylonitrile by sulfoxide chloride

[目的]开发氯化亚砜法生产水杨腈工艺,解决了现有工艺使用剧毒化学品、废水废盐量大等问题。[方法]以水杨酰胺为原料,氯化亚砜为脱水剂合成水杨腈,并进行工艺优化。[结果]水杨腈液相外标收率97.6%,实际收率93%(以水杨酰胺计),纯度99.5%(HPLC)。[结论]该工艺反应条件温和,后处理过程简单(水洗、浓缩、析晶),产品纯度高,废水量较少,适合工业化生产。

[Aims] This study aims to develop the production of salicylonitrile by sulfoxide chloride method, which solved the problems of the existing process using highly toxic chemicals, dangerous operation and large amount of waste water and salt. [Methods] Salicylamide was used as the raw material and sulfoxide chloride was used as dehydrating agent to synthesize salicylonitrile, and the process was optimized. [Results] The liquid phase external standard yield of salicylonitrile was 97.6%, the actual yield was 93%(based on salicylamide), and the purity was 99.5%(HPLC). [Conclusions] The process has mild reaction conditions, simple post-treatment process(washing with water,concentration and crystallization), high product purity and less waste water, and is suitable for industrial production.