浓硫酸催化制备4，6-二氨基间苯二酚盐酸盐  

Synthesis of 4,6-diaminobenzene-1,3-diol dihydrochloride catalyzed by concentrated sulfuric acid

作　　者：陈凤贵[1] 高镱萌[1] 徐愿坚[1] 

机构地区：[1]中国科学院重庆绿色智能技术研究院,环境友好化学过程研究中心,重庆400714

出　　处：《化工新型材料》2015年第4期43-45,48,共4页New Chemical Materials

基　　金：国家自然科学基金(51303206,官能化聚芳酰胺热处理制备聚对苯撑苯并双口恶唑的探索研究);重庆绿色智能技术研究院青年创新基金(Y23H040M10,高性能纤维聚对苯撑苯并口恶唑的聚合工艺研究)

摘　　要：4,6-二氨基间苯二酚(DAR)盐酸盐单体的制备是合成高性能纤维聚对苯撑苯并双口恶唑(PBO)的关键,而间苯二酚乙酰化、肟化法是高效制备该单体的重要方法。新方法采用浓硫酸作为催化剂改进二肟中间体Beckmann重排、水解制备DAR的过程,成功制备得高纯度的DAR单体。并通过对温度、浓硫酸使用量等影响反应的主要因素进行比较研究,总结出浓硫酸催化制备DAR的合适条件。该方法不仅有效解决了使用多聚磷酸制备DAR时操作复杂等问题,而且节约了成本,缩短了反应时间。Concentrated sulfuric acid was used to prepare the 4,6-diaminobenzene-1,3-diol dihydrochloride（DAR）by beckmann rearrangement of dioxime in high yields and high regioselectivity. Conditions for beckmann rearrangement were well studied,especially for effect of the temperature and ratio of concentrated sulfuric acid to dioxime. The results showed that the temperature control was critical in the synthesis of DAR, and the beckmann rearrangement was optimised to be car- ried out at 95（C with the molar ratio of concentrated sulfuric acid to dioxime 8 ~ 1. By using this method,the experiments were carried out with easier operation, shorter time and reduced cost.

关 键 词：2 4二氨基间苯二酚 贝克曼重排 浓硫酸 

分 类 号：TQ243[化学工程—有机化工]