高纯度4,6-二氨基间苯二酚盐酸盐的合成  

Synthesis of 4,6 -diaminoresorcmol dihydrochloride with high purity

作　　者：李金焕[1] 黄玉东[1] 龙军[1] 王超[1] 

机构地区：[1]哈尔滨工业大学理学院,黑龙江哈尔滨150001

出　　处：《哈尔滨工业大学学报》2003年第7期886-889,892,共5页Journal of Harbin Institute of Technology

基　　金：航天创新科技基金(24409035)

摘　　要：从1,2,3-三氯苯出发合成了高纯度的4,6-二氨基间苯二酚盐酸盐,并采用FT-IR、元素分析、1H NMR等方法对各步中间体及4,6-二氨基间苯二酚盐酸盐进行了表征分析.结果表明成功地制得了4,6-二硝基1,2,3-三氯苯及2-氯-4,6-二硝基-1,3-间苯二酚中间体,结合Na元素分析证实,以H3PO4水溶液代替普遍采用的HAc-NaAc水溶液为介质的加氢工艺有效地解决了4,6-二氨基间苯二酚盐酸盐无机盐污染问题,制得了合成聚对苯撑苯并二噁唑(PBO)的高纯度单体--4,6-二氨基间苯二酚盐酸盐.4,6-diaminoresorcinol dihydrochloride was prepared from 1,2,3-trichlorobenzene. Some analyses such as FT-IR, elemental analysis and 'HNMR were used to confirm the intermediates--1,2,3-tri-chloro-4, 6-dinitrobenzene and 2-chloro-4,6-dinitro-resorcinol, and the final product-4,6-diaminoresorcinol dihydrochloride. Furthermore the analysis of sodium quantity in the 4,6-diaminoresorcinol dihydrochloride showed that the contamination problem from some inorganic salts was solved effectively by using phosphoric acid aqueous medium instead of acetic acid -sodium acetate system in the catalytic hydrogenation step. As a result, the monomer for the synthesis of poly(p-phenylenebenzobisoxazole) (PBO) was obtained with high purity.

关 键 词：4 6-二氨基间苯二酚盐酸盐 杂环聚合物 合成 聚对苯撑苯并二嗯唑 红外光谱 表征分析 加氢工艺 无机盐污染 

分 类 号：O633.5[理学—高分子化学]