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高纯度4,6-二氨基间苯二酚盐酸盐的合成
引用本文:李金焕,黄玉东,龙军,王超.高纯度4,6-二氨基间苯二酚盐酸盐的合成[J].哈尔滨工业大学学报,2003,35(7):886-889,892.
作者姓名:李金焕  黄玉东  龙军  王超
作者单位:哈尔滨工业大学,理学院,黑龙江,哈尔滨,150001
基金项目:航天创新科技基金(24409035)
摘    要:从l,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l,2,3-三氯苯及2-氯-4,6-二硝基-l,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嗯唑(PBO)的高纯度单体——4,6-二氨基间苯二酚盐酸盐.

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
文章编号:0367-6234(2003)07-0886-04

Synthesis of 4,6-diaminoresorcinol dihydrochloride with high purity
LI Jin-huan,HUANG Yu-dong,LONG Jun,WANG Chao.Synthesis of 4,6-diaminoresorcinol dihydrochloride with high purity[J].Journal of Harbin Institute of Technology,2003,35(7):886-889,892.
Authors:LI Jin-huan  HUANG Yu-dong  LONG Jun  WANG Chao
Abstract: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.
Keywords:4  6-diaminoresorcinol dihydrochloride  poly (p-phenylenebenzobisoxazole) (PBO)  synthesis
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