4,6-二氨基间苯二酚盐酸盐合成研究

以三氯苯为原料,经硝化、水解和催化加氢三步反应,合成聚对苯撑苯并双噁唑(PBO)单体4,6-二氨基间苯二酚盐酸盐(DADHC)。研究了各中间体和单体合成中的影响因素,确定了各步反应的最佳工艺参数。对合成的各中间体和单体采用元素分析(EA)、傅立叶变换红外光谱(FT-IR)、氢核磁(1H NMR)、碳核磁(13C NMR)和高效液相色谱(HPLC)等方法进行了表征分析。结果表明,各中间体和单体均达到预定要求,纯度和收率较高。研制了一套单体防氧化分离Pd/C过滤装置,实现了Pd/C催化剂的回收再利用,解决了单体易氧化、Pd/C易失活难题,提高了生产效率,降低了生产成本。

Study on synthetic technology of 4,6-diaminoresorcinol dihydrochloride

Taking trichlorobenene as raw material,4,6-diaminoresorcinol dihydrochloride which is monomer of PBO was synthesized by nitration,hydrolyzation and catalytic hydrogenation reaction.The effect factors on synthesis of intermediate and monomer were investigated,and the optimum process parameters in the course of reaction were determined.Performances of intermediate and monomer were characterized by EA,FT-IR,~1H NMR,~(13)C NMR and HPLC methods.The results show that all the intermediates and monomers meet the preset requirements,and they all possess high purity and productivity.A device for filtering Pd/C catalyzer and preventing monomer from oxidation was developed to realize recovery and reuse of Pd/C catalyzer.The easy oxidation problem for monomer and easy loss problem for Pd/C activity were solved so as to improve production efficiency and reduce the cost.