【摘要】 以Pd/C为催化剂,用高浓度(50%)间硝基苯磺酸钠加氢还原制备间氨基苯磺酸钠。对加氢反应的机理进行了分析,采用高效液相色谱建立了反应过程中间体的中控分析方法,采用液相色谱-质谱联用仪对全部中间体结构进行了鉴定。结果表明:工业品原料中含有9%的对硝基苯磺酸钠异构体;反应过程中主要的副产物为氧化偶氮苯磺酸钠;当催化剂活性低时,加氢反应时间延长;主要控制步骤为氧化偶氮苯磺酸钠转化为氢化偶氮苯磺酸钠的过程。更多还原

【Abstract】 Metanilic acid sodium salt was synthesized from high concentration( 50%) sodium m-nitrobenzenesulfonate with Pd/C as catalyst by catalytic hydrogenation. Mechanism of the hydrogenation was analyzed. The reaction process was researched by HPLC,the structures of all intermediates were quantified by LC-MS. The results showed that there was 9% isomer p-nitrobenzene sulfonate in the industrial raw material; the main by-product of the reaction was azoxybenzene; the reaction time was prolonged with the catalyst activity decreased; converting azoxybenzene into hydride azobenzene was the rate-determining step.更多还原