三相相转移催化法对粗间二硝基苯精制的研究（最终修改稿）

The purification of m-dinitrobenzene by Triphrase Transfer catalysis

摘要:

以氯甲基聚苯乙烯树脂与各种叔胺反应制备了不同的聚合物三相相转移催化剂，并用于对间二硝基苯精制的研究，考察了催化剂、氢氧化钠、甲醇的用量及催化剂种类对邻、对二硝基苯转化率的影响，得到了适宜的精制工艺条件为：m（粗间二硝基苯）：m（甲醇）：m（NaOH）：m（聚苯乙烯吡啶树脂）为1:0.8:0.1:0.12，反应温度约76～78℃，反应时间为2h。在该条件下，邻对二硝基苯的转化率在99.5%以上，精制后的间二硝基苯经色谱分析后其纯度达99.8%，聚苯乙烯吡啶树脂催化剂可重复使用7次以上。

Abstract:

a variety of polymeric phase transfer catalysts with quaternary ammonium active center was synthesized by means of quarterisation of tertiary amine and chloromethylated polystyrene polymer.crude m-dinitrobenzene was purified by Phase Transfer Catalyst to tansfer the p-dinitrobenzene and o-dinitrobenzene into nitrodiphenyl ether.The best process conditions and catalyst were determined on the base of reaction yield of different regents and catalysts.It was concluded that polystyrene polymer pyridine and methnol were the best catalyst and oxyalkylation reagent for this reaction.The feasible process conditions m(crude m-dinitrobenzene):m(methnol): m(sodium hydroxide):m(polystyrene polymer pyridine)was 1:0.8:0.1:0.12,tempeture and reaction time were 76-78℃ and 2h.The purity of m-dinitrobenzene was high to 99.5% to prepare the m-phenylenediamine and recycling of polystyrene polymer pyridine resin was very easy and could be used 7 times.