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以氯甲基聚苯乙烯树脂分别与三甲胺、三乙胺、三丁胺、三乙醇胺、吡啶5种叔胺反应,制备了不同的聚合物三相相转移催化剂,并用于间二硝基苯精制,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)=1∶0.8∶0.1∶0.12,反应温度76～78℃,反应时间2 h。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色谱纯度达99.8%,间二硝基苯的收率在99%左右,聚苯乙烯吡啶树脂催化剂可重复使用7次以上。
Different polymeric three-phase phase-transfer catalysts were prepared by the reaction of chloromethyl polystyrene resins with five kinds of tertiary amines, such as trimethylamine, triethylamine, tributylamine, triethanolamine and pyridine, respectively. The effects of the amount of catalyst, sodium hydroxide and methanol and the type of catalyst on the conversion of o- and p-dinitrobenzene were investigated. The optimum technological conditions were as follows: m (crude dinitrobenzene): m Methanol): m (NaOH): m (polystyryl pyridine resin) = 1: 0.8: 0.1: 0.12, reaction temperature 76 ~ 78 ℃, reaction time 2 h. Under these conditions, the conversion of ortho-dinitrobenzene is above 99.5%, the purity of the refined dinitrobenzene is 99.8% after chromatographic analysis, and the yield of m-dinitrobenzene is about 99% , Polystyrene pyridine resin catalyst can be reused more than 7 times.