季铵盐型阴离子交换树脂上邻硝基氯苯乙氧基化生成邻硝基乙氧基苯的清洁工艺

Clean process for the ethoxylation of o-nitrochlorobenzene to o-nitroethoxybenzene using quaternary ammonium anion exchange resin

通过向含有季铵盐型阴离子交换树脂的邻硝基氯苯、乙醇混合物中滴加NaOH溶液的方法得到了标题化合物。单纯形搜索法得到的优化实验条件:反应温度60℃、NaOH浓度50%、NaOH滴加时间2h、搅拌速度800r/min,邻硝基氯苯的转化率为80.3%。该工艺的特点是邻硝基乙氧基苯的选择性接近100%,反应产物容易分离,季铵盐型阴离子交换树脂可回收利用8次。

In this paper, o-nitroethoxybenzene was prepared by using o-nitrochlorobenzene,sodium hydroxide and ethanol as raw materials in the presence of quaternary ammonium anion resin. The results by simple search method experiment indicated that the conversion of o-nitrochlorobenzene was 80.3% and the selectivity of o-nitroethoxybenzene was nearly 100% under the optimized experiment conditions: reaction temperature T = 60℃, NaOH concentration w = 50% , NaOH aq drop-addition time t=2h, stirring speed p=800r/min. The virtues of this process were that recycling use of quaternary ammonium anion resin was easy and could be used 8 times in intermittent operation, another advantage was that the reaction product could be separated easily from the mixture.