管道化氨解合成对乙酰氨基酚新工艺

    Synthesis of p-Acetylaminophenol with Pipeline Reactor

    • 摘要: 目的 采用管道化氨解工艺合成对乙酰氨基酚。方法 将对硝基苯酚钠的40%水溶液、液氨及催化剂氯化铵的1%水溶液以体积流量比9.25∶1∶1.85经预混合器后以0.15 mL·s-1的总流量流经外径6 mm,内径3 mm,总长50 m的管道反应器进行反应,反应温度220 ℃,反应压力6.0 MPa,反应停留时间40 min,脱除溶剂重结晶后得对氨基苯酚钠固体,再经酸化、乙酰化后得到对乙酰氨基酚。结果 得到的对乙酰氨基酚熔点167~169 ℃,三步总收率72.7%。结论 新工艺避免了还原步骤,减少了环境污染,安全性好,反应条件容易控制,并能得到良好的反应效果。

       

      Abstract: OBJECTIVE To prepare p-aminophenol sodium based on p-nitrophenol sodium by amination in pipeline reactor. METHODS The solution mixed with 40% p-nitrophenol sodium solution-ammonia-1% ammonium chloridesolution solution(9.25∶1∶1.85) passed through the pipeline reactor(6 mm×3 mm×50 m) at the speed of 0.15 mL·s-1 for 40 min with the temperature of 220 ℃, pressure of 6.0 MPa. Then p-nitrophenol sodium was prepared by the solution via desolventize, recrystallization, acidification and acetylation. RESULTS The melting point of p-aminophenol sodium achieved was 167-169 ℃, and the total yield was 72.7%. CONCLUSION The new process avoids the reduction step, reduces environmental pollution, and is more safety, controllable and the results are better than the normal process.

       

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