对硝基苯胺水相加氢合成对苯二胺
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Synthesis of p-Phenylenediamine by Hydrogenation of p-Nitroaniline in Water
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    摘要:

    以对硝基苯胺为原料,水为溶剂,考察了水相中负载型镍催化剂催化对硝基苯胺加氢还原的反应性能,并开展了中试实验。考察了反应温度、压力、保温时间、对硝基苯胺浓度、废水套用等因素对催化加氢反应性能的影响。实验结果表明,产品对苯二胺质量分数较高,催化剂和水可循环使用。较佳的工艺条件为:温度110 ℃,保温时间2~3 h,压力2.0 MPa,搅拌转速800 r/min,起始催化剂用量10%(以对硝基苯胺的质量为基准,下同),催化剂损耗0.2%(以起始添加剂催化剂的质量为基准)。此工艺条件下,对硝基苯胺转化率100%,对苯二胺产率99.5%以上。废水套用后排放废水量很少,且对催化剂催化活性、产品质量等没有影响。

    Abstract:

    The reactive behavior on hydrogenation of p-nitroaniline in water catalyzed by supported nickel catalyst was studied. The laboratory test and pilot-plant test were conducted. The effects of reaction temperature, pressure, holding time, p-nitroaniline mass concentration and wastewater recycle on the hydrogenation reaction were investigated. The results showed that the product p-phenylenediamine has high mass fraction, and catalyst and water can be recycled. The optimal reaction parameters are that temperature 110℃, reaction time 2~3 h, pressure 2.0 MPa, stirring speed 800 r/min, dosage of initial catalyst 10% (based on the mass of p-nitroaniline, similarly hereinafter), catalyst loss 0.2% (based on the additive mass of initial catalyst). Under these optimal reaction conditions, the conversion of p-nitroaniline was 100%, and the yield of p-phenylenediamine was over 99.5%. The amount of wastewater discharged after wastewater recycle was small and had no effect on catalytic activity and product quality.

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李建昌.对硝基苯胺水相加氢合成对苯二胺[J].精细化工,2019,36(7):

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历史
  • 收稿日期:2018-12-20
  • 最后修改日期:2019-03-12
  • 录用日期:2019-03-12
  • 在线发布日期: 2019-05-30
  • 出版日期: