催化加氢制备对氨基苯酚提高纯度的研究
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摘要
采用高压釜式反应器,以乙醇-水为溶剂,在压力0.2～2.5MPa、反应温度50～120℃、氢气气氛下,探究了Pd/C催化剂对对硝基苯酚催化加氢制备对氨基苯酚的产品纯度影响。结果表明:Pd/C催化剂具有良好的加氢制备对氨基苯酚反应性能,产品纯度随Pd负载量的增加呈现先增加后减小的趋势,Pd负载量为3%时产品纯度可达98.76%;实验探究出对硝基苯酚催化加氢制备对氨基苯酚最佳反应条件:当乙醇和去离子水之比为5:1,催化剂Pd负载量为3%,氢气压力为0.5MPa,反应温度为85℃时,催化剂负荷量为1/60～1/40,对氨基苯酚收率达98.5%,纯度达99%以上。
The purity of p-aminophenol by catalytic hydrogenation from p-nitrophenol in ethanol-waterusing Pd/C catalystwas investigated under 0.2～2.5 MPa, 50～120℃, hydrogen-containing. The results showed that Pd/C catalyst has good hydrogenation performance. The purity of product increases first and then decreases with the increase of Pd load. When Pd load is 3%, the product purity can reach 98.76%. Experiments to explore optimum reaction conditions was listed: the ratio of ethanol and deionized water(5:1),Pd catalyst load(3%), 0.5 MPa, 85℃. The yield of p-aminophenol was 98.5%, and the purity of was more than 99%.
The purity of p-aminophenol by catalytic hydrogenation from p-nitrophenol in ethanol-waterusing Pd/C catalystwas investigated under 0.2～2.5 MPa, 50～120℃, hydrogen-containing. The results showed that Pd/C catalyst has good hydrogenation performance. The purity of product increases first and then decreases with the increase of Pd load. When Pd load is 3%, the product purity can reach 98.76%. Experiments to explore optimum reaction conditions was listed: the ratio of ethanol and deionized water(5:1),Pd catalyst load(3%), 0.5 MPa, 85℃. The yield of p-aminophenol was 98.5%, and the purity of was more than 99%.
引文
[1]董娟,马振叶,陈日志,等. Pd/Al2O3催化剂的制备及其在对氨基苯酚合成中的应用[J].工业催化,2007, 15(6):62-65.
[2] Manisha JV, Shrikant M K, Raghunath VC. Synthesis of p-Aminophenol by Catalytic Hydrogenation of p-Nitrophenol[J].Organic Process Research&Development, 2003, 7:202-208.
[3]高洪,袁华,喻宗沅.对氨基苯酚的合成及应用评述[J].湖北化工,2000, 17(2):1-2.
[4] Du Y, Chen H L, Chen R Z, et al. Synthesis of p-aminophenol from p-nitrophenolover nano-sized nickel catalysts[J].Applied Catalysis A:General, 2004, 277:259-264.
[5]温卓,孙德福,吴涛.硝基苯加氢制对氨基苯酚工艺过程研究[J].内蒙古石油化工,2009, 4:13-15.
[6]WangAL,YinHB,LuHH,etal.Catalyticactivity ofnickelnanoparticlesinhydrogenationofp-nitrophenolto p-aminophenol[J]. Catalysis Communications, 2009, 10:2060-2064.
[7] Ma Z Y, Zhang L X, Chen R Z, et al. Preparation of Pd–B/Ti O2 amorphous alloy catalysts and theirperformance on liquidphase hydrogenation of p-nitrophenol[J]. Chemical Engineering Journal, 2008, 138:517-522.
[8] Lee L T, Chen M H, Yao C N. Process for manufacturingpaminophenol:US, 4885389[P]. 1989-12-05.
[9]尹春凯,王幸宜,卢冠忠. Pt/C催化剂催化硝基苯加氢制对氨基苯酚工艺过程剖析[J].工业催化, 2000, 8(5):13-17.
[10]肖传发.对硝基苯酚催化加氢制备对氨基苯酚的工艺研究[J].应用化工,2012, 41(3):488-490.
[2] Manisha JV, Shrikant M K, Raghunath VC. Synthesis of p-Aminophenol by Catalytic Hydrogenation of p-Nitrophenol[J].Organic Process Research&Development, 2003, 7:202-208.
[3]高洪,袁华,喻宗沅.对氨基苯酚的合成及应用评述[J].湖北化工,2000, 17(2):1-2.
[4] Du Y, Chen H L, Chen R Z, et al. Synthesis of p-aminophenol from p-nitrophenolover nano-sized nickel catalysts[J].Applied Catalysis A:General, 2004, 277:259-264.
[5]温卓,孙德福,吴涛.硝基苯加氢制对氨基苯酚工艺过程研究[J].内蒙古石油化工,2009, 4:13-15.
[6]WangAL,YinHB,LuHH,etal.Catalyticactivity ofnickelnanoparticlesinhydrogenationofp-nitrophenolto p-aminophenol[J]. Catalysis Communications, 2009, 10:2060-2064.
[7] Ma Z Y, Zhang L X, Chen R Z, et al. Preparation of Pd–B/Ti O2 amorphous alloy catalysts and theirperformance on liquidphase hydrogenation of p-nitrophenol[J]. Chemical Engineering Journal, 2008, 138:517-522.
[8] Lee L T, Chen M H, Yao C N. Process for manufacturingpaminophenol:US, 4885389[P]. 1989-12-05.
[9]尹春凯,王幸宜,卢冠忠. Pt/C催化剂催化硝基苯加氢制对氨基苯酚工艺过程剖析[J].工业催化, 2000, 8(5):13-17.
[10]肖传发.对硝基苯酚催化加氢制备对氨基苯酚的工艺研究[J].应用化工,2012, 41(3):488-490.