摘要
采用浸渍、还原法制备了不同活性炭负载铂(Pt/AC)催化剂,考察了其催化3,4-二甲基硝基苯、3-戊酮和氢气一锅法制备N-(1-乙基丙基)-3,4-二甲基苯胺性能,并用氮气物理吸附、XRD对它们的结构进行了表征。结果表明,大孔径的活性炭负载0. 5%Pt对催化3,4-二甲基硝基苯、3-戊酮和氢气制备N-(1-乙基丙基)-3,4-二甲基苯胺具有优异性能。在3,4-二甲基硝基苯/催化剂质量比为100∶1、373 K、1. 0 MPa氢气、反应120 min的最佳反应条件下,N-(1-乙基丙基)-3,4-二甲基苯胺选择性达99. 1%。
Various activated carbons supported Pt catalysts were prepared by impregnation reduction method and investigated for synthesis of N-(1-ethylpropyl)-3,4-dimethylaniline from 3,4-dimethyl nitrobenzene,3-pentanone and hydrogen. Their structures were characterized by N_2 adsorption-desorption and Xray diffraction. It was found that the activated carbon with large pore size supported 0. 5% Pt exhibited better catalytic performance for synthesis of N-( 1-ethylpropyl)-3,4-dimethylaniline from 3,4-dimethyl nitrobenzene,3-pentanone and hydrogen. The yield of N-( 1-ethylpropyl)-3,4-dimethylaniline could reach99. 1% in 120 min under the optimal reaction conditions of 3,4-dimethyl nitrobenzene and catalyst at a mass ratio of 100∶ 1,373 K and 1. 0 MPa H_2.
引文
[1] Galli A,Souza D D,Machado S A S. Pendimethalin determination in natural water,baby food and river sediment samples using electroanalytical methods[J]. Microchemical Journal,2011,98(1):135-143.
[2]徐振元,严新焕,许丹倩,等.一步法合成N-(1-乙基丙基)-3,4-二甲基苯胺[J].高校化学工程学报,2002,16(1):75-78.
[3]张頔.除草剂二甲戊灵的合成研究进展[J].广州化工,2012,40(16):47-48.
[4]胡智燕,罗书平,许丹倩.酸性离子液体催化合成N-(1-乙基丙基)-3,4-二甲基苯胺[J].现代农药,2011,10(5):32-33.
[5]张钰,张启忠,张吉波,等.连续法合成N-(3-戊基)-3,4-二甲基苯胺工艺研究[J].吉林化工学院学报,2003,20(4):11-13.
[6]陈光文,党敏辉,陈毅征.一种N-(1-乙基丙基)-3,4-二甲基苯胺的合成方法:CN,104250215A[P]. 2013-06-27.
[7] Sun Y H,Zhang G J,Liu J W,et al. Effect of different activated carbon support on CH4-CO2reforming over Cobased catalysts[J]. International Journal of Hydrogen Energy,2018,43(3):1497-1507.
[8]王德举,郭友娣,王辉,等. Pd/C催化剂氢解α,α-二甲基苄醇制异丙苯[J].工业催化,2016,24(8):67-71.
[9]李国峰,陈梅,孔瑛,等.表面改性活性炭负载催化剂Pt-Sn/AC的制备及其催化性能[J].合成化学,2017,25(10):827-831.
[10]江罗,陈标华,张吉瑞,等.活性炭孔径分布对乙炔氢氯化低固汞催化剂性能的影响[J].化工学报,2018,69(1):423-428.
[11]朱虹,韩文锋,柴海芳,等. Ru基氨合成催化剂石墨化炭载体的制备[J].催化学报,2007,28(3):196-200.