摘要
采用溶胶-凝胶法制备Co/SiO_2催化剂,用于异佛尔酮腈(IPN)氢氨化"一锅法"催化反应制备异佛尔酮二胺(IPDA)。采用H_2-TPR,XRD,TEM,BET,XPS等方法对催化剂试样进行了表征。表征结果显示,焙烧好的催化剂前体于550℃下H_2还原,活性组分钴主要是以Co(0)的形式存在,呈现3~5 nm与160 nm两种粒径分布,比表面积约为260~270 m^2/g,平均孔径为12~13 nm。实验结果表明,当体系pH=5.0、Co负载量为30%(w)时制备的催化剂性能最佳;在优化的催化反应条件下,IPN转化率达98.4%,IPDA收率达73.5%;催化剂重复使用8次后仍能保持良好的催化性能,催化效果优于商用催化剂Raney Co。
A series of Co/SiO2 catalysts were prepared by sol-gel method and were applied to the ＂one-pot＂ synthesis of isophorone diamine（1PDA） through the hydroamination of isophorone nitrile（IPN）. The catalysts were characterized by means of H2-TPR, XRD, TEM, BET and XPS. The results indicated that, when the calcined catalyst precursors were reduced with H2 at 550 ℃, the active component cobalt existed in the form of Co（0）, with the BET specific surface area of 260-270 m2/g, average pore diameter of 12-13 nm and two different particle size distributions of 3-5 nm and 160 nm separately. It was showed that the Co/SiO2 catalyst with the cobalt loading of 30%（w） prepared at pH 5.0 exhibited the best catalytic performances, over which the IPN conversion and the IPDA yield reached 98.6% and 73.5%, respectively. The catalyst could be reused 8 times without obvious lose of the activity, which was superior to a commercial Raney Co catalyst.
出处
《石油化工》
CAS
CSCD
北大核心
2016年第10期1186-1191,共6页
Petrochemical Technology
基金
国家自然科学基金项目(21276230
21476211)
浙江省自然科学基金项目(LY14B060003
LY16B060004)
