为了探索乙二胺绿色合成的新工艺,采用自制的负载型双组分复合金属氧化物NiO/CuO/Al2O3为催化剂,对乙二醇进行催化氨化制备乙二胺,用气相色谱法对反应物进行分析检测,采用X射线衍射仪(XRD)、X射线光电子能谱分析仪(XPS)等技术手段对催化剂结构进行了表征. 通过考察催化剂组成、物料比、温度和时间等因素对反应的影响,确定了合成乙二胺的最佳工艺条件:催化剂活性组分n(Ni)∶n(Cu)=3∶1、催化剂加入量3%、氨醇质量比4∶1、反应温度180 ℃、反应压力0.6 MPa、反应时间4 h,乙二胺的选择性达56.7%,乙二醇转化率达68.6%. 与传统的二氯乙烷法相比较,本工艺更清洁友好.
To explore a new green process for synthesis of ethylenediamine, ethylenediamine was prepared by catalytic amination of ethylene glycol in the presence of supported two-component composite metal oxides NiO/CuO/Al2O3 catalyst.The structure of the catalyst was characterized by X-ray diffraction(XRD), X-ray photoelectron spectroscopy(XPS) methods.The reaction mixture was analyzed by gas chromatography(GC).The effects of catalyst composition, material ratio, temperature and reaction time on the reaction were investigated.The selectivity of ethylene diamine could reach 56.7% under the condition that n(Ni)∶n(Cu) ratio was 3∶1, catalyst loading was 3%, NH3/HOCH2CH2OH mass ratio was 4∶1, and the reation was performed at 180 ℃, 0.6 MPa and for 4 h.Compared with traditional dichloroethane method, this process is more clean and friendly.
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