常压催化胺化制取聚醚胺反应的研究

Research on synthesis of polyether amine via catalytic amination under atmospheric pressure

为克服常规制备聚醚胺需要高温、高压等苛刻反应条件的不足,制备了一种Pd-Mg-Ba/r-Al_2O_3型催化剂,探索了聚醚在常压下催化胺化的可行性。主要考察了催化剂活性组分质量分数、反应温度、氢气用量、氨气用量、进料速率对胺化反应的影响。确立了反应合适条件为:催化剂组成Pd(0.5%)-Mg(2%)-Ba(2%)/r-Al_2O_3,反应温度为200℃,氨气、氢气用量为n(聚醚)∶n(NH3)∶n(H2)=1∶8∶8,反应空速为0.3 h-1。同时,利用核磁共振波谱及化学分析对产品结构及性质进行了分析。结果表明,该常压工艺为后续工业常压生产提供重要依据。

In order to avoid the rigorous reaction conditions in the synthesis of polyether amine such as high temperature and high pressure,a kind of Pd-Mg-Ba/r-Al2O3 catalyst is prepared and then used to seek for the feasibility of conducting the reaction under atmospheric pressure. The influences of the mass concentration of catalyst active components,reaction temperature,H2 dosage,NH3 dosage and feed rate on the amination reaction are studied. The suitable reaction conditions are determined as follows： the composition of catalyst is Pd（ 0. 5%）-Mg（ 2%）-Ba（ 2%）/rAl2O3,reaction temperature is at 200℃,n（ polyether） ∶ n（ NH3） ∶ n（ H2） = 1∶ 8∶ 8,and WHSV is 0. 3 h-1. The gained products are characterized by NMR and chemical analysis. This research can provide helpful support for the application of atmospheric pressure process in industrial production.