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以硅球为载体,用浸渍法制备了一系列不同负载量的磷钨负载型催化剂。通过X射线衍射(XRD)、傅里叶变换红外(FTIR)和紫外-可见漫反射光谱(UVVis DRS)对合成催化剂进行表征,并考察了催化剂在顺丁烯二酸氧化制备DL-酒石酸反应中的催化性能。结果表明,加入磷酸后,磷钨能更有效的分散在载体表面。通过控制PW负载量,可有效调整催化剂的表面性质及氧化反应催化性能。当n(W)∶n(P)=1∶2.2,负载量w(PW)=30%,焙烧温度400℃,焙烧时间4 h,催化活性较好。在反应温度70℃,反应时间3 h,催化剂在反应体系中的质量分数为2.5%,水解温度105℃,水解时间3 h,顺丁烯二酸的转化率为95.6%,DL-酒石酸的收率达91.7%。
A series of phosphorus-tungsten supported catalysts with different loadings were prepared by impregnation method using silica balls as support. The synthesized catalysts were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) and ultraviolet-visible diffuse reflectance spectroscopy (UVVis DRS). The effects of catalyst on the DL-tartaric acid oxidation by maleic acid oxidation The catalytic performance. The results show that, after the addition of phosphoric acid, phosphorus and tungsten can be more effectively dispersed in the carrier surface. By controlling the PW load, the surface properties of the catalyst and the catalytic performance of the oxidation reaction can be effectively adjusted. When n (W): n (P) = 1: 2.2, the loading w (PW) = 30%, the calcination temperature 400 ℃, the calcination time 4 h, the catalytic activity is better. The reaction temperature was 70 ℃, the reaction time was 3 h, the mass fraction of catalyst in the reaction system was 2.5%, the hydrolysis temperature was 105 ℃, the hydrolysis time was 3 h, the conversion of maleic acid was 95.6%, the yield of DL-tartaric acid Rate of 91.7%.