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作 者:郝佳[1] 冷一欣[1] 韶晖[1] 王俊[1] 黄春香[2]
机构地区:[1]常州大学石油化工学院,江苏常州213164 [2]江苏省先进催化与绿色制造协同创新中心,常州大学,江苏常州213164
出 处:《精细化工》2016年第4期440-444,共5页Fine Chemicals
摘 要: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 different mass loading of phosphotung-based catalysts was synthesized by a impregnation method using silicone ball as the support.The supported catalysts were characterized by X-ray powder diffraction(XRD),Fourier transform infrared spectroscopy(FTIR) and UV-Vis diffuse reflection spectroscopy(UVVis DRS).The catalytic behaviors of these catalysts in the oxidative reaction of maleic acid to DL-tartaric acid were also investigated.The results indicated that tungsten could more effectively dispersed in the surface of the carrier after adding phosphate.The surface properties and oxidation catalyst performance were effectively adjusted by controlling mass loading of PW.The supported catalyst had better catalytic reactivity when molar ratio of W / P was 1 ∶ 2.2,mass loading of PW was 30%,activation temperature was 400 ℃ and activation time was 4 h.The conversion rate of maleic acid was 95.6% and yield of DL-tartaric acid was up to 91.7% when the mass fraction of catalyst in mixed solution was 2.5%,reaction temperature was 70 ℃,reaction time was 3 h,hydrolysis temperature was 105 ℃ and hydrolysis time was 3 h.
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