不同烧制气氛对丙烯酸催化剂性质影响的研究  

Study on effect of different calcination atmospheres on properties of acrylic acid catalysts

作　　者：王静 苏晋 张利杰 周鹏 孙彦民 李佳 WANG Jing;SU Jin;ZHANG Lijie;ZHOU Peng;SUN Yanmin;LI Jia(CNOOC Tianjin Chemical Research and Design Insititute Co.,Ltd.,Tianjin 300131,China)

机构地区：[1]中海油天津化工研究设计院有限公司,天津300131

出　　处：《无机盐工业》2024年第9期164-170,共7页Inorganic Chemicals Industry

摘　　要：采用溶液法制备了含Mo-V的复合氧化物前驱体,经喷雾干燥后的前驱体在不同气氛(5%H_(2)+95%N_(2)、N_(2)、5%O_(2)+95%N_(2)、空气和O_(2))中焙烧处理,获得Mo-V-W-Sb系列复合金属氧化物催化剂,并将其应用于丙烯醛气相氧化制丙烯酸反应。采用电感耦合等离子体发射光谱仪(ICP-OES)、X射线荧光光谱仪(XRF)、X射线衍射仪(XRD)、氮气物理吸附仪、透射电子显微镜(TEM)、化学吸附仪和电位滴定仪对催化剂进行了表征。实验结果表明,不同的焙烧气氛对Mo-V-W-Sb系列催化剂的晶相结构、物化性质及催化性能均产生了明显的影响。前驱体在弱氧化性气氛(5%O_(2)+95%N_(2))中烧制时,有利于制备出含有较纯Mo_(3)VO_(11+x)活性相、相对较大比表面积(6.8 m^(2)/g)、适中结晶度和还原温度(约415℃),以及最适宜n(V^(5+))[/n(V^(3+))+n(V^(4+))+n(V^(5+))]为0.019的催化剂,且该催化剂表现出最佳的催化性能,高达99.5%的丙烯醛转化率和88.7%的丙烯酸收率。The composite oxide precursors containing Mo-V were prepared by solution method,and the precursors after spray drying were calcined under different atmospheres(5%H_(2)+95%N_(2),N_(2),5%O_(2)+95%N_(2),air and O_(2))to obtain Mo-V-W-Sb series composite metal oxide catalysts.And they were applied to the vapor phase oxidation of acrolein to acrylic acid.The catalysts were characterized by inductively coupled plasma⁃optical emission spectrometer(ICP-OES),X-ray fluorescence spectrometer(XRF),X-ray diffractometer(XRD),nitrogen physical adsorption analyzer,transmission electron microscope(TEM),temperature program reduction(H2-TPR)and potentiometric titrator.The experimental results indicated that the calcination atmosphere had a significant impact on the crystal structure,physicochemical properties,and catalytic perfor⁃mance of the Mo-V-W-Sb series catalysts.When the precursor was thermotreated in a weakly oxidizing atmosphere(5%O_(2)+95%N_(2)),it was beneficial to prepare a catalyst with pure Mo_(3)VO_(11+x)active phase,relatively larger specific surface area(6.8 m^(2)/g),moderate crystallinity and reduction temperature(about 415℃),and the most suitable n(V^(5+))[/n(V^(3+))+n(V^(4+))+n(V^(5+))]=0.019.Furthermore,this catalyst exhibited the best reaction performance in the oxidation of acrolein to acrylic acid,with a conversion rate of 99.5%acrolein and a yield of 88.7%acrylic acid.

关 键 词：复合氧化物 气相氧化 丙烯酸 催化性能 

分 类 号：TQ136.12[化学工程—无机化工]