以流态化催化裂化废催化剂(SFCC)为载体、Ni为活性组分、柠檬酸(CA)为螯合剂,采用改进的溶液真空浸渍还原法制备了C_9石油树脂加氢催化剂Ni/CA-SFCC,采用低温物理吸附、FT-IR、XRD、SEM-EDS、ICP-AES、XPS、H_2-TPR等技术表征催化剂结构形貌等,并评价了其催化C_9石油树脂加氢活性。结果表明,SFCC载体的比表面积为75.42m~2/g,Ni/CA-SFCC的比表面积为83.92m~2/g;Ni/CA-SFCC中的Ni以较小的晶粒高度分散于载体表面;制备过程中,柠檬酸分解的炭优先填充SFCC载体的沟壑,使催化剂表面变得平整;Ni/CA-SFCC和未经柠檬酸改性的Ni/SFCC中的Ni质量分数分别为13.38%和10.96%,其还原温度分别为466℃和400℃。Ni/CA-SFCC催化C_9石油树脂的氢化度为91.2%,而Ni/SFCC催化所得的氢化度仅为55.0%。C_9石油树脂加氢改性产品的加纳(Gardner)色号从原料的11号降低到4号,硫质量分数从原料的0.016%降低到0.00024%。
Spent fluid catalytic cracking(SFCC)supported Ni catalyst Ni/CA-SFCC for C_9 petroleum resin hydrogenation was prepared by improved solution vacuum-impregnation reduction method with citric acid as chelating agent.The structure,morphology and catalytic activity of Ni/CA-SFCC were characterized by low temperature physical adsorption,FT-IR,XRD,SEM-EDS,ICP-AES,XPS,H_2-TPR.The results indicated that the surface area of the support SFCC was 75.42m~2/g,while that of Ni/CA-SFCC was 83.92 m~2/g.The active component of Ni was highly dispersed in the support surface with smaller grain.During the preparation the carbon from citric acid decomposition was preferentially filled on SFCC,which made the surface of Ni/CA-SFCC being smooth.The Ni loadings of Ni/CA-SFCC and unmodified Ni/SFCC were 13.38% and 10.96%(mass fraction)with the reduction peak temperatures of 466℃ and 400℃,respectively.The hydrogenation degree of C_9 petroleum resin catalyzed by Ni/CA-SFCC was 91.2%,while that by Ni/SFCC was only 55.0%.The Gardner color of the hydrogenated C_9 petroleum resin catalyzed by Ni/CA-SFCC was reduced to 4from 11 and the sulfur mass fraction was reduced to 0.00024%from0.016%,respectively.