摘要
为C9石油树脂加氢改性和催化裂化(FCC)废触媒再生利用,以FCC废触媒为载体,有机溶剂为助剂,采用负压浸渍法制备负载型非贵金属镍催化剂,并对其催化C9石油树脂加氢性能研究。通过电感耦合等离子光谱分析(ICP-AES)、比表面积测定(BET)、扫描电镜分析(SEM)、X射线衍射分析(XRD)、红外光谱分析(FT-IR)等技术对催化剂结构形貌和催化活性进行表征;以CQF-2型高压釜为反应器,在温度250℃、压力8.0 MPa和搅拌转速400 r/min条件下,考察催化剂对C9石油树脂加氢反应活性及选择性的影响,应用BR-1溴值溴指数测定仪和Gandner色度仪对反应产物进行分析鉴定。结果表明,FCC新触媒镍含量为0.003 8 wt%;FCC废触媒镍含量为0.84 wt%,比表面积为91.75 m2/g,孔容为0.025 cm3/g,孔径为7.81 nm;SEM分析表明FCC废触媒孔道被堵塞;XRD图谱表明FCC废触媒由Y型分子筛、Al2O3和ZSM-5构成,FCC废触媒负载镍主要以晶粒形态存在;FT-IR分析表明FCC废触媒中镍没有以共价键形式存在;在镍负载量为30 wt%时,C9石油树脂加氢改性产品Gandner色号为6、氢化率为82.01%。
In order to investigate the hydrogenation modification of C9 petroleum resin and the recy-cling of spent fluid catalytic cracking ( FCC) catalyst, Ni catalyst was prepared by the vacuum-im-pregnation reduction method using Ni as active metal,pretreated spent FCC catalyst as carrier,and organic solvent as auxiliary. The catalytic performance of the Ni catalyst for C9 petroleum resin hy-drogenation was studied. The structure, morphology and catalytic activity of the catalysts were char-acterized by FT-IR, XRD, SEM, ICP-AES, and BET methods. The effects of catalyst on the reac-tivity and selectivity of C9 petroleum resin hydrogenation were investigated under the conditions of temperature of 250 ℃, hydrogen pressure of 8. 0 MPa, and stirring speed of 400 r/min in a CQF-2 stainless steel autoclave. The products of C9 petroleum resin hydrogenation were analyzed by bro-mine index analyzer and Gandner colorimeter. The results showed that the Ni content of FCC catalyst was 0. 0038 wt%, while that of spent FCC catalyst was 0. 84 wt%. The BET surface area, average pore volume and average pore size of spent FCC catalyst were 91. 75 m2/g, 0. 025 cm3/g and 7. 81 nm, respectively. The analysis of SEM indicated that the pores of spent FCC catalyst were blocked. XRD results showed that the spent FCC catalyst was composed by Y molecular sieve, Al2 O3 and ZSM-5, and the Ni existed on the catalyst was highly dispersed in the support surface and existed in the form of crystalline grain. In addition, the results of FT-IR showed that there was no covalent bond of Ni in the spent FCC catalyst. The Gardner color of the hydrogenated C9 petroleum resin reduced to 6 and the hydrogenation rate was 82. 01% when the Ni content increased to 30 wt%.
出处
《广西大学学报(自然科学版)》
CAS
北大核心
2016年第5期1636-1644,共9页
Journal of Guangxi University(Natural Science Edition)
基金
国家自然科学基金资助项目(51563001
21466002)
广西石化资源加工及过程强化技术重点实验室主任课题基金(2015Z011)