微米蛋壳型Ni/SFC3R催化C5石油树脂 加氢反应研究

Study on Micro-size Eggshell Type Ni/SFC3R Catalyst Catalytic C5 Petroleum Resin Hydrogenation

摘要:

以废FCC触媒（SFC3R）为载体，采用浸渍法制备了微米级蛋壳型Ni/SFC3R催化剂，利用 FIB（聚焦离子束）-EDX、XRD、H2-TPR和TEM技术对催化剂结构、表面物相和还原性进行了表征；考察了反应温度、压力和时间对C5石油树脂加氢反应的影响，并应用Gardner色号、软化点、GPC、FT-IR和1H-NMR等方法对加氢改性C5石油树脂进行了性能和结构分析。结果表明，SFC3R为分子筛结构，Ni活性组分主要分布在载体外层形成蛋壳分布，NiO的平均粒径为21.5nm，具有良好的分散性；C5石油树脂加氢的最优反应条件为：温度280℃，压力8.0 MPa，时间5h，所得的加氢改性C5石油树脂Gardner色号<1，颜色为水白色，硫含量<10mg/kg，溴值为0.45 gBr/100g，C5石油树脂中的不饱和键加氢基本达到饱和。

Abstract:

A micro-size eggshell Ni-based catalyst supported in fluid catalytic cracking catalyst residue (SFC3R) was synthesized by impregnation. The structure, morphology and reducibility of the catalyst were characterized by FIB-EDX、XRD、H2-TPR and TEM. The eggshell Ni/SFC3R catalyst was used for C5 petroleum resin hydrogenation，and the effects of temperature，pressure and reaction time were investigated. The properties and structure of hydrogenated C5 petroleum resin were analyzed by the method of Gardner color number， softening point， GPC， FT-IR and 1H-NMR. Results show that SFC3R contains zeolite structure and the Ni active component is mainly distributed in the outer layer of the SFC3R to form the eggshell distribution. The crystallite size of NiO of eggshell Ni/SFC3R catalyst is 21.5 nm, which exhibit good dispersion. The optimum conditions of C5 petroleum resin hydrogenation were found as temperature 280 ℃，H2 pressure 8.0 MPa and reaction time 4 h. The Gardner color of hydrogenated C5 petroleum resin is below 1# and the color is water white. The sulfur content and bromine number of hydrogenated C5 petroleum resin is <10mg/kg and 0.45 gBr/100g， respectively. And the unsaturated bond of C5 petroleum resin reaches saturation basically.