石油化工2013,Vol.42Issue(2):198-203,6.
S2O82-/ZrO2-SiO2固体超强酸的合成及其催化合成硬脂酸正丁酯
Preparation of S2O82-/ZrO2-SiO2 Solid Super Acid Catalyst and Its Activity in Synthesis of Butyl Stearate
摘要
Abstract
Solid super acid catalysts S2O82-/ZrO2-SiO2 were prepared by co-precipitation from zirconium(Ⅳ) nitrate and sodium silicate and then impregnation with ammonium persulfate solution,and characterized by means of XRD,FTIR and SEM.The catalytic activity of the catalysts in the esterification of stearic acid and butanol to butyl stearate was investigated.The effects of the catalyst preparation conditions and the esterification reaction conditions on the catalyst activity were studied.The results showed that adding SiO2 into ZrO2 retarded the crystallization and phase transformation of ZrO2.When the calcination temperature was at 550 ℃,tetragonal ZrO2 and monoclinic ZrO2 coexisted in the catalysts,and there were some needle-like crystals coated on the surface of the catalysts.Under the catalyst preparation conditions of n(Zr(NO3)4) ∶ n(Na2SiO3) 2.0 ∶ 1.5,(NH4)2S2O8 impregnating solution concentration 0.5 mol/L,impregnating time 2 h,calcination temperature 450 ℃ and calcination time 3 h,the catalytic activity of the S2O82-/ZrO2-SiO2 catalyst was high,and estirification rate was up to 98.3% under the optimal esterification conditions of stearic acid dosage 5.7 g,n(stearic acid) ∶ n(butanol) 1 ∶ 3,catalyst dosage 0.2 g,reaction temperature 120 ℃ and reaction time 2.5 h.关键词
固体超强酸催化剂/氧化锆/氧化硅/硬脂酸/正丁醇/硬脂酸正丁酯Key words
solid super acid catalyst/ zirconia/ silica/ stearic acid/ butanol/ butyl stearate分类
化学化工引用本文复制引用
曾飞虎,林玉香,陈锦辉,林继辉..S2O82-/ZrO2-SiO2固体超强酸的合成及其催化合成硬脂酸正丁酯[J].石油化工,2013,42(2):198-203,6.基金项目
福建省教育厅B类项目(JB11271) (JB11271)
大学生创新性实验计划项目(201212992003). (201212992003)