(江苏大学 化学化工学院, 镇江 212013)
摘 要: 以十六烷基三甲基溴化铵为模板剂, 以硅酸钠、 氯化镍、 氯化钴等无机盐为原料, 水热法合成出含Ni介孔分子筛和含Co介孔分子筛。 采用XRD、 FT-IR、 TPR、 TEM和比表面积孔径测定等方法对样品进行表征。 结果表明: 合成了长程有序性好的含Ni和含Co介孔分子筛; 含Ni介孔分子筛的比表面积为753.3 m2/g, 平均孔径为3.23 nm, 750 ℃焙烧3 h, 100 ℃水热处理5 d介孔结构仍然存在; 含Co介孔分子筛的比表面积为744.1 m2/g, 平均孔径为4.44 nm, 650 ℃焙烧后转变为虫蛀状介孔结构, 750 ℃焙烧3 h后介孔有序性变得很差, 100 ℃水热处理5 d后转变为虫蛀状结构。
关键字: 含Ni介孔分子筛; 含Co介孔分子筛; 合成; 表征
(School of Chemistry and Chemical Engineering, Jiangsu University,
Zhenjiang 212013, China)
Abstract: Ni(or Co)-mesoporous molecular sieve was hydrothermally synthesized from inorganic salts as sodium silicate, nickel chloride and cobalt chloride as starting material by using cetyltrimeethyl ammonium bromide (CTAB) as the template. The samples were characterized by XRD, TEM, TPR, FT-IR and N2 physical adsorption. The results show that the long-range and well-ordered Ni(or Co)-mesoporous molecular sieve was synthesized. The as prepared Ni-mesoporous molecular sieve has a specific surface area of 753.3 m2/g and an average pore size of 3.23 nm. The pore structure of the as prepared Ni-mesoporous molecular sieve remains after calcination at 750 ℃ for 3 h or hydrothermal treatment at 100 ℃ for 5 d. The as prepared Co-mesoporous molecular sieve has a specific surface area of 744.1 m2/g and an average pore size of 4.44 nm. The as prepared Co-mesoporous molecular sieve is transformed into wormhole-like mesoporous structure after calcination at 650 ℃ or hydrothermal treatment at 100 ℃ for 5 d. The mesoporous structure of the as prepared Co-mesoporous molecular sieve is partially destroyed after calcination at 750 ℃ for 3 h.
Key words: Ni-mesoporous molecular sieve; Co-mesoporous molecular sieve; synthesis; characterization