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含钴介孔分子筛的微波合成及其稳定性
作者:姜廷顺 唐雅静 张丽 赵谦 殷恒波  
单位:江苏大学化学化工学院 江苏大学化学化工学院 江苏农林职业技术学院 江苏大学化学化工学院 江苏大学化学化工学院 江苏 镇江212013 江苏 镇江212013 江苏 句容212400 江苏 镇江212013 江苏 镇江212013 
关键词:含钴介孔分子筛  微波合成  表征  稳定性 
分类号:O643.3
出版年,卷(期):页码:2008,36(S1):6-11
DOI:
摘要:
以硅酸钠和氯化钴为原料、十六烷基三甲基溴化铵为模板剂,采用微波辐照法合成4种不同钴含量的含钴介孔分子筛(cobalt-containing mesoporous molecular sieves,Co-MCM-41)。用X射线粉末衍射仪、Fourier变换红外分析、程序升温还原分析、透射电子显微镜、比表面积和孔径测定仪等表征样品的物理化学性能,并研究了合成的Co-MCM-41的稳定性。结果表明:在摩尔比n(SiO_2):n(CoO)=1.0:0.05~1.0:0.2的范围内都可以合成出有序性好的Co-MCM-41。随着Co添加量的增加,Co-MCM-41的比表面积减小,但孔径略有增加,所合成的Co-MCM-41经750℃焙烧3h后仍然具有介孔结构;但是,850℃焙烧3h后,其介孔结构被破坏:100℃水热处理5d后,Co-MCM-41仍然具有介孔结构,样品的比表面积降低很多,并且呈现出虫蛀状介孔结构。
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Cobalt-containing mesoporous molecular sieves (Co-MCM-41) with different cobalt contents were synthesized by the microwave irradiation method and using inorganic salt sodium silicate and cobalt chloride as raw materials,and cetyl trimethyl ammonium bromide as template agent.The physicochemical properties of the as synthesized Co-MCM-41 were characterized by various techniques such as X-ray diffraction,Fourier transform infrared spectroscopy,temperature programmed reduction, transmission electron microscope,and N_2 adsorptiun-desorption technique,and the stability of the synthesized Co-MCM-41 was also investigated.The results show that well-ordered Co-MCM-41 can be synthesized when the molar ratio n(SiO_2):n(CoO) in the starting material is between 1.0:0.05 and 1.0:0.2.The specific surface area of the synthesized mesoporous molecular sieve decreases with the increasing of the amount of cobalt added,and the pore size of synthesized samples slightly increases.The synthesized Co-MCM-41 still has a mesostructure after calcination at 750℃for 3 h,but the mesostructure is damaged after calcination at 850℃for 3 h.On the other hand,the mesostructure of the synthesized sample is still retained after hydrothermal treatment at 100℃for 5 d,but the specific surface area greatly decreases,and the synthesized sample exhibits a worm-like mesoporous structure.
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基金项目:
江苏省高校自然科学基金(04KJD130040);; 江苏大学高级人才基金(JDG2006074)资助项目。
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