化工进展 ›› 2012, Vol. 31 ›› Issue (01 ): 156-162.

• 材料科学与技术 • 上一篇    下一篇

一步法合成载铁有序介孔碳材料的形成机理

凌晓凤,顾  娟,李健生,孙秀云,韩卫清,沈锦优,王连军   

  1. (南京理工大学环境与生物工程学院,江苏 南京 210094
  • 出版日期:2012-01-05 发布日期:2012-01-25

Mechanism of the synthesis of ordered Fe-containing mesoporous carbon composite materials in one-pot

LING Xiaofeng,GU Juan,LI Jiansheng,SUN Xiuyun,HAN Weiqing, SHEN Jinyou,WANG Lianjun   

  1. (School of Environmental & Biological Engineering,Nanjing University of Science and Technology,Nanjing 210094,Jiangsu,China)
  • Online:2012-01-05 Published:2012-01-25

摘要: 采用软模板路线以三嵌段共聚物F127为模板剂,间苯二酚-甲醛缩聚所形成酚醛树脂(RF)为碳源,与酚羟基有络合作用的无机铁盐为金属前体,在无外加酸碱催化剂的条件下,利用铁盐的水解反应形成酚醛缩聚所需酸性环境,多组分共组装一步合成了载铁有序介孔碳材料(Fe/OMC)。对Fe/OMC合成各阶段过程进行了分析,利用X射线衍射、透射电子显微镜等手段对材料进行表征,比较了不同老化时间、硝酸铁投加量及酚醛比例等合成条件对材料结构的影响规律。结果表明,在较长的老化时间(≥60 h)、适宜的n(Fe)/n(R)比(0.05~0.2)和n(R)/n(F)比[(1/1.5)~(1/2)]条件下,均可形成有序的介孔结构。在此基础上,提出了载铁有序介孔碳材料的形成机理。

关键词: 一步法, 软模板, 铁, 有序介孔碳, 形成机理

Abstract: Ordered Fe-containing mesoporous carbon composite materials(Fe/OMC)have been synthesized via soft-templating routes by using triblock copolymer F127 as a template agent,resorcinol (R)-formaldehyde(F)as a carbon precursor,inorganic iron salts having complex reaction with phenols as a metal precursor in one-pot. The main strategy of this approach was to utilize the acidity self-generated from the hydrolysis of inorganic salts in the aqueous solutions as the catalyst for RF polymerization,where no addition of mineral acids was necessary. The resultant Fe/OMC materials were characterized by X-ray diffraction,Transmission electron microscopy. The influences of the aging time,the dosage of iron nitrate and the molar ratio of R/F on the structure of the obtained materials were investigated. Results show that the ordered mesoporous structure can be obtained under the synthetic condition of the aging time≥60 h,n(Fe)/n(R)=0.05—0.2,n(R)/n(F)=1/1.5—1/2.0. Moreover,a possible mechanism of the synthesis of Fe/OMC was proposed.

Key words: one-pot, soft-templating, iron, ordered mesoporous carbon, mechanism