Chen Yanguang, Cong Shuli, Wang Qiqi, Han Hongjing, Lu Jia, Kang Yue, Kang Wei, Wang Haiying, Han Shuyu, Song Hua, Zhang Jiaojing
College of Chemistry & Chemical Engineering, Northeast Petroleum University, Daqing, 163318, China; Provincial Key Laboratory of Oil & Gas Chemical Technology, Northeast Petroleum University, Daqing, 163318, China.
College of Chemistry & Chemical Engineering, Northeast Petroleum University, Daqing, 163318, China; Provincial Key Laboratory of Oil & Gas Chemical Technology, Northeast Petroleum University, Daqing, 163318, China.
J Hazard Mater. 2018 May 5;349:18-26. doi: 10.1016/j.jhazmat.2018.01.004. Epub 2018 Jan 12.
A novel approach was proposed to prepare ZSM-5 zeolite via hydrothermal synthesis by using Al(OH), which was extracted from fly ash by a staged treatment, as an aluminum source. The synthesis parameters and crystal growth of ZSM-5 were optimized. The optimization of crystal growth for ZSM-5 was investigated under the effect of organic steric-hindrance agents. The crystal phase and morphology of the ZSM-5 were characterized by X-ray diffractometry and scanning electron microscopy, and the particle size distribution was measured by laser particle-size analyzer. The crystal growth of ZSM-5 under different hydrothermal conditions obeyed the "S" regulation. According to the analysis, the formation of ZSM-5 crystal occurred via four steps: (1) the formation of amorphous aluminosilicate by the condensation of silicate ions and aluminate ions; (2) the particle growth and aggregation of the amorphous aluminosilicate; (3) crystallization and crystal growth of ZSM-5; (4) Gentle growth after the zeolite crystal reaches a certain size. The addition of organic steric hindrance agents resulted in a decrease in grain size and crystal-particle formation with a narrow size distribution. Single-grain dispersion resulted and the micropore volume, mesopore volume, and specific surface areas were improved by the presence of organic steric agents.
提出了一种新颖的方法,通过水热合成制备ZSM-5沸石,使用经分步处理从粉煤灰中提取的Al(OH)₃作为铝源。对ZSM-5的合成参数和晶体生长进行了优化。研究了在有机空间位阻剂作用下ZSM-5晶体生长的优化情况。通过X射线衍射仪和扫描电子显微镜对ZSM-5的晶相和形貌进行了表征,并用激光粒度分析仪测量了粒径分布。不同水热条件下ZSM-5的晶体生长遵循“S”形规律。分析表明,ZSM-5晶体的形成经历四个步骤:(1) 硅酸根离子和铝酸根离子缩合形成无定形硅铝酸盐;(2) 无定形硅铝酸盐的颗粒生长和聚集;(3) ZSM-5的结晶和晶体生长;(4) 沸石晶体达到一定尺寸后的缓慢生长。有机空间位阻剂的加入导致晶粒尺寸减小,形成晶体颗粒,且粒径分布变窄。实现了单颗粒分散,有机空间位阻剂的存在改善了微孔体积、中孔体积和比表面积。