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硅酸盐通报 ›› 2018, Vol. 37 ›› Issue (4): 1188-1194.

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煤系高岭土插层-水热法制备亚微米级13 X分子筛

徐嘉晨;吴红丹;周志辉;尧鹏魁;张青鹏   

  1. 武汉科技大学冶金矿产资源高效利用与造块湖北省重点实验室,武汉,430081
  • 出版日期:2018-04-15 发布日期:2021-01-18

Intercalation-Hydrothermal Preparation of Submicron 13X Zeolite with Coal-Measure Kaolin

XU Jia-chen;WU Hong-dan;ZHOU Zhi-hui;YAO Peng-kui;ZHANG Qing-peng   

  • Online:2018-04-15 Published:2021-01-18

摘要: 以煤系高岭土为原料,制备了高岭土/二甲基亚砜插层复合物,并对产物进行表征,结果表明,在60 ℃超声水浴插层处理3 h,700℃热处理的插层剥离效果较好,制得的偏高岭土的粒径为100~900 nm.以制得的偏高岭土为原料,采用水热法成功制备了亚微米级13X沸石分子筛.利用XRD、SEM和静态饱和吸水量测定等手段对不同预晶化过程、晶化时间下制备的产物进行分析,并对亚微米级13X分子筛的生长过程进行了研究.预晶化时间4 h,晶化时间24 h条件下,制备的13X沸石分子筛晶体呈八面体晶型,形状规则,大小均一,粒径为100 nm,其相对结晶度为90.72%,静态饱和吸水率达33.17%.比表面积为909 m2/g,总微孔容为0.15 cm3/g,孔径大小为33×10-9μm.

关键词: 煤系高岭土;插层;亚微米级;13X分子筛

Abstract: The kaolin/dimethylsulfoxide intercalation composite was synthesized and using coal-measure kaolin as raw materials.The results show that the optimum conditions of intercalation and exfoliation are ultrasonic bath at 60℃for 3 h,heat treatment at 700 ℃and the size of metakaolin is 100-900 nm.13X zeolite is synthesized by hydrothermal preparation from metakaolinite.The solid products obtained at different pre-crystallization process and crystallization time were characterized by XRD, SEM and static water adsorption test method to study the growth process of the 13X zeolite preparation.The results show that the optimized reaction conditions are as follows:pre-crystallization time was 4 h,crystallization time is 24 h.Under these conditions,13X zeolite with the octahedral crystal type and uniform size have an relative crystallinity of 90.72%and water absorption ratio is 33.17%.BET surface area is 909 m2/g, total micropore volume is 0.15 cm3/g,pore size is 33×10-9μm.

Key words: coal-measure kaolin;intercalation;sub-micron scale;13X zeolite

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