甲醇体系辅助合成的高硅铝摩尔比ZSM 5分子筛  

Synthesis of ZSM 5 zeolite with high Si/Al mole ratio in an methanol system

作　　者：陶金泉 崔岩[1] 张淑莹 迟克彬[1] 周亚松[2] TAO Jinquan;CUI Yan;ZHANG Shuying;CHI Kebin;ZHOU Yasong(PetroChina Petrochemical Institute,PetroChina Company limited,Beijing 102206,China;School of Environmental and Chemical Engineering,China University of Petroleum(Beijing),Beijing 102206,China)

机构地区：[1]中国石油天然气股份有限公司石油化工研究院,北京102206 [2]中国石油大学(北京)化学工程与环境学院,北京102206

出　　处：《东北石油大学学报》2021年第4期103-111,120,I0007,I0008,共12页Journal of Northeast Petroleum University

基　　金：中国石油天然气股份有限公司直属科研院所基金项目(2020-CB-05-05)。

摘　　要：以偏铝酸钠、工业级硅胶、甲醇等为原料,考察醇硅摩尔比、晶化时间、碱硅摩尔比等对晶化反应的影响,通过添加微量晶种辅助晶化合成高结晶度的高硅铝摩尔比ZSM 5分子筛;采用X线衍射、扫描电镜、N 2吸附等表征方法,对ZSM 5分子筛晶型、形貌、分散度、孔道结构等进行表征。结果表明:当硅铝摩尔比低于100时,单一甲醇体系可以合成高结晶度的纯相ZSM 5分子筛,晶体的分散性较好,多呈规则六棱柱状。在体系晶化时间过长、碱硅摩尔比小于0.107时出现麦羟硅钠石杂晶。添加微量晶种可合成硅铝摩尔比为150的高结晶度纯相ZSM 5分子筛,缩短晶化诱导期和总晶化时间,晶粒尺寸约为1μm,晶体形貌多呈规则六棱柱或孪晶六棱柱。在一定范围内提高晶种的加入量可以改善产品晶体的团聚现象,晶体分散性提高。This thesis deals with the effects of the amount of methanol,crystallization time and the mole ratios of alkali-silica under the crystallization reaction.Adding a small amount of crystal seeds can successfully synthesize well-crystallinity high Si/Al mole ratio ZSM 5 zeolite.X ray diffraction,scanning electron microscopy and N 2 adsorption were used to characterize the crystal form,morphology,dispersion and pore structure.The experimental result shows that when the Si/Al mole ratio is lower than 100,the pure ZSM 5 zeolite with high crystallinity can be directly synthesized in single methanol system.In the mean time the crystal has good dispersion and regular hexagonal prism shape.If the alkali-silica mole ratio is lower than 0.107 or the crystallization time is drawn-out,it will lead to the formation of heterocrysts with malladrite in the system.After adding a small amount of crystal seeds in the methanol system,the high crystallinity ZSM 5 molecular sieves with 150 Si/Al mole ratio can be directly synthesized.The addition of crystal seeds shortens the crystallization induction period and the total crystallization time,and the grain size is about 1μm,the crystal morphology is mostly hexagona or twin hexagonal prism.Increasing the amount of crystal seeds can obviously improve the phenomenon of crystal agglomeration in a certain range,it can also improve the crystal dispersion.

关 键 词：ZSM 5分子筛 甲醇 晶种 水热合成 晶粒 硅铝摩尔比 

分 类 号：TQ426[化学工程]