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作 者:高宁宁 刘相李 拓鹏飞 高俊魁[1] 钟进[1] 王辉国[1] 郁灼[1] Gao Ningning;Liu Xiangli;Tuo Pengfei;Gao Junkui;Zhong Jin;Wang Huiguo;Yu Zhuo(SINOPEC Research Institute of Petroleum Processing,Beijing 100083)
机构地区:[1]中国石化石油化工科学研究院,北京100083
出 处:《石油炼制与化工》2022年第2期69-76,共8页Petroleum Processing and Petrochemicals
基 金:中国石油化工股份有限公司合同项目(420058-5)。
摘 要:为了合成结晶度较高的纯低硅X分子筛,系统研究了合成体系的硅铝比[n(SiO_(2))n(Al_(2)O_(3))]、碱硅比[n(Na_(2)O+K_(2)O)n(SiO_(2))]、水碱比[n(H_(2)O)n(Na_(2)O+K_(2)O)]、钾碱比[n(K_(2)O)n(Na_(2)O+K_(2)O)]及老化温度、晶化温度对产物性质的影响规律,采用X射线衍射、甲苯动态吸附、X射线荧光光谱、固体核磁共振、扫描电镜对产物进行表征。结果表明:随着合成体系硅铝比、碱硅比、水碱比、钾碱比、老化温度、晶化温度的升高,所得低硅X分子筛的结晶度和合成产物的甲苯吸附容量均呈先升高后降低趋势;合成体系优选的硅铝比为2.05、碱硅比为3.25、水碱比为17、钾碱比为0.23、老化温度为50~80℃、晶化温度为95℃,所得低硅X分子筛的形貌为0.5~1.5μm晶粒聚集的球体,硅铝比为2.0,不含非骨架铝。In order to synthesize pure low-silicon X zeolite with high crystallinity,the effects of n(SiO_(2))n(Al_(2)O_(3)),n(Na_(2)O+K_(2)O)n(SiO_(2)),n(H 2O)n(Na_(2)O+K_(2)O)and n(K 2O)n(Na_(2)O+K_(2)O)as well as aging and crystallization temperature on the properties of the products were systematically investigated.The products were characterized by X-ray diffraction,dynamic adsorption of toluene,X-ray fluorescence spectrum,solid state nuclear magnetic resonance,and scanning electron microscopy.The results showed that with the increase of n(SiO_(2))n(Al_(2)O_(3)),n(Na_(2)O+K_(2)O)n(SiO_(2)),n(H_(2)O)n(Na_(2)O+K_(2)O),n(K_(2)O)n(Na_(2)O+K_(2)O),aging temperature and crystallization temperature,the crystallinity and toluene adsorptive capacity of the synthesized low silicon X zeolite was increased firstly and then decreased.Under the optimum conditions covering a n(SiO_(2))n(Al_(2)O_(3))of 2.05,a n(Na_(2)O+K_(2)O)n(SiO_(2))of 3.25,a n(H 2O)n(Na_(2)O+K_(2)O)of 17,a n(K_(2)O)n(Na_(2)O+K_(2)O)of 0.23,an aging temperature of 50-80℃,and a crystallization temperature of 95℃,the low-silicon X zeolite with high crystallinity degree can be obtained.The low-silicon X zeolite with a n(SiO_(2))n(Al_(2)O_(3))of 2.0 without non-framework Al,shows sphere morphorology wich a diameter of 0.5-1.5μm.
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