Influence of temperature ramp rate and crystallization mode on synthesis of SAPO-5 via solid-phase transformation

doi:10.3969/j.issn.0438-1157.2013.02.045

CIESC Journal ›› 2013, Vol. 64 ›› Issue (2): 735-741.DOI: 10.3969/j.issn.0438-1157.2013.02.045

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Influence of temperature ramp rate and crystallization mode on synthesis of SAPO-5 via solid-phase transformation

LIU Xuguang^1,2, CHEN Shengbo², ZHANG Baoquan^1,2

1. State Key Laboratory of Chemical Engineering, School of Chemical Engineering and Technology, Tianjin University, Tianjin 300072, China;
2. School of Materials Science and Engineering, Qingdao University of Science and Technology, Qingdao 266042, Shandong, China

Received:2012-10-18 Revised:2012-11-19 Online:2013-02-05 Published:2013-02-05
Supported by:
supported by the Key Program of the National Natural Science Foundation of China (21136008) and Taishan Scholars Program of Shandong Province(ts20081119).

升温速率和晶化模式对固相转化合成SAPO-5的影响

刘旭光^1,2, 陈圣博², 张宝泉^1,2

1. 天津大学化工学院,化学工程联合国家重点实验室,天津 300072;
2. 青岛科技大学材料学院,山东青岛 266042

通讯作者: 张宝泉
作者简介:刘旭光(1983—),男,博士,讲师。
基金资助:
国家自然科学基金重点项目(21136008);山东省泰山学者计划项目(ts20081119)。

Abstract

Abstract: Solid-phase transformation is a favorable method for preparation of Si substituted aluminophosphate molecular sieves (SAPO-5).The influence of temperature ramp rate and crystallization mode on the structure of SAPO-5 crystals was investigated by using XRD,SEM and EDS.Pure SAPO-5 phase could be synthesized with high (140℃·h^-1) and low (5.8℃·h^-1) temperature ramp rates.But SAPO-5 as well as SAPO-34 would be obtained with medium temperature ramp rates (17.5—70℃·h^-1).Crystallization mode affected obviously the morphology of SAPO-5.With medium temperature ramp rates,sphere-shaped and hexagonal plate-like SAPO-5 crystals were prepared under dynamic and static crystallization modes respectively.But the substitution mechanism of Si might be SM3 under both crystallization modes.However,crystallization mode did not influence the morphology of SAPO-5 prepared at high and low temperature ramp rates.Substitution mechanism of Si might be SM2 and SM3 under dynamic and static crystallization mode respectively.

Key words: SAPO-5, temperature programmed rate, crystallization mode, substitution mechanism

摘要： 固相转化法有利于合成硅取代型磷酸铝分子筛(SAPO-5)。采用XRD、SEM、EDS表征方法研究了升温速率和晶化模式对SAPO-5分子筛结构的影响。结果表明,在高升温速率(140℃·h^-1)和低升温速率(5.8℃·h^-1)下能合成出纯SAPO-5分子筛,在中等升温速率(17.5～70℃·h^-1)下则有SAPO-34分子筛与SAPO-5伴生。此外,晶化模式对SAPO-5分子筛的形貌有显著影响。在中等升温速率下,动态晶化形成的SAPO-5分子筛为球形,静态晶化则为六边形片状,但Si的取代机制均可能为SM3取代。在高升温速率和低升温速率下,晶化模式不影响SAPO-5分子筛的形貌。而Si在动态晶化时为SM2取代,静态晶化时为SM3取代。

关键词: SAPO-5, 程序升温速率, 晶化模式, 取代机制

CLC Number:

LIU Xuguang, CHEN Shengbo, ZHANG Baoquan. Influence of temperature ramp rate and crystallization mode on synthesis of SAPO-5 via solid-phase transformation[J]. CIESC Journal, 2013, 64(2): 735-741.

刘旭光, 陈圣博, 张宝泉. 升温速率和晶化模式对固相转化合成SAPO-5的影响[J]. 化工学报, 2013, 64(2): 735-741.

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Influence of temperature ramp rate and crystallization mode on synthesis of SAPO-5 via solid-phase transformation

升温速率和晶化模式对固相转化合成SAPO-5的影响

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