DICP OpenIR
Crystallization and Si incorporation mechanisms of SAPO-34; Crystallization and Si incorporation mechanisms of SAPO-34
Tan, J; Liu, ZM; Bao, XH; Liu, XC; Han, XW; He, CQ; Zhai, RS
KeywordMechanism Mechanism Molecular Sieves Molecular Sieves Sapo-34 Sapo-34 Synthesis Synthesis Characterization Characterization
Source PublicationMICROPOROUS AND MESOPOROUS MATERIALS ; MICROPOROUS AND MESOPOROUS MATERIALS
2002-06-01 ; 2002-06-01
Volume53Issue:1-3Pages:97-108
Indexed BySCI ; SCI
SubtypeArticle ; Article
WOS HeadingsScience & Technology ; Science & Technology ; Physical Sciences ; Physical Sciences ; Technology ; Technology
WOS SubjectChemistry, Applied ; Chemistry, Applied ; Chemistry, Physical ; Chemistry, Physical ; Nanoscience & Nanotechnology ; Nanoscience & Nanotechnology ; Materials Science, Multidisciplinary ; Materials Science, Multidisciplinary
WOS Research AreaChemistry ; Chemistry ; Science & Technology - Other Topics ; Science & Technology - Other Topics ; Materials Science ; Materials Science
WOS KeywordSOLID-STATE NMR ; SOLID-STATE NMR ; MOLECULAR-SIEVES ; MOLECULAR-SIEVES ; SILICON INCORPORATION ; SILICON INCORPORATION ; CATALYTIC CONVERSION ; CATALYTIC CONVERSION ; METHANOL ; METHANOL ; ZEOLITES ; ZEOLITES
AbstractIn this study of the synthesis of SAPO-34 molecular sieves, XRD, SEM, XRF, IR and NMR techniques were applied to monitor the crystalloid, structure and composition changes of the samples in the whole crystallization process in order to get evidence for the crystallization as well as Si incorporation mechanism of SATO-34. XRD results revealed that the crystallization contained two stages. In the first 2.5 h (the earlier stage), high up to similar to80% of relative crystallinity could be achieved and the crystal size of SAPO-34 was almost the same as that of any longer time, indicating a fast crystallization feature of the synthesis. In this stage, IR revealed that the formation of SAPO-34 framework structure was accompanied by the diminution of hydroxyls, suggesting that crystal nuclei of SAPO-34 may arise from the structure rearrangement of the initial gel and the condensation of the hydroxyls. NMR results reveal that the template and the ageing period are crucial for the later crystallization of SAPO-34. Preliminary structure units similar to the framework of SAPO-34 have already formed before the crystallization began (0 h and low temperature). Evidence from IR, NMR, and XRF shows that the formation of the SAPO-34 may be a type of gel conversion mechanism, the solution support and the appropriate solution circumstance are two important parameters of the crystallization of SAPO-34. Meanwhile, NMR measurements demonstrated that about 80% of total Si atoms directly take part in the formation of the crystal nuclei as well as in the growth of the crystal grains in the earlier stage (<2.5 h). Evidence tends to support that Si incorporation is by direct participation mechanism rather than by the Si substitution mechanism for P in this stage (<2.5 h). In the later stage (>2.5 h), the relative content of Si increased slightly with a little decrease of Al and P. The increase of Si(4Al) and the appearance of the Si(3Al), Si(2Al), Si(1Al) and Si(OAl) in this stage suggest that substitution of the Si atoms for the phosphorus and for the phosphorus and aluminum pair takes place in the crystallization. The relationship among structure, acidity and crystallization process is established, which suggests a possibility to improve the acidity and catalytic properties by choosing a optimum crystallization time, thus controlling the number and distribution of Si in the framework of SAPO-34. (C) 2002 Elsevier Science Inc. All rights reserved.; In this study of the synthesis of SAPO-34 molecular sieves, XRD, SEM, XRF, IR and NMR techniques were applied to monitor the crystalloid, structure and composition changes of the samples in the whole crystallization process in order to get evidence for the crystallization as well as Si incorporation mechanism of SATO-34. XRD results revealed that the crystallization contained two stages. In the first 2.5 h (the earlier stage), high up to similar to80% of relative crystallinity could be achieved and the crystal size of SAPO-34 was almost the same as that of any longer time, indicating a fast crystallization feature of the synthesis. In this stage, IR revealed that the formation of SAPO-34 framework structure was accompanied by the diminution of hydroxyls, suggesting that crystal nuclei of SAPO-34 may arise from the structure rearrangement of the initial gel and the condensation of the hydroxyls. NMR results reveal that the template and the ageing period are crucial for the later crystallization of SAPO-34. Preliminary structure units similar to the framework of SAPO-34 have already formed before the crystallization began (0 h and low temperature). Evidence from IR, NMR, and XRF shows that the formation of the SAPO-34 may be a type of gel conversion mechanism, the solution support and the appropriate solution circumstance are two important parameters of the crystallization of SAPO-34. Meanwhile, NMR measurements demonstrated that about 80% of total Si atoms directly take part in the formation of the crystal nuclei as well as in the growth of the crystal grains in the earlier stage (<2.5 h). Evidence tends to support that Si incorporation is by direct participation mechanism rather than by the Si substitution mechanism for P in this stage (<2.5 h). In the later stage (>2.5 h), the relative content of Si increased slightly with a little decrease of Al and P. The increase of Si(4Al) and the appearance of the Si(3Al), Si(2Al), Si(1Al) and Si(OAl) in this stage suggest that substitution of the Si atoms for the phosphorus and for the phosphorus and aluminum pair takes place in the crystallization. The relationship among structure, acidity and crystallization process is established, which suggests a possibility to improve the acidity and catalytic properties by choosing a optimum crystallization time, thus controlling the number and distribution of Si in the framework of SAPO-34. (C) 2002 Elsevier Science Inc. All rights reserved.
Language英语 ; 英语
URL查看原文 ; 查看原文
WOS IDWOS:000176020100010 ; WOS:000176020100010
Citation statistics
Cited Times:193[WOS]   [WOS Record]     [Related Records in WOS]
Document Type期刊论文
Identifierhttp://cas-ir.dicp.ac.cn/handle/321008/83761
Collection中国科学院大连化学物理研究所
AffiliationChinese Acad Sci, Dalian Inst Chem Phys, State Key Lab Catalysis, Dalian 116023, Peoples R China
Recommended Citation
GB/T 7714
Tan, J,Liu, ZM,Bao, XH,et al. Crystallization and Si incorporation mechanisms of SAPO-34, Crystallization and Si incorporation mechanisms of SAPO-34[J]. MICROPOROUS AND MESOPOROUS MATERIALS, MICROPOROUS AND MESOPOROUS MATERIALS,2002, 2002,53, 53(1-3):97-108, 97-108.
APA Tan, J.,Liu, ZM.,Bao, XH.,Liu, XC.,Han, XW.,...&Zhai, RS.(2002).Crystallization and Si incorporation mechanisms of SAPO-34.MICROPOROUS AND MESOPOROUS MATERIALS,53(1-3),97-108.
MLA Tan, J,et al."Crystallization and Si incorporation mechanisms of SAPO-34".MICROPOROUS AND MESOPOROUS MATERIALS 53.1-3(2002):97-108.
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