Microporous and Mesoporous Materials最新文献_第5页

Adsorption of CO2, CH4, N2 and He on MFI, CHA and DDR zeolites

IF 4.8 3区材料科学

Microporous and Mesoporous Materials Pub Date : 2025-03-11 DOI: 10.1016/j.micromeso.2025.113599

Iliana Kyriazidou, Mojtaba Sinaei Nobandegani, Jonas Hedlund, Liang Yu

{"title":"Adsorption of CO2, CH4, N2 and He on MFI, CHA and DDR zeolites","authors":"Iliana Kyriazidou, Mojtaba Sinaei Nobandegani, Jonas Hedlund, Liang Yu","doi":"10.1016/j.micromeso.2025.113599","DOIUrl":"10.1016/j.micromeso.2025.113599","url":null,"abstract":"<div><div>The adsorption equilibrium isotherms of the common components of natural gas and biogas, CO<sub>2</sub>, CH<sub>4</sub>, N<sub>2</sub>, and He were experimentally measured over wide temperature ranges on all-silica MFI, CHA, and DDR zeolite crystals. First, large zeolite crystals, suitable for adsorption measurements, were synthesized and characterized by XRD and SEM. In the next step, gas adsorption data was recorded and the Toth equation was fitted to the measured adsorption data, and the adsorption capacity at saturation (<em>C</em><sub><em>sat</em></sub>), affinity constant (<em>b</em>), and Toth heterogeneity parameter (<em>t</em>) were estimated. Finally, the van't Hoff equation was used to calculate the isosteric enthalpy of adsorption and adsorption entropy for all gases on each zeolite. The results reveal that the Toth equation can accurately predict the adsorption of gases on the studied microporous zeolite crystals in the investigated temperature range. To the best of our knowledge, the saturation adsorption capacity and adsorption enthalpy for helium on CHA and DDR zeolites have been determined experimentally for the first time in the present work. The estimated adsorption parameters presented in this work are accurate, primarily due to the large crystals used for the adsorption measurements and the recording of low-temperature adsorption equilibrium isotherms over broad temperature ranges. These factors are crucial for the reliability of our results, which are invaluable for understanding adsorption and mass transfer in zeolite materials, as well as for advancing the development of zeolite materials for gas separation.</div></div>","PeriodicalId":392,"journal":{"name":"Microporous and Mesoporous Materials","volume":"390 ","pages":"Article 113599"},"PeriodicalIF":4.8,"publicationDate":"2025-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143619535","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Role of silanol groups and hydrothermal rehydroxylation on the functionalization of SBA-15 with APTES for CO2 capture

IF 4.8 3区材料科学

Microporous and Mesoporous Materials Pub Date : 2025-03-11 DOI: 10.1016/j.micromeso.2025.113597

Reyna Ojeda-López , J. Marcos Esparza-Schulz , Isaac J. Pérez-Hermosillo , Enrique Vilarrasa-García , Enrique Rodriguez-Castellón

{"title":"Role of silanol groups and hydrothermal rehydroxylation on the functionalization of SBA-15 with APTES for CO2 capture","authors":"Reyna Ojeda-López , J. Marcos Esparza-Schulz , Isaac J. Pérez-Hermosillo , Enrique Vilarrasa-García , Enrique Rodriguez-Castellón","doi":"10.1016/j.micromeso.2025.113597","DOIUrl":"10.1016/j.micromeso.2025.113597","url":null,"abstract":"<div><div>To identify the most suitable initial characteristics of an APTES-functionalized SBA-15 material, a series of SBA-15 samples was synthesized. Firstly, to remove the template, two methods were employed: i) water and ethanol washing method, and ii) calcination method where three calcination temperatures were explored (350, 450 and 550 °C), all carried out in a constant air flow. The purpose of avoiding calcination of the material is to prevent the loss of silanol groups, which play a key role in the chemical modification with amino groups. And secondly, a portion of these materials were subjected to a hydrothermal process to improve the amount of surface silanol groups, groups on which APTES molecules are anchored. As a result, eight materials were obtained and subsequently functionalized with APTES. Based on the nitrogen adsorption isotherms, an increase in pore size was observed when the material is rehydroxylated, which demonstrates the formation of silanol groups. Upon functionalization, the average pore size decreased by approximately 1.0 nm, suggesting the formation of new bonds between the surface silanol groups with the ethoxy groups of the APTES molecule. The CO<sub>2</sub> uptake capacity showed promising results for most of the materials, with the uncalcined materials presenting the highest values, 2.52 and 2.32 mmol g<sup>−1</sup> at 1 bar and 25 °C for S15WC-F and S15WC-FR, respectively.</div></div>","PeriodicalId":392,"journal":{"name":"Microporous and Mesoporous Materials","volume":"390 ","pages":"Article 113597"},"PeriodicalIF":4.8,"publicationDate":"2025-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143679917","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Zeolite structure directing agents based upon bulky pyridinium molecules

IF 4.8 3区材料科学

Microporous and Mesoporous Materials Pub Date : 2025-03-11 DOI: 10.1016/j.micromeso.2025.113575

Allen Burton, Trong Pham, Hilda Vroman, Stuart Soled, Eugene Terefenko, Andre Sutrisno

{"title":"Zeolite structure directing agents based upon bulky pyridinium molecules","authors":"Allen Burton, Trong Pham, Hilda Vroman, Stuart Soled, Eugene Terefenko, Andre Sutrisno","doi":"10.1016/j.micromeso.2025.113575","DOIUrl":"10.1016/j.micromeso.2025.113575","url":null,"abstract":"<div><div>We report new zeolite frameworks synthesized with bulky pyridinium molecules as structure directing agents (SDAs). Aluminosilicate zeolite EMM-63 is prepared in potassium-containing hydroxide media with N,2,3,5-tetramethypyridinium or its skeletal isomer N,2,4,6-tetramethylpyridinium. Two new zeolites (EMM-64 and EMM-65) are prepared with 1-methyl-6,7-dihydro-5H-cyclopenta[b]pyridin-1-ium. EMM-64 is crystallized in fluoride media with or without aluminum, and EMM-65 is prepared as a borosilicate in hydroxide media. The same SDA molecule can be used to prepare an aluminosilicate with the <strong>RTH</strong> topology, a framework with large cavities and an 8 × 8 channel system. Within each <strong>RTH</strong> cavity, two SDA molecules form a dimer that is not pi-stacked but instead packs with each pyridinium ring interacting with the unsaturated C5 ring of the neighboring molecule. These interactions optimize the van der Waals interactions both within the dimer and between the dimer and the zeolite framework. The diffraction data of EMM-64 are indexed in tetragonal space group <em>I4</em><sub><em>1</em></sub><em>22</em> or <em>I4</em><sub><em>3</em></sub><em>22</em> with unit cell dimensions <em>a</em> = 13.8 Å and <em>c</em> = 18.0 Å, and the unit cell composition is |C<sub>9</sub>NH<sub>12</sub>F<sub>0.9</sub>|<sub>4</sub>Si<sub>64</sub>O<sub>128</sub>. The dense framework structure of EMM-64 possesses a tortuous 3D 8R channel system and is unusual in that the framework is chiral. EMM-64 possesses a 5<sup>12</sup>8<sup>4</sup> cavity with a flat shape like that of the occluded SDA molecule. The fluoride is sited within the 4<sup>2</sup>5<sup>4</sup>6<sup>2</sup> cages of EMM-64.</div></div>","PeriodicalId":392,"journal":{"name":"Microporous and Mesoporous Materials","volume":"390 ","pages":"Article 113575"},"PeriodicalIF":4.8,"publicationDate":"2025-03-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143642952","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Ammonia-assisted dry-gel conversion for preparation of TS-1 with enriched Ti(OSi)3OH active sites

IF 4.8 3区材料科学

Microporous and Mesoporous Materials Pub Date : 2025-03-10 DOI: 10.1016/j.micromeso.2025.113595

Huanhao Lin , Xin Sun , Yucheng Jin , Yunkai Yu , Yueming Liu

{"title":"Ammonia-assisted dry-gel conversion for preparation of TS-1 with enriched Ti(OSi)3OH active sites","authors":"Huanhao Lin , Xin Sun , Yucheng Jin , Yunkai Yu , Yueming Liu","doi":"10.1016/j.micromeso.2025.113595","DOIUrl":"10.1016/j.micromeso.2025.113595","url":null,"abstract":"<div><div>Defective Ti(IV) species, i.e. Ti(OSi)<sub>3</sub>OH, are highly active catalytic sites within the TS-1 framework, and developing efficient methods to enrich these species has attracted significant attention from both academia and industry sectors. Herein, we developed an ammonia-assisted dry-gel conversion (DGC) method to synthesize TS-1-AM enriched with Ti(OSi)<sub>3</sub>OH species using NH<sub>3</sub> (ammonia, AM) as a modifier. Comprehensive characterization using XRD, UV–Vis, SEM, XPS, pyridine-IR, solid-state MAS NMR confirmed the abundant presence of Ti(OSi)<sub>3</sub>OH species in TS-1-AM. The modified catalyst demonstrated exceptional performance in alkene epoxidation, achieving approximately 150% higher catalytic activity compared to the parent TS-1, while maintaining excellent cycling stability. Further studies revealed that the synergistic effect of NH<sub>3</sub> and H<sub>2</sub>O molecules facilitated the selective cleavage of framework Si-O-Ti bonds, promoting the conversion of Ti(OSi)<sub>4</sub> species to Ti(OSi)<sub>3</sub>OH species. Furthermore, the condensation of surface silica hydroxyls, particularly silica hydroxyl nests, enhanced surface hydrophobicity. This straightforward DGC method provides an efficient approach for synthesizing titanosilicates enriched with highly active Ti(OSi)<sub>3</sub>OH species.</div></div>","PeriodicalId":392,"journal":{"name":"Microporous and Mesoporous Materials","volume":"390 ","pages":"Article 113595"},"PeriodicalIF":4.8,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143636866","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Efficient synthesis of smaller crystal ZSM-5 zeolite in low TPAOH-to-silica ratio dry-gel hydrothermal system

IF 4.8 3区材料科学

Microporous and Mesoporous Materials Pub Date : 2025-03-10 DOI: 10.1016/j.micromeso.2025.113596

Jiahui Hu, Hao Jiang, Yitong Guo, Jing Liu, Dan Xu, Guoxing Wu, Yanhui Yi, Zhongkui Zhao, Hongchen Guo

{"title":"Efficient synthesis of smaller crystal ZSM-5 zeolite in low TPAOH-to-silica ratio dry-gel hydrothermal system","authors":"Jiahui Hu, Hao Jiang, Yitong Guo, Jing Liu, Dan Xu, Guoxing Wu, Yanhui Yi, Zhongkui Zhao, Hongchen Guo","doi":"10.1016/j.micromeso.2025.113596","DOIUrl":"10.1016/j.micromeso.2025.113596","url":null,"abstract":"<div><div>The present study is related to the synthesis of nano-sized ZSM-5 zeolite with a dry-gel hydrothermal (DHT) method which is different from the known dry-gel conversion (DGC) method, for it allows the crystallization of the dry-gel in water or n-butylamine solution and the use of common autoclaves. The effects of TPAOH/SiO<sub>2</sub> ratio on the crystal size of ZSM-5 zeolite product, and the viability of synthesizing nano-sized ZSM-5 zeolite using the new method from a TPAOH-poor dry-gel with the aid of co-template n-butylamine are emphasized. Results show that, under the same TPAOH/SiO<sub>2</sub> ratio conditions, DHT synthesis is more beneficial for obtaining smaller crystal size ZSM-5 zeolite than the conventional hydrothermal (CHT) synthesis. The DHT synthesis can be implemented with a TPAOH-rich dry-gel (for example, TPAOH/SiO<sub>2</sub>≥0.15) by using simply water as crystallizing solution, to yield discrete nano-sized ZSM-5 zeolite (crystal size 70 nm), or with a TPAOH-poor dry-gel (for example, TPAOH/SiO<sub>2</sub> = 0.075) by using a concentrated NBA aqueous solution (for example, a solution contains 75 % NBA) as crystallizing solution, to yield aggregates of nano-sized ZSM-5 zeolite (primary particle size 200 nm). The nano-sized ZSM-5 zeolites synthesized by the DHT method are inclined to have larger mesoporous and macroporous volume. After being doped with zinc ions, they become promising catalysts for the aromatization of n-hexane (n-h).</div></div>","PeriodicalId":392,"journal":{"name":"Microporous and Mesoporous Materials","volume":"390 ","pages":"Article 113596"},"PeriodicalIF":4.8,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143628772","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Coadsorption of CO2/CH4 onto zeolitic imidazolate frameworks: The role of inner surface polarity, framework flexibility and topology 沸石咪唑酸盐框架上的 CO2/CH4 凝聚：内表面极性、框架柔性和拓扑结构的作用

IF 4.8 3区材料科学

Microporous and Mesoporous Materials Pub Date : 2025-03-10 DOI: 10.1016/j.micromeso.2025.113557

Rimita Bose , Volodymyr Bon , Thasleem B. Nanakkal , Parasuraman Selvam , Stefan Kaskel , Niket S. Kaisare

{"title":"Coadsorption of CO2/CH4 onto zeolitic imidazolate frameworks: The role of inner surface polarity, framework flexibility and topology","authors":"Rimita Bose , Volodymyr Bon , Thasleem B. Nanakkal , Parasuraman Selvam , Stefan Kaskel , Niket S. Kaisare","doi":"10.1016/j.micromeso.2025.113557","DOIUrl":"10.1016/j.micromeso.2025.113557","url":null,"abstract":"<div><div>The ZIF sub-family of metal-organic frameworks (MOFs) possesses considerable robustness, tunability of pores, flexibility. These properties make ZIFs potential materials for selective CO<sub>2</sub> adsorption from mixture of gases. However, the lack of experimental multi-component co-adsorption studies makes it challenging for translating the fundamental understanding towards large-scale separation applications. Hence, we focused on both single component adsorption and CO<sub>2</sub>/CH<sub>4</sub> co-adsorption measurements. The selected frameworks include ZIF-8, ZIF-90, ZIF-7, ZIF-11 and ZIF-71, which laid the foundation of understanding the influence of functional groups, structural flexibility, crystal size and topology on CO<sub>2</sub> selectivity in presence of CH<sub>4</sub>. The results indicate that polar functional group and gate-opening flexibility are a couple of key parameters to improve CO<sub>2</sub> selectivity for ZIFs. Topology of ZIFs, on the other hand, did not show a significant effect on CO<sub>2</sub> selectivity. The Ideal Adsorbed Solution Theory (IAST) is used to show the compatibility between the theoretical and experimental selectivity. The IAST exhibits mismatch for ZIF-90, indicates limitation of the theory in considering the thermodynamic analysis of framework-guest interactions. The present study highlights the factors influencing CO<sub>2</sub> selectivity in presence of CH<sub>4</sub> through both single and multi-component adsorption isotherms.</div></div>","PeriodicalId":392,"journal":{"name":"Microporous and Mesoporous Materials","volume":"390 ","pages":"Article 113557"},"PeriodicalIF":4.8,"publicationDate":"2025-03-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143628773","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

The effect of SBA-15 doping with NbVOx and TaVOx on the extractive catalytic oxidative desulfurization of dibenzothiophene

IF 4.8 3区材料科学

Microporous and Mesoporous Materials Pub Date : 2025-03-08 DOI: 10.1016/j.micromeso.2025.113592

Katarzyna Stawicka, Julia Gajewska, Maria Ziolek, Maciej Trejda

引用次数: 0

Mesoporous carbon nanospheres encapsulated CoFe2O4 to enhance peroxymonosulfate activation for achieving efficient sulfamethoxazole degradation

IF 4.8 3区材料科学

Microporous and Mesoporous Materials Pub Date : 2025-03-08 DOI: 10.1016/j.micromeso.2025.113591

Wenhao Zhao, Ruifu Han, Chenglong Ge, Denghui Zhang, Chunming Jiang, Xuan Zhang

{"title":"Mesoporous carbon nanospheres encapsulated CoFe2O4 to enhance peroxymonosulfate activation for achieving efficient sulfamethoxazole degradation","authors":"Wenhao Zhao, Ruifu Han, Chenglong Ge, Denghui Zhang, Chunming Jiang, Xuan Zhang","doi":"10.1016/j.micromeso.2025.113591","DOIUrl":"10.1016/j.micromeso.2025.113591","url":null,"abstract":"<div><div>To effectively improve the electron transfer ability mediated by carbon nanomaterials and enhance their activation ability towards peroxymonosulfate (PMS), a novel bimetallic/carbon matrix composite (Mesoporous carbon nanospheres encapsulated CoFe<sub>2</sub>O<sub>4</sub>, CoFe<sub>2</sub>O<sub>4</sub>@MCHS) was prepared for the activation of PMS to degrade sulfamethoxazole (SMX). The system removed 98.55 % of SMX in 30 min using a lower concentration of catalyst (0.05 g/L) and oxidant (1 mM). The superior catalytic performance of CoFe<sub>2</sub>O<sub>4</sub>@MCHS was due to the high specific surface area and pore structure, which offered numerous active sites, while the distinctive yolk-shell architecture safeguarded the active center and enhanced catalyst stability. Surface-bound radicals and electron transfer played a dominant role in the SMX degrading process, while the CoFe<sub>2</sub>O<sub>4</sub>@MCHS/PMS system exhibited enhanced oxidation of electron-rich organic compounds. Moreover, CoFe<sub>2</sub>O<sub>4</sub>@MCHS/PMS exhibited tolerance to a broad spectrum of initial pH levels and demonstrated significant resistance to prevalent anions and humic acid in water, sustaining an effective degradation across various aqueous environments. Four possible degradation pathways of SMX were proposed. In summary, the CoFe<sub>2</sub>O<sub>4</sub>@MCHS/PMS system was both extremely effective and environmentally friendly, offering a novel approach to treat antibiotic wastewater.</div></div>","PeriodicalId":392,"journal":{"name":"Microporous and Mesoporous Materials","volume":"390 ","pages":"Article 113591"},"PeriodicalIF":4.8,"publicationDate":"2025-03-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143591990","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Effect of synthesis parameters on ZIF-8 morphology: Insights from experimental and statistical integrated analysis 合成参数对 ZIF-8 形态的影响：实验和统计综合分析的启示

IF 4.8 3区材料科学

Microporous and Mesoporous Materials Pub Date : 2025-03-07 DOI: 10.1016/j.micromeso.2025.113588

Cristina Sanchez Cereceda, Yuncheng Du

{"title":"Effect of synthesis parameters on ZIF-8 morphology: Insights from experimental and statistical integrated analysis","authors":"Cristina Sanchez Cereceda, Yuncheng Du","doi":"10.1016/j.micromeso.2025.113588","DOIUrl":"10.1016/j.micromeso.2025.113588","url":null,"abstract":"<div><div>Zeolitic Imidazole Framework-8 (ZIF-8) is an important class of metal-organic frameworks (MOFs), which has gained significant attention due to its unique morphological properties, such as high surface area and tunable porosity, making it suitable for applications in catalysis and gas storage. The synthesis of ZIF-8 is highly sensitive to various parameters, including precursor concentration, which affects its morphology and functionality. While many studies have examined the effects of synthesis parameters on ZIF-8 synthesis, they typically adjust only one factor at a time, thus overlooking the potential combined effect of multiple parameters. This study focuses on the joint effect of three critical parameters, i.e., precursor concentration, temperature, and solvent composition, on ZIF-8 morphology. Specifically, a three-factor, three-level experimental design is used to guide our investigation by varying the molar ratio of Zn<sup>2+</sup>:Hmim:solvent (1:60:2228, 1:100:2228, and 1:140:2228), temperatures (0 °C, 24 °C, and 50 °C), and solvent mixtures (methanol:water in volume ratios of 50:50, 70:30, and 90:10). The results show that the size of ZIF-8 varied from 57 nm to 222 nm, with the largest surface area of 1380 m<sup>2</sup>/g observed for nanoparticles sized around 170 nm. Additionally, multivariate control chart analysis is performed to quantitatively evaluate the individual and combined effects of these parameters on morphology. This analysis suggests that the molar ratio is the most significant factor affecting the size, providing insights into the morphology optimization of ZIF-8 for different applications.</div></div>","PeriodicalId":392,"journal":{"name":"Microporous and Mesoporous Materials","volume":"390 ","pages":"Article 113588"},"PeriodicalIF":4.8,"publicationDate":"2025-03-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143591989","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0

Application of Raman spectroscopy and chemometrics in the mechanochemical synthesis of TIFSIX-3-Ni HUMs using twin screw extrusion 拉曼光谱和化学计量学在使用双螺杆挤压法机械化学合成 TIFSIX-3-Ni HUMs 中的应用

IF 4.8 3区材料科学

Microporous and Mesoporous Materials Pub Date : 2025-03-07 DOI: 10.1016/j.micromeso.2025.113558

Ahmed Metawea , Ahmad B. Albadarin , Ozren Jovic , Nicolas Abdel Karim Aramouni , Gavin Walker , Rabah Mouras

{"title":"Application of Raman spectroscopy and chemometrics in the mechanochemical synthesis of TIFSIX-3-Ni HUMs using twin screw extrusion","authors":"Ahmed Metawea , Ahmad B. Albadarin , Ozren Jovic , Nicolas Abdel Karim Aramouni , Gavin Walker , Rabah Mouras","doi":"10.1016/j.micromeso.2025.113558","DOIUrl":"10.1016/j.micromeso.2025.113558","url":null,"abstract":"<div><div>Hybrid ultra-microporous materials (HUMs) are a novel category of porous materials featuring a distinctive 3D structure composed of square lattice layers. In this study, HUMs was produced on a small scale using either solvothermal or ball milling synthesis methods. Building on the successful synthesis of HUMs via ball milling, twin-screw extrusion (TSE) appears to be a suitable method for large-scale and potentially continuous synthesis. The effect of process parameters, such as feeding rate, screw speed, barrel temperature, and liquid-to-solid ratio L/S (m/m), on the properties of the TIFSIX-3-Ni HUM was investigated. The results are presented in two sections: In the first section, we conducted a characterization and qualitative investigation to determine the crystallinity of the collected powder by analysing PXRD diffractograms. The second section involves a quantitative study using partial least squares (PLS) multi-variate analysis to measure the conversion rate of the HUM acquired. This was achieved by utilizing the most effective developed calibration model. The PXRD analysis revealed that the most favourable parameters for producing the HUM involve operating at 50 and 150 RPM, at L/S of 0.5 (m/v), and manually feeding. The highest yield of inactivated TIFSIX-3-Ni was 77.7 %, achieved using Raman spectroscopy combined with the PLS model for quantitative analysis This study marks the first successful continuous synthesis of HUMs and the development of a predictive model for process optimization.</div></div>","PeriodicalId":392,"journal":{"name":"Microporous and Mesoporous Materials","volume":"391 ","pages":"Article 113558"},"PeriodicalIF":4.8,"publicationDate":"2025-03-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"143777604","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

引用次数: 0