Synthesis of Nanosiliceous Zeolite and its Functionalization with Silane Derivatives

2013 ◽  
Vol 62 (3) ◽  
Author(s):  
Norfariha Hassan ◽  
Zainab Ramli ◽  
Salasiah Endud
Keyword(s):  
Particle Size ◽  
Surface Modification ◽  
Hydrothermal Method ◽  
Surface Area ◽  
Crystal Morphology ◽  
Synthesis Method ◽  
Silanol Group ◽  
Bet Surface Area ◽  
Post Synthesis ◽  
Good Support

A nanosiliceous zeolite has been synthesized using hydrothermal method. Theoretically, nanosiliceous zeolite contains a lot of silanol group which allow the functionalization process for surface modification. Siliceous zeolite of the type silicalite (Sil) has been synthesized hydrothermally at 150°C for 4 days. The silicalite material was then functionalized with silane derivatives i.e 3–(triethoxysilyl)–propylamine (APTES), octadecyltrichlorosilane (OTS) and (3–mercaptopropyl)–trimethoxysilane (MPTS) using post–synthesis method. XRD results showed the formation of silicalite phase crystallinity. The FTIR result showed that Sil–OTS gave the highest intensity of the vibration assigned for silane derivative, followed by Sil–APTES and Sil–MPTS. The BET surface area of the functionalized–Sil decreased, showing the attachment of silane derivatives to silicalite has occurred. FESEM results showed sheet of hexagonal stick together to form granule–like crystal morphology of functionalized–Sil samples with larger particle size was observed for Sil–OTS, followed by Sil–APTES and Sil–MPTS after functionalization process. The functionalized–Sil sample is expected to be a good support for chemosensor molecules.

scholarly journals Microwave-Assisted vs. Conventional Hydrothermal Synthesis of MoS2 Nanosheets: Application towards Hydrogen Evolution Reaction

Crystals ◽  
2020 ◽  
Vol 10 (11) ◽  
pp. 1040 ◽  
Author(s):  
Getachew Solomon ◽  
Raffaello Mazzaro ◽  
Vittorio Morandi ◽  
Isabella Concina ◽  
Alberto Vomiero
Keyword(s):  
Hydrothermal Synthesis ◽  
Hydrothermal Method ◽  
Hydrogen Evolution ◽  
Hydrogen Evolution Reaction ◽  
Current Density ◽  
Crystal Morphology ◽  
Synthesis Method ◽  
Synthesis Methods ◽  
Mos2 Nanosheets ◽  
Microwave Assisted

Molybdenum sulfide (MoS2) has emerged as a promising catalyst for hydrogen evolution applications. The synthesis method mainly employed is a conventional hydrothermal method. This method requires a longer time compared to other methods such as microwave synthesis methods. There is a lack of comparison of the two synthesis methods in terms of crystal morphology and its electrochemical activities. In this work, MoS2 nanosheets are synthesized using both hydrothermal (HT-MoS2) and advanced microwave methods (MW-MoS2), their crystal morphology, and catalytical efficiency towards hydrogen evolution reaction (HER) were compared. MoS2 nanosheet is obtained using microwave-assisted synthesis in a very short time (30 min) compared to the 24 h hydrothermal synthesis method. Both methods produce thin and aggregated nanosheets. However, the nanosheets synthesized by the microwave method have a less crumpled structure and smoother edges compared to the hydrothermal method. The as-prepared nanosheets are tested and used as a catalyst for hydrogen evolution results in nearly similar electrocatalytic performance. Experimental results showed that: HT-MoS2 displays a current density of 10 mA/cm2 at overpotential (−280 mV) compared to MW-MoS2 which requires −320 mV to produce a similar current density, suggesting that the HT-MoS2 more active towards hydrogen evolutions reaction.

scholarly journals Polymer-Assisted Modification of Metal-Organic Framework MIL-96 (Al): Influence on Particle Size, Crystal Morphology and Perfluorooctanoic Acid (PFOA) Removal

2020 ◽  
Author(s):  
Luqman Hakim Mohd Azmi ◽  
Daryl R. Williams ◽  
Bradley P. Ladewig
Keyword(s):  
Particle Size ◽  
Crystal Morphology ◽  
Low Cost ◽  
Metal Organic Framework ◽  
Synthesis Method ◽  
Perfluorooctanoic Acid ◽  
Water Soluble ◽  
Water Soluble Polymer ◽  
Metal Organic ◽  
Organic Framework

<div><b>Abstract</b></div><div>A new synthesis method was developed to prepare an aluminum-based metal organic framework (MIL-96) with a larger particle size and different crystal habits. A low cost and water-soluble polymer, hydrolyzed polyacrylamide (HPAM), was added in varying quantities into the synthesis reaction to achieve >200% particle size enlargement with controlled crystal morphology. The modified adsorbent, MIL-96-RHPAM2, was systematically characterized by SEM, XRD, FTIR, BET and TGA-MS. Using activated carbon (AC) as a reference adsorbent, the effectiveness of MIL-96-RHPAM2 for perfluorooctanoic acid (PFOA) removal from water was examined. The study confirms stable morphology of hydrated MIL-96-RHPAM2 particles as well as a superior PFOA adsorption capacity (340 mg/g) despite its lower surface area, relative to standard MIL-96. MIL-96-RHPAM2 suffers from slow adsorption kinetics as the modification significantly blocks pore access. The strong adsorption of PFOA by MIL-96-RHPAM2 was associated with the formation of electrostatic bonds between the anionic carboxylate of PFOA and the amine functionality present in the HPAM backbone. Thus, the strongly held PFOA molecules in the pores of MIL-96-RHPAM2 were not easily desorbed even after eluted with a high ionic strength solvent (500 mM NaCl). Nevertheless, this simple HPAM addition strategy can still chart promising pathways to impart judicious control over adsorbent particle size and crystal shapes while the introduction of amine functionality onto the surface chemistry is simultaneously useful for enhanced PFOA removal from contaminated aqueous systems.<br></div>

scholarly journals Polymer-Assisted Modification of Metal-Organic Framework MIL-96 (Al): Influence on Particle Size, Crystal Morphology and Perfluorooctanoic Acid (PFOA) Removal

2020 ◽  
Author(s):  
Luqman Hakim Mohd Azmi ◽  
Daryl R. Williams ◽  
Bradley P. Ladewig
Keyword(s):  
Particle Size ◽  
Crystal Morphology ◽  
Low Cost ◽  
Metal Organic Framework ◽  
Synthesis Method ◽  
Perfluorooctanoic Acid ◽  
Water Soluble ◽  
Water Soluble Polymer ◽  
Metal Organic ◽  
Organic Framework

<div><b>Abstract</b></div><div>A new synthesis method was developed to prepare an aluminum-based metal organic framework (MIL-96) with a larger particle size and different crystal habits. A low cost and water-soluble polymer, hydrolyzed polyacrylamide (HPAM), was added in varying quantities into the synthesis reaction to achieve >200% particle size enlargement with controlled crystal morphology. The modified adsorbent, MIL-96-RHPAM2, was systematically characterized by SEM, XRD, FTIR, BET and TGA-MS. Using activated carbon (AC) as a reference adsorbent, the effectiveness of MIL-96-RHPAM2 for perfluorooctanoic acid (PFOA) removal from water was examined. The study confirms stable morphology of hydrated MIL-96-RHPAM2 particles as well as a superior PFOA adsorption capacity (340 mg/g) despite its lower surface area, relative to standard MIL-96. MIL-96-RHPAM2 suffers from slow adsorption kinetics as the modification significantly blocks pore access. The strong adsorption of PFOA by MIL-96-RHPAM2 was associated with the formation of electrostatic bonds between the anionic carboxylate of PFOA and the amine functionality present in the HPAM backbone. Thus, the strongly held PFOA molecules in the pores of MIL-96-RHPAM2 were not easily desorbed even after eluted with a high ionic strength solvent (500 mM NaCl). Nevertheless, this simple HPAM addition strategy can still chart promising pathways to impart judicious control over adsorbent particle size and crystal shapes while the introduction of amine functionality onto the surface chemistry is simultaneously useful for enhanced PFOA removal from contaminated aqueous systems.<br></div>

scholarly journals One-Step Synthesis of Spherical γ-Fe2O3 Nanopowders and the Evaluation of Their Photocatalytic Activity for Orange I Degradation

2015 ◽  
Vol 2015 ◽  
pp. 1-8 ◽  
Author(s):  
Chunhua Liang ◽  
Hui Liu ◽  
Jianmin Zhou ◽  
Xiaochun Peng ◽  
Haizhou Zhang
Keyword(s):  
Particle Size ◽  
Reaction Time ◽  
Synthesis Method ◽  
Total Pore Volume ◽  
Xrd Analysis ◽  
Bet Surface Area ◽  
Particle Sizes ◽  
Aqueous Synthesis ◽  
One Step ◽  
The One

Maghemite (γ-Fe2O3) nanopowders were synthesized under aeration (oxidizing) conditions by aqueous synthesis in this study. The microstructures of the prepared powders were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and BET-BJH. The XRD analysis and the chemical experiments showed that well-crystallized γ-Fe2O3 nanoparticles were successfully obtained with a mean particle size of approximately 17 nm. The prepared γ-Fe2O3 was spherical with a BET surface area of 14.357 m2/g and a total pore volume of 0.050 cm3/g. Varying the reaction conditions, such as pH, temperature, and reaction time, we obtained crystallized γ-Fe2O3 powders with different crystallization extent and different particle sizes. When the pH of the reaction suspension was increased, the reaction time was prolonged, and the reaction temperature was increased, the γ-Fe2O3 powders underwent superior crystallization and had larger particle sizes. All the obtained γ-Fe2O3 powders had significant photocatalytic activities under both UV and visible light irradiation for Orange I degradation, and the powders with better crystallization and larger particle size had relatively lower activities for Orange I photocatalytic degradation. The one-step aqueous synthesis method presented in this paper may provide an advantageous pathway to synthesize large quantities of this important iron oxide.

scholarly journals Synthesis of Hydrophobic Mesoporous Material MFS and Its Adsorption Properties of Water Vapor

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Guotao Zhao ◽  
Zhenxiao Zhao ◽  
Junliang Wu ◽  
Daiqi Ye
Keyword(s):  
Water Vapor ◽  
Surface Area ◽  
Mesoporous Material ◽  
High Surface ◽  
Synthesis Method ◽  
Gravimetric Method ◽  
Total Pore Volume ◽  
Adsorption Properties ◽  
Bet Surface Area ◽  
Mcm 41

Fluorine-containing hydrophobic mesoporous material (MFS) with high surface area is successfully synthesized with hydrothermal synthesis method by using a perfluorinated surfactant SURFLON S-386 template. The adsorption properties of water vapor on the synthesized MFS are also investigated by using gravimetric method. Results show that SEM image of the MFS depicted roundish morphology with the average crystal size of 1-2 μm. The BET surface area and total pore volume of the MFS are 865.4 m2 g−1and 0.74 cm3 g−1with a narrow pore size distribution at 4.9 nm. The amount of water vapor on the MFS is about 0.41 mmol g−1at 303 K, which is only 52.6% and 55.4% of MCM-41 and SBA-15 under the similar conditions, separately. The isosteric adsorption heat of water on the MFS is gradually about 27.0–19.8 kJ mol−1, which decreases as the absorbed water vapor amount increases. The value is much smaller than that on MCM-41 and SBA-15. Therefore, the MFS shows more hydrophobic surface properties than the MCM-41 and SBA-15. It may be a kind of good candidate for adsorption of large molecule and catalyst carrier with high moisture resistance.

Methanol Conversion to Propylene over Mo-HZSM-5 Zeolite

2013 ◽  
Vol 834-836 ◽  
pp. 476-480
Author(s):  
Hai Rong Zhang ◽  
Hong Yan Liu ◽  
Yu Jiang ◽  
Xiao Hua Chang ◽  
Kai Yuan ◽  
...  
Keyword(s):  
Hydrothermal Method ◽  
Surface Area ◽  
Fixed Bed ◽  
Nitrogen Adsorption ◽  
Methanol Conversion ◽  
Catalytic Performance ◽  
Bet Surface Area ◽  
Al Content ◽  
Strong Acidity

A series of Mo-ZSM-5 zeolites have been synthesized by in site hydrothermal method and their catalytic performance for methanol conversion to propylene was tested in a fixed bed reaction at WHSV=4 h-1, pressure of 1 atm, and MeOH/H2O (mol) ratio of 1. The effect of Mo and Al content on the structure and acidity of Mo-ZSM-5 zeolites were characterized by nitrogen adsorption and NH3-TPD. The results showed that Mo incorporation gradually decreased the BET surface area and weaken the strong acidity on the surface of the zeolites. At 470 °C, the maximum selectivity of propylene and the P/E (Propylene to Ethane) ratio were achieved 45.04 % and 7.30, which were higher than those over Mo free HZSM-5 by 4.12% and 3.47, respectively. Mo-ZSM-5 zeolites are promising catalysts for methanol conversion to propylene with a high P/E.

scholarly journals R-Silsesquioxane-Based Network Polymers by Fluoride Catalyzed Synthesis: An Investigation of Cross-Linker Structure and Its Influence on Porosity

Materials ◽  
2020 ◽  
Vol 13 (8) ◽  
pp. 1849 ◽  
Author(s):  
Nai-hsuan Hu ◽  
Joseph C. Furgal
Keyword(s):  
Surface Area ◽  
Environmental Remediation ◽  
General Structure ◽  
Synthesis Method ◽  
Porous Networks ◽  
Pore Size Distributions ◽  
Solvent Systems ◽  
Cross Linker ◽  
Post Synthesis ◽  
Synthesized Materials

Silsesquioxane-based networks are an important class of materials that have many applications where high thermal/oxidative stability and porosity are needed simultaneously. However, there is a great desire to be able to design these materials for specialized applications in environmental remediation and medicine. To do so requires a simple synthesis method to make materials with expanded functionalities. In this article, we explore the synthesis of R-silsesquioxane-based porous networks by fluoride catalysis containing methyl, phenyl and vinyl corners (R-Si(OEt)3) combined with four different bis-triethoxysilyl cross-linkers (ethyl, ethylene, acetylene and hexyl). Synthesized materials were then analyzed for their porosity, surface area, thermal stability and general structure. We found that when a specified cage corner (i.e., methyl) is compared across all cross-linkers in two different solvent systems (dichloromethane and acetonitrile), pore size distributions are consistent with cross-linker length, pore sizes tended to be larger and π-bond-containing cross-linkers reduced overall microporosity. Changing to larger cage corners for each of the cross-linkers tended to show decreases in overall surface area, except when both corners and cross-linkers contained π-bonds. These studies will enable further understanding of post-synthesis modifiable silsesquioxane networks.

scholarly journals Two-Step Hydrothermal Synthesis of Well-Dispersed (Na0.5Bi0.5)TiO3 Spherical Powders

2019 ◽  
Vol 2019 ◽  
pp. 1-8 ◽  
Author(s):  
Zhuo Shi ◽  
Lianlai Sun ◽  
Kun Liu ◽  
Yingying Zhang ◽  
Weiyuan Wang ◽  
...  
Keyword(s):  
Particle Size ◽  
Hydrothermal Synthesis ◽  
Hydrothermal Method ◽  
Synthesis Method ◽  
Spherical Shape ◽  
Raw Material ◽  
Second Step ◽  
In Situ Crystallization ◽  
Uniform Particle Size

(Na0.5Bi0.5)TiO3 (NBT) powders that have well-dispersed, uniform particle size and well-developed spherical shape were successfully prepared by a two-step hydrothermal synthesis method. Nanosized TiO2 powders were firstly synthesized by a hydrothermal method, and then the TiO2 particles are used as a raw material to synthesize NBT powders. It was found that by using the TiO2 nanoparticles as Ti source, the well-dispersed spherical NBT powders with about 200 nm in size could be obtained at 200°C for 4 h with a low mineralizer concentration of 6 mol/L NaOH in the second step. The formation of spherical NBT powders can be explained by first generating nuclei on the surface of TiO2 nanoparticles via in situ crystallization mechanism and then crystal growing and agglomerating by dissolution-recrystallization mechanism.

Development of Heterostructured Ferroelectric SrZrO3/CdS Photocatalysts with Enhanced Surface Area and Photocatalytic Activity

2020 ◽  
Vol 20 (6) ◽  
pp. 3770-3779 ◽  
Author(s):  
Umar Farooq ◽  
Farheen Naz ◽  
Ruby Phul ◽  
Nayeem Ahmad Pandit ◽  
Sapan Kumar Jain ◽  
...  
Keyword(s):  
Particle Size ◽  
Dielectric Constant ◽  
Photocatalytic Activity ◽  
Surface Area ◽  
Room Temperature ◽  
Average Particle Size ◽  
Chemical Deposition ◽  
Bet Surface Area ◽  
Cds Nanoparticles ◽  
Average Particle

This paper reports the attempt to develop an efficient heterostructure photocatalyst by employing SrZrO3 as ferroelectric substrate with deposited nanostructured CdS semiconductor on the surface. Primarily bare SrZrO3 and CdS nanoparticles were synthesized by using polymeric citrate precursor and co-precipitation routes, respectively. The chemical deposition technique was used to develop the CdS over the surface of the pre-synthesized SrZrO3 nanoparticles. The synthesized bare nanoparticles and their heterostructure were characterized by XRD which shows the formation of orthorhombic and face centred cubic (FCC) phases of SrZrO3 and CdS, respectively. TEM was used to estimate the morphology and particle size of as-synthesized nanoparticles, which shows the average particle size of 14, 24 and 25 nm for SrZrO3, CdS and SrZrO3/CdS, respectively. The BET surface area of SrZrO3, CdS and SrZrO3/CdS samples was found to be 299, 304 and 312 m2/g respectively. Methylene blue was used as model pollutant to determine the photocatalytic activity of the synthesized nanomaterials. The heterostructure shows an enhanced activity as compared to bare nanoparticles. Dielectric constant and dielectric loss of the nanoparticles was investigated as a function of frequency at room temperature and as a function of temperature at 500 kHz. The room temperature dielectric constant for SrZrO3, CdS and SrZrO3/CdS was found to be 13.2, 17.8 and 25.5 respectively at 100 kHz.

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