Rapid Synthesis of MCM-41 from Rice Husk Using Ultrasonic Wave: Optimation of Sonication Time

2019 ◽  
Vol 948 ◽  
pp. 198-205
Author(s):  
Suyanta Suyanta ◽  
Eko Sri Kunarti ◽  
Bambang Rusdiarso ◽  
Dritta Anies Cahaya ◽  
Efa Radnawati ◽  
...  
Keyword(s):  
Optimum Condition ◽  
Ultrasonic Wave ◽  
Rice Husk ◽  
Nitrogen Adsorption ◽  
Sonication Time ◽  
Ultrasound Waves ◽  
Comb Structure ◽  
Silica Source ◽  
Adsorption Desorption ◽  
Mcm 41

Ultrasound waves with 48 KHz of frequency were applied for the synthesis of MCM-41 using rice husk as the silica source. The effect of sonication time (30, 60, 90, 120, 150, 180, and 210 min) on the crystallinity of calcined MCM-41 was investigated. Characterization using XRD and FTIR indicated that the ordered structure of MCM-41 could be synthesized by ultrasonic wave. Sonication time at 150 min was found to be the optimum condition. The nitrogen adsorption-desorption isotherms informed that the mesoporous material produced at the optimum condition has 794.73 m2·g-1of surface area, 3.02 nm of BJH pore diameter, 1.17 nm of wall thickness, and 0.68 ml·g-1 of pore volume. While based on the TEM image, the material has hexagonal or a honey-comb structure.

scholarly journals Synthesis of Nb/MCM-48 material using rice husk ash as silica source with different SI/NB molar ratios

2021 ◽  
Vol 45 (171) ◽  
pp. 85-95
Author(s):  
Victor De Aguilar Pedott ◽  
Iemedelais Bordin ◽  
Carolina Elisa Demaman Oro ◽  
Ricardo Jorge Macieski ◽  
Diego Ivan Petkowicz ◽  
...  
Keyword(s):  
Rice Husk ◽  
Rice Husk Ash ◽  
Nitrogen Adsorption ◽  
Structure Directing Agent ◽  
Alternative Source ◽  
Molar Ratios ◽  
Silica Source ◽  
In Situ Deposition ◽  
Adsorption Desorption

The large amount of rice produced in Brazil generates a large volume of co-products, such as, Rice Husk (RH) and Rice Husk Ash (RHA). These co-products have amounts of silicon (Si) present in their structure, which can be used to synthesize silica-based materials as zeolites and MCM-type structures. The synthesis of MCM-48 material was carried out at room temperature, using the ionic liquid [C16MI·Cl] as structure-directing agent, depositing the niobium in situ during the synthesis with different molar ratios of Si/Nb (5, 20, 50 and 80). The material obtained was subjected to characterization by X-Ray Diffraction (XRD), Nitrogen Adsorption/Desorption isotherms and Scanning Electron Microscopy (SEM). The results confirm the formation of Nb/MCM-48 materials, in which their properties are consistent with those described in the literature. The deposition of Nb on MCM-48 did not change its structural properties, such as specific surface area and pore distribution for Si/Nb higher than 5. The results obtained demonstrate the success in the synthesis of mesoporous materials Nb/MCM-48 using industrial residues of rice as an alternative source of silicon, and in situ deposition of the niobium metal on the structure.

Preparation of Mesoporous Silica from Rice Husk Ash: Effect of Depolymerizing Agents on Physico-Chemical Properties

2010 ◽  
Vol 93-94 ◽  
pp. 664-667 ◽  
Author(s):  
Supakij Suttiruengwong ◽  
P. Puathawee ◽  
M. Chareonpanich
Keyword(s):  
Rice Husk ◽  
Rice Husk Ash ◽  
Chemical Properties ◽  
Nitrogen Adsorption ◽  
Mesoporous Silicas ◽  
Organic Residues ◽  
Hydrophobic Property ◽  
Carbon Chains ◽  
Physico Chemical ◽  
Adsorption Desorption

The aim of this work was to prepare mesoporous silicas derived from rice husk ash (RHA) using three different depolymerizing agents; glycerol, 1,3 propanediol and 1,4 butanediol. The reaction of RHA with different depolymerizing agents was carried out between 200-250°C for 2 hrs. The solution was then hydrolyzed with deionized water to obtain gels. After a few washing step, gels were oven-dried and calcined at 500 °C for 24 hrs. Prepared mesoporous silicas were then characterized using Nitrogen adsorption-desorption measurement, FTIR, TGA, SEM, XRD and XRF. The percent hydrophobicity was determined based on the amount of moisture absorbed using TGA. It was shown that RHA reacted with depolymerizing agents above 200°C to form gels, which, after hydrolysis and calcination, still maintained the mesoporous characteristics. The BET and SEM results indicated that the RHA reacted with 1,3 propanediol had highest pore volume (0.95 cm3/g) and specific surface area (129.30 m2/g) compared to RHA reacted with glycerol and 1,4 butanediol. The distribution of pores computed from BJH desorption branch was also more uniform. FTIR indicated that there was no significant change in the chemical structure of RHA reacted with different depolymerizing agents. The residual C-H bands were found in FTIR spectra for all prepared mesoporous silicas. TGA thermograms confirmed the existence of organic residues (below 2 %wt), which might result from incomplete elimination even after calcination. This was found to be an important factor affecting the hydrophobic property of the reacted RHA. The hydrophobicity of RHA may be tailored by controlling depolymerizing agents and organic residues. Depolymerizing agents with longer carbon chains also favoured the hydrophobic characteristics.

Catalytic Activity of Argentum-loaded MCM-41 for Ozonation of p- Chlorobenzoic Acid (p-CBA) in Aqueous Solution

2015 ◽  
Vol 18 (1) ◽  
Author(s):  
Zhaoqi Pan ◽  
Junyu Zeng ◽  
Bingyan Lan ◽  
Laisheng Li
Keyword(s):  
Aqueous Solution ◽  
Nitrogen Adsorption ◽  
Hexagonal Structure ◽  
Bet Surface Area ◽  
X Ray Diffraction ◽  
Chlorobenzoic Acid ◽  
Transmission Electron ◽  
Initial Ph ◽  
Adsorption Desorption ◽  
Mcm 41

AbstractArgentum-loaded MCM-41 (Ag/MCM-41) was synthesized successfully by a hydrothermal method and used as a catalyst for the ozonation of p-chlorobenzoic acid (p-CBA) in aqueous solution. Ag/MCM-41 was characterized by low angle X-ray diffraction (XRD), nitrogen adsorption-desorption and transmission electron microscopy (TEM). Characterizations suggest that the prepared samples retained a highly regulated mesopores of hexagonal structure and a high BET surface area. The influences of argentum content, initial pH, reaction temperature on the catalytic ozonation were also evaluated. Ag/MCM-41/O

Synthesis and Characterization of Mesoporous Molecular Sieve Al-MCM-41 Using Kaolin as Raw Material

2013 ◽  
Vol 779-780 ◽  
pp. 201-204
Author(s):  
Miao Li ◽  
Hong Wang ◽  
Xian Qing Li ◽  
Jin Rong Liu
Keyword(s):  
Molecular Sieve ◽  
Nitrogen Adsorption ◽  
Mesoporous Molecular Sieve ◽  
Raw Material ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Adsorption Desorption ◽  
Calcined Kaolin ◽  
Mcm 41

Ordered hexagonally mesoporous molecular sieve Al-MCM-41 with Si/Al (atom) ratio=9 was prepared by hydrothermal synthesis using raw kaolin. X-ray diffraction (XRD), Nitrogen adsorption desorption, Transmission Electron Microscope (TEM) and Energy Dispersive X-ray Detector (EDX) were employed to characterise raw kaolin, calcined kaolin, as-synthesized and calcined Al-MCM-41. The results indicated that characteristic reflections of raw kaolin disappeared after calcination, both of as-synthesized and calcined Al-MCM-41 exhibited well ordered hexagonally mesoporous molecular sieve structure.

scholarly journals Synthesis of Amorphous Aluminosilicates from Bintan’s Red Mud as Alumina Source

2018 ◽  
Vol 18 (4) ◽  
pp. 580
Author(s):  
Futri Wulandari ◽  
Eka Putra Ramdhani ◽  
Yatim Lailun Ni’mah ◽  
Ahmad Anwarud Dawam ◽  
Didik Prasetyoko
Keyword(s):  
Red Mud ◽  
Nitrogen Adsorption ◽  
X Ray Diffraction ◽  
Structure Directing Agent ◽  
Alumina Production ◽  
Hydrolysis Method ◽  
Alkali Fusion ◽  
Silica Source ◽  
Bauxite Ore ◽  
Adsorption Desorption

Red mud is a generated by-product in alumina production from bauxite ore. In this study, Bintan’s red mud has been used as alumina and silica source to synthesize amorphous mesoporous aluminosilicates material. Alkali fusion method with a NaOH/red mud ratio 0.8; 1.0; 1.2; 1.4 and 1.5 followed by hydrolysis method was used to extract dissolved alumina and silica from red mud. Synthesis of amorphous aluminosilicates by hydrothermal method was conducted at 80 °C for 24 h. Cetyltrimethylammonium bromide (CTABr) was added as the structure directing agent. Aluminosilicate products were characterized using FTIR spectroscopy (Fourier Transform Infra-Red Spectroscopy), XRD (X-ray Diffraction), SEM (Scanning Electron Microscopy), and nitrogen adsorption-desorption. XRD and SEM result shows that the product was amorphous with low uniformity in terms of surface morphology and particle size. Nitrogen adsorption-desorption profile shows that all aluminosilicates products has a meso pore structure, confirmed by the highest pore distribution at 3.05–17.70 nm. The highest surface area and pore volume were obtained in ASM 0.8 (NaOH/red mud ratio = 0.8) i.e. 177.97 m2/g and 1.09 cm3/g, respectively.

scholarly journals UTILIZATION OF RICE HUSK AS RAW MATERIAL IN SYNTHESIS OF MESOPOROUS SILICATES MCM-41

2011 ◽  
Vol 11 (3) ◽  
pp. 279-284 ◽  
Author(s):  
Suyanta Suyanta ◽  
Agus Kuncaka
Keyword(s):  
Ftir Spectroscopy ◽  
Sodium Silicate ◽  
Rice Husk ◽  
Hydrothermal Process ◽  
X Ray Diffraction ◽  
Rice Husk Silica ◽  
X Ray ◽  
Silica Source ◽  
Significant Difference ◽  
Mcm 41

The research about synthesis and characterization of MCM-41 from rice husk has been done. Silica (SiO2) was extracted from rice husk by refluxing with 3M hydrochloric solution at 80 °C for 3 h. The acid-leached rice husk was filtered, washed, dried and calcined at 650 °C for 6 h lead the rough powder of rice husk silica with light brown in color. Characterization was carried out by X-ray diffraction (XRD) and FTIR spectroscopy method. Rice husk silica was dissolved into the sodium hydroxide solution leading to the solution of sodium silicate, and used as silica source for the synthesis of MCM-41. MCM-41 was synthesized by hydrothermal process to the mixture prepared from 29 g of distilled water, 8.67 g of cetyltrimethyl ammonium bromide (CTMAB), 9.31 g of sodium silicate solution, and amount mL of 1 M H2SO4. Hydrothermal process was carried out at 100 °C in a teflon-lined stainless steel autoclave heated in the oven for 36 h. The solid phase was filtered, then washed with deionised water, and dried in the oven at 100 °C for 2 h. The surfactant CTMAB was removed by calcination at 550 °C for 10 h with heating rate 2 °C/min. The as-synthesized and calcined crystals were characterized by using FTIR spectroscopy, X-ray diffraction and N2 physisorption methods. In order to investigate the effect of silica source, the same procedure was carried out by using pure sodium silicate as silica source. It was concluded that silica extracted from rice husk can be used as raw materials in the synthesis of MCM-41, there is no significant difference in crystallinity and pore properties when was compared to material produced from commercial sodium silicate.

Microwave-assisted immobilization of metallophthalocyanines in mesoporous channels of MCM-41

2007 ◽  
Vol 11 (02) ◽  
pp. 118-124 ◽  
Author(s):  
Mahtab Pirouzmand ◽  
Mostafa M. Amini ◽  
Nasser Safari
Keyword(s):  
Microwave Irradiation ◽  
Textural Properties ◽  
Nitrogen Adsorption ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Solvent Free Conditions ◽  
Short Period ◽  
Vis Spectroscopy ◽  
Adsorption Desorption ◽  
Mcm 41

Metallophthalocyanines have been assembled in MCM-41 channels by microwave irradiation of a mixture of ion-exchanged MCM-41, and 1,2-dicyanobenzene under solvent-free conditions in a considerably short period of time. The prepared materials have been characterized by diffuse reflectance UV-vis spectroscopy, X-ray powder diffraction XRD, differential scanning calorimetry DSC, and Brunauer-Emmett-Teller BET nitrogen adsorption desorption techniques. The X-ray diffraction and Brunauer-Emmett-Teller results showed that the textural properties of MCM-41 were preserved during microwave irradiation.

Adsorption Behavior of Phenol in Aqueous Solution on MCM-41 Grafted by Different Functional Groups

2014 ◽  
Vol 955-959 ◽  
pp. 74-79
Author(s):  
Xiao Jun Sun ◽  
Xiao Chun Yan ◽  
Yu Jie Feng ◽  
Xian Bin Liu
Keyword(s):  
Aqueous Solution ◽  
Adsorption Capacity ◽  
Functional Groups ◽  
Ph Value ◽  
Nitrogen Adsorption ◽  
Adsorption Behaviors ◽  
Prepared Material ◽  
Adsorption Amount ◽  
Adsorption Desorption ◽  
Mcm 41

Four types of organo-functionalized mesoporous silicas were synthesized by post-grafting method, and characterized by powder X-ray diffraction, nitrogen adsorption/desorption and fourier transform infrared spectroscopy. In addition, adsorption behaviors of the prepared material modified with different functional groups were studied by adsorption of phenol in aqueous solution. When the concentration of phenol was 800 mg/L, the equilibrium adsorption capacity of N-aminoethyl-γ-aminopropyl-MCM-41, aminopropyl-MCM-41, mercaptopropyl-MCM-41 and propyl-MCM-41 was respectively as 2.5 times, 2.2 times, 1.9 times, and 1.7 times as that of MCM-41. It was due to the introduction of organo-functional groups, changing the polarity of the channel surface, and increasing the hydrophobic properties. N-aminoethyl-γ-aminopropyl and aminopropyl groups could generate acid-base interactions with phenol, therefore, their adsorption capacity increased much more. Besides, the pH value of the solution could significantly affect the adsorption amount of phenol on samples. The result showed that with the increase of pH, the adsorption amount of phenol increased at first, and then decreased. The maximum adsorption amount of all the prepared materials occurred at about pH value of 6.

Preparation and Characterization of Silica Aerogels/Glass Wool Composites

2012 ◽  
Vol 534 ◽  
pp. 106-109 ◽  
Author(s):  
Jing Xiao Liu ◽  
Xiao Jie Wang ◽  
Fei Shi ◽  
Jia Yu Luo
Keyword(s):  
Thermal Conductivity ◽  
Silica Aerogel ◽  
Ambient Pressure ◽  
Measurement Instrument ◽  
Conductivity Measurement ◽  
Nitrogen Adsorption ◽  
Ambient Pressure Drying ◽  
Glass Wool ◽  
Silica Source ◽  
Adsorption Desorption

Using industrial water glass as silica source, silica aerogel/glass wool composite heat insulation materials were prepared through the gel moulding, surface modification and ambient pressure drying method. The microstructure and porous characteristics of the silica aerogel/glass wool composites were studied by scanning electron microscopy (SEM) and BET nitrogen adsorption-desorption method. The thermal conductivity of silica aerogel/glass wool composites was measured by the thermal conductivity measurement instrument. The results indicate that the as-prepared silica aerogel/glass wool composites exhibit strong hydrophobicity and excellent thermal insulation performance. The thermal conductivity of the obtained silica aerogel/glass wool composites is 1.1×10-2～2.0 W∙m-1∙K-1, and with the increasing of aerogels content, the thermal conductivity of the composites could be decreased further.

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