scholarly journals One-step synthesis of nitrogen-grafted copper-gallic acid for enhanced methylene blue removal

2021 ◽  
Vol 11 (1) ◽  
Author(s):  
Shella Permatasari Santoso ◽  
Vania Bundjaja ◽  
Artik Elisa Angkawijaya ◽  
Chintya Gunarto ◽  
Alchris Woo Go ◽  
...  

AbstractNitrogen-grafting through the addition of glycine (Gly) was performed on a metal- phenolic network (MPN) of copper (Cu2+) and gallic acid (GA) to increase its adsorption capacity. Herein, we reported a one-step synthesis method of MPN, which was developed according to the metal–ligand complexation principle. The nitrogen grafted CuGA (Ng-CuGA) MPN was obtained by reacting Cu2+, GA, and Gly in an aqueous solution at a molar ratio of 1:1:1 and a pH of 8. Several physicochemical measurements, such as Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), N2 sorption, X-ray diffraction (XRD), and thermal gravimetry analysis (TGA), were done on Ng-CuGA to elucidate its characteristics. The analysis revealed that the Ng-CuGA has non-uniform spherical shaped morphology with a pore volume of 0.56 cc/g, a pore size of 23.25 nm, and thermal stability up to 205 °C. The applicational potential of the Ng-CuGA was determined based on its adsorption capacity against methylene blue (MB). The Ng-CuGA was able to adsorb 190.81 mg MB per g adsorbent at a pH of 6 and temperature of 30 °C, which is 1.53 times higher than the non-grafted CuGA. Detailed assessment of Ng-CuGA adsorption properties revealed their pH- and temperature-dependent nature. The adsorption capacity and affinity were found to decrease at a higher temperature, demonstrating the exothermic adsorption behavior.

2011 ◽  
Vol 80-81 ◽  
pp. 440-443
Author(s):  
Gui Yang Liu ◽  
Jun Ming Guo ◽  
Bao Sen Wang ◽  
Ying He ◽  
Li Li Zhang

In this paper, a low-temperature self-mixing combustion synthesis method was introduced to prepare spinel LiMn2O4. Low-melting raw materials and fuel (acetate salts as starting materials and urea as fuel) were molten to a homogeneous liquid mixture at ~100°C. The mixture was then ignited and calcined at a higher temperature, final products were obtained. The products were determined by X-ray diffraction (XRD) and scanning electric microscope (SEM). XRD analysis indicated that product with higher purity was obtained at 550°C for 5h when the molar ratio of Li:Mn:urea=1:2:4. The impurity Mn2O3 was appeared in the products when the igniting temperature >600°C, and the content of Mn2O3 increased with the increasing igniting temperatures. SEM investigation indicated that the particles of the products were small and agglomerated. The igniting temperature monitoring indicated that the combustion reaction rate increased with increasing igniting temperature, and this did not favor for the formation of LiMn2O4.


2019 ◽  
Vol 19 (01) ◽  
pp. 1950003
Author(s):  
P. R. Ghutepatil ◽  
S. H. Pawar

In this paper, uniform and superparamagnetic nanoparticles have been prepared using one-step polyol synthesis method. Structural, morphological and magnetic properties of obtained MnFe2O4 nanoparticles have been investigated by using X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscope (FE-SEM), transmission electron microscopy (TEM), vibrating sample magnetometry (VSM) and thermogravimetric analysis (TGA) techniques. Structural investigation showed that the average crystallite size of obtained nanoparticles was about 10[Formula: see text]nm. Magnetic study revealed that the nanoparticles were superparamagnetic at room temperature with magnetization 67[Formula: see text]emu/g at room temperature. The self-heating characteristics of synthesized MnFe2O4 nanoparticles were studied by applying external AC magnetic field of 167.6 to 335.2[Formula: see text]Oe at a fixed frequency of 265[Formula: see text]kHz. The SAR values of MnFe2O4 nanoparticles were calculated for 2, 5, 10[Formula: see text]mg[Formula: see text]mL[Formula: see text] concentrations and it is observed that the threshold hyperthermia temperature is achieved for all concentrations.


2018 ◽  
Vol 281 ◽  
pp. 813-818 ◽  
Author(s):  
Xin Liu ◽  
Jia Ke Li

Bismuth vanadate (BiVO4 ) powders were synthesized using Bi (NO3)3.5H2O and NH4VO3 as raw materials, NaOH and HNO3 for pH adjustment. The samples were characterized by X-ray diffraction ( XRD ), scanning electron microscopy (SEM ) and UV-vis diffuse reflectance spectra techniques. The results show that the pH of precursor solution has great effect on the composition and morphology of products. Synthetic product was BiVO4 with two kinds of crystal shape ( monoclinic and tetragonal ) with pH of 3; synthetic product was pure monoclinic phase BiVO4 when the pH is between 5-9. Whereas, V2O5 and Bi2O3 appeared when the pH was 11; synthetic product was a mixture of V2O5 and Bi2O3 with pH of 13, and BiVO4 don’t exist. The photocatalytic activity was evaluated by the degradation of methylene blue solution. It is shown that the synthetic sample has the best photocatalytic ability with pH of 5. The degradation of methylene blue reaches 84.7% when irradiated for 240 min by high pressure mercury lamp, and the sample synthesized at 13 for pH has strong adsorption capacity and poor photocatalytic ability.


2015 ◽  
Vol 1101 ◽  
pp. 286-289 ◽  
Author(s):  
Maya Rahmayanti ◽  
Sri Juari Santosa ◽  
Sutarno

Gallic acid-modified magnetites were synthesized by one and two-step reactions via the newly developed sonochemical co-precipitation method. The two-step reaction included the formation of magnetite powder and mixing the magnetite powder with gallic acid solution, while the one-step reaction did not go through the formation magnetite powder. The obtained gallic acid-modified magnetites were characterized by the Fourier Transform Infrared (FTIR) spectroscopy, the X-Ray Diffraction (XRD) and the Scanning Electron Microscopy (SEM). More over, the magnetic properties were studied by using a Vibrating Sample Magnetometer (VSM). The characterization results showed that there were differences in crystalinity, surface morphology and magnetic properties of products that were formed by one and two-step reactions.


2015 ◽  
Vol 659 ◽  
pp. 121-126 ◽  
Author(s):  
Pat Sooksaen

Aluminium borate nanowhiskers with varying aspect ratio were synthesized via sol–gel synthesis. The morphology of aluminum borate (Al4B2O9 and Al18B4O33) nanowhiskers could be controlled by varying the aluminum to boron (Al:B) molar ratio in the sol–gel derived precursors. Sintering temperatures (850 and 1100°C) and sintering times (4 and 32 hours) also affected the phase composition and size of the nanowhiskers. Citric acid was also added in the sol–gel derived precursors as a surface stabilizer for obtaining uniform finely dispersed nanostructures. Fine nanowhiskers were obtained by the calcination at 850°C, whereas higher temperature of 1100°C led to thicker and longer nanowhiskers and became rod-like crystals. The morphology and phase composition were investigated by field emission scanning electron microscope and X-ray diffraction. Chemical bond vibrations in the synthesized nanowhiskers were investigated by Fourier-transform infrared spectroscopy.


Author(s):  
Jingjing Tian ◽  
Jun Qu ◽  
Lei Wan ◽  
Qiwu Zhang ◽  
Huimin Gao

In this study, Li-Al-OH layered double hydroxide (LDH), which was prepared by solvent-free one-step mechanochemical reaction of LiOH and Al(OH)3, was applied to remove boron from aqueous solution. Dry-grinding for 3 h at a rotational speed of 500 rpm, Li/Al molar 1/2 was the optimum condition to prepare highly crystalline of Li-Al LDH phase with no evident impure phases. Two milling products with Li/Al molar ratio at 1/2 and 2/2 were evaluated for boron adsorption. The results confirmed that Li/Al molar ratio 2/2 sample showed high boron adsorption capacity due to the physical adsorption of Li-Al-OH LDH and chemical synergism of phase gel Al(OH)3. The adsorption isotherms, described by the Langmuir model, indicated maximum monolayer boron uptake capacity 45.45 mg/g, implying competitive adsorption capacity of the material in our experiment.


2019 ◽  
Vol 59 ◽  
pp. 166-179 ◽  
Author(s):  
Betül Gürünlü ◽  
Mahmut Bayramoğlu

Graphene is one of the most promising materials discovered in last years. It is usually synthesized by Hummers’ method requiring the usage of many chemicals. As an alternative to traditional methods, in this study a bottom-up synthesis method was developed from various saccharides such as starch, mannose, cellulose, fructose, arabinose, and xylose by carbonization at 600 °C to 800 °C in LiCl/KCl molten salt system. The proposed method is environmental friendly and economic. Graphene yields at 600 °C are higher than at 800 °C. Graphene products give peak at 2θ = 23° on the X-Ray Diffraction (XRD) patterns. As the temperature is increased, amorph structure is observed on the XRD patterns. Raman spectroscopy results show that intensity of D band peak over intensity of G band peak (ID/IG) values of graphene products synthesized from arabinose and cellulose at 600 °C, graphene from arabinose synthesized at 800 °C are 0.76, 0.65 and 0.85 respectively, which show that these products are few-layered. According to X-ray photoelectron spectroscopy (XPS) results, graphene products synthesized at 600 °C have higher carbon content than those synthesized at 800 °C.


2019 ◽  
Vol 19 (11) ◽  
pp. 7436-7441
Author(s):  
Chu Zhang ◽  
Qi-Yu Wang ◽  
Ming-De Li ◽  
Guo-Dong Zhang

Sub-micrometer particles of β-Bi2O3 were successfully synthesized via a one-step self-propagating high-temperature synthesis (SHS) method for the first time. The experiments were carried out in the air at room temperature. The products were characterized by scanning electron microscope (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). In this study, three experiments were designed to optimize the heat source, Bi source and additive for the reaction system. Results showed that the system composed of Al, Bi2O3 and Al2O3 powders could synthesize monodisperse high-purity β-Bi2O3 spherical particles with the average diameter of 369 nm and the as-prepared products kept stable after being exposed in air for one month. Then, the influences of the ratio of the three components on system were investigated. Interestingly, it was found that a slight adjustment on the ratio of Al:Bi2O3:Al2O3 had significant effects on the reactions happening in a system. Specifically, when the amount of Al2O3 exceeds the molar ratio of 2:1:1 (Al:Bi2O3:Al2O3), it is difficult to ignite the reaction system; when the amount is less than 2:1:0.5, the reaction system becomes too violent to obtain pure products. However, there are no obvious differences on the morphology and structure of final products with the two ratios because of few changes in adiabatic temperature. Preparation of β-Bi2O3 by SHS technique enjoying many advantages, such as high efficiency, inexpensive experimental equipment and simple processes, would has a promising prospect for industrial application.


2010 ◽  
Vol 173 ◽  
pp. 78-83
Author(s):  
Kwee Yong Tan ◽  
Tan Kim Lee ◽  
Lim Kean Pah ◽  
Shaari Abdul Halim ◽  
Tan Kar Ban ◽  
...  

SiC added MgB2 polycrystalline samples were synthesized at low (650°C) and high (850°C) temperatures in order to study the sintering effect on the phase formation and superconducting properties. The MgB2 bulks with additions of 0wt%, 1wt%, 3wt% and 5wt% SiC were studied with powder X-ray diffraction technique. We observed that MgB2 remained as the primary phase for both sintering temperatures in all samples with the presence of MgO and Mg2Si as the main impurities. Some diffraction peaks associated with unreacted SiC is also noticeable. The relative intensity of the Mg2Si peaks was found to decrease in samples sintered at higher temperature. Temperature dependent magnetic moment measurements showed that the superconducting transition temperature, Tc decreases as the SiC addition level increases while lower sintering temperature degrades Tc to a greater extent. The changes in the physical properties is discussed based on the results of phase formation, full width half maximum (FWHM), lattice parameter and crystallite size.


2014 ◽  
Vol 938 ◽  
pp. 40-45 ◽  
Author(s):  
K.N. Porchelvi ◽  
S. Meenakshi ◽  
Kanniyan Pandian

We have synthesized metal phthalocyanine modified multiwalled carbon nanotube by a solid-phase synthesis method by heating a reaction mixture of phthalic anhydride, ammonium molybdate and MWCNT in a required molar ratio using muffle furnace. The metal phthalocyanine modified MWCNT samples collected and then washed extensively with various solvents to removal all impurities and unreacted starting materials. The resulting nanocomposite was characterized by IR, UV-Visible spectroscopy, Scanning Electron Microscopy, X-ray diffraction and Raman spectroscopy. The nanostructure of the CuPc/MWCNT assembly exhibits a homogeneous nanocomposite. The electrocatalytic study of the CuPc/MWCNT assembly towards the oxidation of nitrite was investigated. An enhanced oxidation peak current was noted with lowering oxidation over potential ranges. The proposed method can be applied for the amperometry detection of nitrite present in food samples.


Sign in / Sign up

Export Citation Format

Share Document