scholarly journals Air-Flow Impacting: A New Mechanochemical Method for Continuous, Highly Efficient, Large-Scale Synthesis of Metal–Organic Frameworks and Mechanistic Research

2021 ◽  
Vol 8 ◽  
Author(s):  
Jun Zhao

The novel air-flow impacting (AFI) synthesis technology for mechanochemical synthesis of MOFs (ZIF-67) was first reported. AFI was an improvement of the traditional mechanochemical synthesis method. The results indicated that ZIF-67 was successfully synthesized after 30 min at a rate of 60 kg h−1. The as-prepared ZIF-67 was characterized by Fourier transform infrared spectroscopy (FT-IR), powder x-ray diffraction (P-XRD), thermogravimetric analysis (DTA/TG), scanning electron microscope (SEM), transmission electron microscope (TEM), and single-crystal x-ray diffraction. The kinetic analysis of the reaction mechanism was carried out by detecting the P-XRD patterns of the products with different reaction times. The synthesis belonged to the one-dimensional diffusion-controlled model.

2021 ◽  
Vol 116 ◽  
pp. 5-14
Author(s):  
Marta Babicka ◽  
Magdalena Woźniak ◽  
Kinga Szentner ◽  
Sławomir Borysiak ◽  
Krzysztof Dwiecki ◽  
...  

The aim of this study was to compare parameters of nanocellulose obtained by two different procedures: hydrolysis with ionic liquids (1-allyl-3-methylimidazolium chloride and 1-ethyl-3-methylimidazolium acetate) and hydrolysis with ionic liquids in combination with hydrolysis using a cellulolytic enzyme from Trichoderma reesei. Avicel cellulose was treated with two ionic liquids: 1-allyl-3-methylimidazolium chloride (AmimCl) and 1-ethyl 3-methylimidazolium acetate (EmimOAc). In the two-step hydrolysis cellulose after treatment with ionic liquids was additionally hydrolyzed with a solution of enzymes. In order to characterize the obtained material, the following analyses were used: infrared spectroscopy, X-ray diffraction and dynamic light scattering. The results indicated that cellulose obtained by two-step nanocellulose production methods (first hydrolysis with ionic liquids and then with enzymes) showed similar parameters (particle size, XRD patterns and degree of crystallinity) as the material after the one-step process, i.e. hydrolysis with ionic liquids.


2020 ◽  
Vol 15 (2) ◽  
pp. 348-366 ◽  
Author(s):  
Ke Chen ◽  
Guangzu He ◽  
Qiong Tang ◽  
Qahtan A.Yousif

The SCMNPs@BPy-SO3H catalyst was prepared and characterized using Fourier Transform Infrared Spectroscopy (FTIR), Thermogravimetric Analysis (TGA), Vibrating Sample Magnetometry (VSM), Energy Dispersive X-ray Spectroscopy (EDX), X-ray Diffraction (XRD), and Scanning Electron Microscopy (SEM). Afterwards, its capability was efficiently used to promote the one-pot, three-component synthesis of pyrano[2,3-c]pyrazole and 2-amino-3-cyano-pyrano[3,2-c]chromen-5(4H)-one derivatives. The strategy resulted in the desired products with excellent yields and short reaction times. The SCMNPs@BPy-SO3H catalyst was readily recovered using a permanent magnetic field and it was reused in six runs with a slight decrease in catalytic activity. Copyright © 2020 BCREC Group. All rights reserved 


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.


2011 ◽  
Vol 2011 ◽  
pp. 1-8 ◽  
Author(s):  
Pingting He ◽  
Jie Tao ◽  
Jianjun Xue ◽  
Yulan Chen

A homogeneous and transparent titania (TiO2) sol with nanosized anatase TiO2particles was prepared by hydrothermal synthesis method. The transmission electron microscope and X-ray diffraction were used to characterize the structure and morphology of particulates in the TiO2sol and purchased TiO2powder. The results show that the homogeneous anatase crystalline phase was formed and the size of the spindle-like particle in sol was about 20 nm in width and 150 nm in average length, and the particulates of the purchased powder were globular-like about 50 nm in diameter. In addition, a consistent set of in vitro experimental protocols was used to study the effects of nano-TiO2sol as prepared and nano-TiO2powder on mouse peritoneal macrophage. The cytotoxicity tests in vitro indicate that, with the increasing of TiO2sol concentration contaminated with the cells, the relative proliferation rate of macrophage cells was improved slightly after the cells contaminated for 24 h, but it reduced rapidly after contaminated for 48 h. The purchased nano-TiO2powder inhibited the growth of the cells obviously as cultivating with macrophage both for 24 h and 48 h.


2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Yang Liu ◽  
Yang Jiao ◽  
Fengyu Qu ◽  
Lihong Gong ◽  
Xiang Wu

Large scale SnO2nanotubes are successfully obtained by a facile hydrothermal method at a mild temperature. The morphologies and the microstructures of the as-synthesized SnO2products are characterized by scanning electron microscope (SEM) and transmission electron microscope (TEM). The average diameter of the nanotubes is about 100 nm. The phase and composition of the as-obtained products are investigated by X-ray diffraction (XRD). A series of comparison experiments were conducted by varying the experimental parameters, such as temperature, time, and the amount of the alkali, to study the formation mechanism of SnO2nanotubes.


2007 ◽  
Vol 22 (10) ◽  
pp. 2838-2844 ◽  
Author(s):  
B.J. Park ◽  
W.B. Im ◽  
W.J. Chung ◽  
H.S. Seo ◽  
J.T. Ahn ◽  
...  

ZnS:Mn2+ phosphors were synthesized by a modified solid-state reaction method. In the synthesis method, a sealed vessel is used, where heat and pressure are simultaneously utilized. The effects of various synthesis conditions such as temperature, Mn concentration, and pressure on the cathodoluminescence (CL) were investigated. Among them, pressure had an effect on CL property as much as others. It was observed that CL intensities of ZnS:Mn2+ phosphors increased with the increase of pressure and the best sample showed higher intensity than that of a commercial one by 180%. X-ray diffraction (XRD) and electron paramagnetic-resonance (EPR) were used to understand the enhancement. No change of XRD patterns was observed but the full width at half-maximum (FWHM) of the most intense cubic (111) peak of ZnS:Mn2+ decreased with the increase of pressure. EPR signal intensity of Mn2+ increased with the increase of pressure. The improved crystallinity and more substitution of Zn2+ with Mn metal were believed to be responsible for the enhancement.


2011 ◽  
Vol 391-392 ◽  
pp. 935-939
Author(s):  
Ning Li ◽  
Bo Rong Wu ◽  
Chuan Xiong Zhou ◽  
Yong Huan Ren ◽  
Chun Wei Yang ◽  
...  

The doped and undoped LiFePO4/C samples are prepared by two-step solid-state reaction. The X Ray Diffraction (XRD) results indicate that metal ions are successfully doped in LiFePO4 without any unexpected phase. The Scanning Electron Microscope (SEM) shows that the particle morphologies of samples are near-spherical with about 200-300nm size which can be observed in all samples. The electrochemical tests indicate that doping oversize ions will increase electrode polarization. The limitation of the Li+ migration is intensified by doping metal ions with high valence. LiFePO4/C samples doped with Mn2+ and Ti4+behave better at low temperature, especially the one doped with Ti4+. Battery with this Ti4+doped material can yield 77mAhg-1 when discharge at -20°C and 0.5C, about 26mAhg-1 higher than the undoped one.


2012 ◽  
Vol 506 ◽  
pp. 94-97 ◽  
Author(s):  
M. Sutapun ◽  
B. Boonchom ◽  
Naratip Vittayakorn

Zn3(PO4)2.4H2O, which is an important component of biomedical zinc phosphate cement, was synthesized from an aqueous solution of zinc oxide and orthophosphoric acid by the sonochemical method. This synthesis method yielded best results with respect to high purity and crystallinity. Structural characteristics of the compound were investigated by X-ray diffraction (XRD), Fourier transform infrared (FT-IR) and scanning electron microscopy (SEM). FT-IR spectra indicated the presences of different crystallographic PO43ion and H2O molecules for the Zn3(PO4)2.4H2O and Zn3(PO4)2structures. The resulting XRD patterns showed the purity phases of orthorhombic Zn3(PO4)2.4H2O and the monoclinic for its final decomposed Zn3(PO4)2product. The thermal stability, crystallite size, and plate-like microparticles of Zn3(PO4)2.4H2O and Zn3(PO4)2are different in this work from those in previous reports, which may be caused by the starting reagents and reaction condition for the sonochemical method.


2013 ◽  
Vol 2013 ◽  
pp. 1-4 ◽  
Author(s):  
Jing Wang ◽  
Yang Jiao ◽  
Yang Liu ◽  
Zhenglin Zhang ◽  
Fengyu Qu ◽  
...  

We showed large-scale synthesis of ZnS nanobelts by simply thermal evaporation of ZnS powder in the presence of Au catalysts at 1020°C. Scanning electron microscope (SEM), transmission electron microscope (TEM), and X-ray diffraction (XRD) analyses demonstrated that the as-obtained ZnS nanobelts possess hexagonal wurtzite structures. The nanobelts have lengths ranging from tens to hundreds of micrometers, thicknesses of tens of nanometers, and widths ranging from hundreds of nanometers to the order of micrometers. The growth process was proposed on the basis of known vapor-liquid-solid (VLS) mechanism. Room temperature photoluminescence measurements showed that the as-synthesized ZnS nanostructures had a strong green emission bands at a wavelength of 427 nm, which can be attributed to deep-level emissions induced by defects or impurities.


2015 ◽  
Vol 1087 ◽  
pp. 329-333
Author(s):  
Sharifah Adzila ◽  
S. Ramesh ◽  
I. Sopyan ◽  
Mohd Hamdi Abdul Shukor

The mechanochemical synthesis method was employed to synthesis hydroxyapatite (HA) and magnesium (Mg) doped hydroxyapatite (HA) powders. The effects of Mg2+ into the synthesized HA powder properties were investigated. Characterization of the synthesized HA (Mg-free HA) and Mg–doped HA at various concentrations (1% - 9% MgHA) were accomplished through X-ray diffraction (XRD) and Fourier transform infrared (FTIR) analyses. The nano size powder of HA and Mg-doped HA were successfully synthesized through the present method and the influenced of Mg2+ in the HA was also indicated by the different peaks intensity and the crystal sizes obtained.


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