Hydrotalcites with heterogeneous anion distributions: a first approach to producing new materials to be used as vehicles for the successive delivery of compounds

Clay Minerals ◽  
2020 ◽  
Vol 55 (1) ◽  
pp. 31-39 ◽  
Author(s):  
Franchescoli D. Velázquez-Herrera ◽  
Geolar Fetter
Keyword(s):  
Microwave Irradiation ◽  
Divalent Cation ◽  
New Materials ◽  
X Ray Diffraction ◽  
X Ray ◽  
Synthesis Parameters ◽  
Crystallization Method ◽  
Anion Distribution

ABSTRACTHydrotalcites with heterogeneous distributions of anions between their layers were synthesized. Some synthesis parameters were studied to verify their influence on the anionic segregation properties of the hydrotalcites. The nature of the divalent cation and the crystallization method were most relevant. Zinc, in contrast to magnesium, assisted in discriminating carbonates and attracting nitrates to form hydrotalcites with heterogeneous distributions using microwave irradiation. Furthermore, the identification of this kind of hydrotalcite could be easily verified by determining the presence of a double reflection in the 003 X-ray diffraction (XRD) maximum, which definitively characterized a heterogeneous anion distribution. Finally, the reason as to why in some cases the hydrotalcite presented two reflections in the 003 XRD peak was elucidated.

Synthesis of SBA-15/MCM-41 bimodal mesoporous silica

2016 ◽  
Vol 1817 ◽  
Author(s):  
Leyla Y. Jaramillo ◽  
Wilson A. Henao ◽  
Elizabeth Pabón-Gelves
Keyword(s):  
Mesoporous Silica ◽  
Textural Properties ◽  
New Materials ◽  
X Ray Diffraction ◽  
Main Interest ◽  
Structure Directing Agent ◽  
X Ray ◽  
Synthesis Parameters ◽  
Nanostructured Silica ◽  
Mcm 41

ABSTRACTNanostructured silica materials with different morphologies and adjustable pore size have been studied by researches worldwide for several applications such as catalysis, separation, adsorption, and templates for new materials. The main interest in the development of these materials is to obtain a structure with a specific combination of pore sizes for a particular application. The morphology and textural properties of pores can be easily changed with the modification of the synthesis parameters, among these, the choice of surfactant or structure directing agent (SDA).Accordingly, in this work, three types of nanostructured silica with different mesoporosity were synthesized by using of CTAB and Pluronic 123 as structure directing agents: SBA-15 and MCM-41 unimodal mesoporous silica and SBA-15/MCM-41 bimodal mesoporous silica.To evaluate the effect of surfactant on the morphology and textural properties of pores, the materials were characterized by scanning electron microscopy (SEM), X-ray Diffraction (XRD) and nitrogen sorption (BET).

scholarly journals MSMEG_6292, a Mycobacterium smegmatis RNA polymerase secondary channel-binding protein: purification, crystallization and X-ray diffraction analysis

2018 ◽  
Vol 74 (9) ◽  
pp. 543-548
Author(s):  
Abyson Joseph ◽  
Valakunja Nagaraja ◽  
Ramanathan Natesh
Keyword(s):  
Rna Polymerase ◽  
Mycobacterium Smegmatis ◽  
Transcriptional Activity ◽  
Molecular Replacement ◽  
X Ray Diffraction ◽  
Secondary Channel ◽  
X Ray ◽  
Cell Parameters ◽  
Crystallization Method ◽  
Better Than

The transcriptional activity of RNA polymerase (RNAP) is controlled by a diverse set of regulatory factors. A subset of these regulators modulate the activity of RNAP through its secondary channel. Gre factors reactivate stalled elongation complexes by enhancing the intrinsic cleavage activity of RNAP. In the present study, the protein MSMEG_6292, a Gre-factor homologue from Mycobacterium smegmatis, was expressed heterologously in Escherichia coli and purified using standard chromatographic techniques. The hanging-drop vapour-diffusion crystallization method yielded diffraction-quality crystals. The crystals belonged to the trigonal space group P3121 (or its enantiomorph P3221), with unit-cell parameters a = b = 83.15, c = 107.07 Å, α = β = 90, γ = 120°. The crystals diffracted to better than 3.0 Å resolution. Molecular-replacement attempts did not yield any phasing models; hence, platinum derivatization was carried out with K2PtCl4 and derivative data were collected to 3.4 Å resolution.

Microwave-assisted solvent-free synthesis and spectral and structural characterization of cyclotriphosphazene hexakis(o-tolylamide)

2018 ◽  
Vol 73 (12) ◽  
pp. 999-1003 ◽  
Author(s):  
Mohammad Hakimi ◽  
Homeyra Rezaei ◽  
Keyvan Moeini ◽  
Heidar Raissi ◽  
Vaclav Eigner ◽  
...  
Keyword(s):  
Nmr Spectroscopy ◽  
Microwave Irradiation ◽  
Stacking Interactions ◽  
X Ray Diffraction ◽  
Aromatic Rings ◽  
X Ray ◽  
Microwave Assisted ◽  
Ft Ir ◽  
Solvent Free Synthesis

AbstractA new cyclotriphosphazene, 2,2,4,4,6,6-hexakis (o-tolylamono)-1,3,5,2λ5,4λ5,6λ5-triazatriphosphinine (MPAP), was prepared using microwave irradiation and identified by elemental analysis, FT-IR, Raman, 31P NMR spectroscopy, and single-crystal X-ray diffraction. In the crystal, in addition to hydrogen bonds, the network is further stabilized by inter- and intramolecular π–π stacking interactions between aromatic rings.

scholarly journals Portland clinker with civil construction waste: influence of pellet geometry on the formation of crystalline phases

2020 ◽  
Vol 20 (4) ◽  
pp. 205-223
Author(s):  
Fernanda Nepomuceno Costa ◽  
Daniel Véras Ribeiro ◽  
Cléber Marcos Ribeiro Dias
Keyword(s):  
Sustainable Development ◽  
Portland Cement ◽  
Rietveld Method ◽  
Industrial Process ◽  
3D Printer ◽  
New Materials ◽  
X Ray Diffraction ◽  
Construction Waste ◽  
X Ray ◽  
Portland Cement Association

Abstract Efforts to reduce greenhouse gas emissions in the context of sustainable development have intensified, with the development of research aimed at the production of new materials and binders for construction. This article analyzes the influence of pellet geometry in the production of clinkers, with the incorporation of construction waste (CCW). Procedures adapted from the method proposed by Brazilian Portland Cement Association were adopted in studies of laboratory clinkers, in an attempt to simulate the stages of the industrial process. Pellets were prepared with the same formulation, however, with four different geometries: spherical, with diameters of 1 cm, 2 cm and 3 cm, with manual molding, and semi-spherical, with a diameter of 2 cm, using molds of PLA (polylactic acid) printed on a 3D printer to facilitate the molding of the clinkers in a standardized way. Clinkers were characterized mineralogically by x-ray diffraction (XRD) and the Rietveld method was used to quantify the phases. Variations in the quantities of the alite and belite phases were observed depending on the geometry of the pellets, although the same calcination conditions were used. This is probably due to the variation in the surface area (exposure area) and the gradients of the cooling rate.

Metal-Controlled Assembly Tuning Coordination Polymers with Flexible 2-(1H-imidazole-1-yl)acetic Acid (Hima)

2006 ◽  
Vol 59 (9) ◽  
pp. 647 ◽  
Author(s):  
Yong-Tao Wang ◽  
Gui-Mei Tang ◽  
Da-Wei Qin
Keyword(s):  
Coordination Polymers ◽  
Weak Interactions ◽  
Critical Role ◽  
Three Dimensional ◽  
Supramolecular Network ◽  
Water Medium ◽  
New Materials ◽  
X Ray Diffraction ◽  
X Ray ◽  
Supramolecular Networks

Three new inorganic–organic coordination polymers based on a versatile linking unit 2-(1H-imidazole-1-yl)acetate (Hima) and divalent Mn(ii), Ni(ii), and Cu(ii) ions, exhibiting two kinds of two dimensionalities with different topological structures, have been prepared in water medium and structurally characterized by single-crystal X-ray diffraction analysis. Reaction of MnCl2·4H2O and Ni(NO3)2·6H2O with Hima yielded neutral two-dimensional (2D) coordination polymers [M(ima)2]n, M = Mn(ii) 1, and Ni(ii) 2 with isostructural 2D coordination polymers possessing (3,6) topology structures, which further stack into three-dimensional (3D) supramolecular networks through C–H···O weak interactions. However, when Cu(NO3)2·4H2O was used, a neutral 2D coordination polymer [Cu(ima)2]n 3 consisting of rhombus units was generated, which showed a 3D supramolecular network through C–H···O weak interactions. Among these polymers, the building block ima anion exhibits different coordination modes. These results indicate that the versatile nature of this flexible ligand, together with the coordination preferences of the metal ions, plays a critical role in construction of these novel coordination polymers. Spectral and thermal properties of these new materials have also been investigated.

scholarly journals Valorization of Brick and Glass CDWs for the Development of Geopolymers Containing More Than 80% of Wastes

Minerals ◽  
2020 ◽  
Vol 10 (8) ◽  
pp. 672
Author(s):  
Dimitris Kioupis ◽  
Aggeliki Skaropoulou ◽  
Sotirios Tsivilis ◽  
Glikeria Kakali
Keyword(s):  
Electron Microscopy ◽  
Compressive Strength ◽  
Circular Economy ◽  
X Ray Diffraction ◽  
Glass Waste ◽  
X Ray ◽  
Optimum Synthesis ◽  
Synthesis Parameters ◽  
Construction And Demolition Wastes ◽  
Scanning Electron

One of the areas of priority in a circular economy, regarding waste management, regards the valorization of construction and demolition wastes (CDW). This study suggests the synthesis of geopolymeric binders based almost entirely on construction and demolition wastes. Ceramic waste was used as the aluminosilicate precursor of the geopolymer synthesis, while glass waste was applied in the preparation of the activation solution. A fractional experimental design defined the optimum synthesis parameters, based on compressive strength values. The final products were characterized by means of X-Ray Diffraction (XRD), Fourier-Transform Infrared Spectroscopy (FTIR) and Scanning Electron Microscopy (SEM). The glass waste was appropriately processed in order to prepare the activation solution for the geopolymerization of brick waste. In this work, CDW-based geopolymers were produced with a compressive strength in the range 10–44 MPa. The developed products contained 80–90 wt.% CDWs, depending on the method of activator preparation.

Catalytic Performance of Copper-Substituted Polyoxotungstate Materials and X-Ray Structure of a New Sandwich-Type Compound

2008 ◽  
Vol 587-588 ◽  
pp. 538-542 ◽  
Author(s):  
Salete S. Balula ◽  
Luís Cunha-Silva ◽  
Isabel C.M.S. Santos ◽  
Filipe A. Almeida Paz ◽  
João Rocha ◽  
...  
Keyword(s):  
Potassium Salt ◽  
Room Temperature ◽  
High Selectivity ◽  
Catalytic Performance ◽  
New Materials ◽  
X Ray Diffraction ◽  
Good Efficiency ◽  
X Ray ◽  
Sandwich Type ◽  
Copper Centre

Mono-substituted and sandwich-type copper substituted polyoxoanions ([PW11CuO39]5− and [Cu4(H2O)2(PW9O34)2]10−) were studied as catalysts for the epoxidation of cyclooctene and geraniol, using the green oxidant H2O2, with the results suggesting good efficiency at room temperature. High selectivity and reasonable conversion data were found after the first minutes of reaction. The copper centre may be responsible for this performance and our on-going research focuses in the preparation of new materials incorporating copper into polyoxometalates (POMs). In this context, we have also isolated a new crystalline dimeric sandwich-type polyoxocoppertungstate {H7.05[Cu3WO(H2O)(CuW9O34)(Cu0.6W9O34)]}7.75−. This compound was isolated as potassium salt and structurally characterized by FTIR and single-crystal X-ray diffraction (XRD). The polyoxoanion is composed by the [CuW9O34]12− and [Cu0.6W9O34]12.8− anionic fragments, joined together by a rhomb-like arrangement of three Cu2+ and one W6+ metallic centres, all exhibiting octahedral coordination geometries.

scholarly journals Electrochemical deposition of coatings of highly entropic alloys from non-aqueous solutions

2016 ◽  
Vol 60 (1) ◽  
pp. 6-12 ◽  
Author(s):  
V. Jeníček ◽  
L. Diblíková ◽  
M. Bláhová
Keyword(s):  
Aqueous Solutions ◽  
Electrochemical Deposition ◽  
Absorption Spectrometry ◽  
New Materials ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Electrochemical Coating ◽  
First Results ◽  
Combination Of Methods

Abstract The paper deals with electrochemical deposition of coatings of highly entropic alloys. These relatively new materials have been recently intensively studied. The paper describes the first results of electrochemical coating with highly entropic alloys by deposition from non-aqueous solutions. An electrochemical device was designed and coatings were deposited. The coatings were characterised with electronic microscopy scanning, atomic absorption spectrometry and X-ray diffraction methods and the combination of methods of thermic analysis of differential scanning calorimetry and thermogravimetry.

Microwave irradiation used for all steps of pre-pillaring Al-montmorillonite

Clay Minerals ◽  
2009 ◽  
Vol 44 (2) ◽  
pp. 267-278 ◽  
Author(s):  
S. Yapar ◽  
R. M. Torres Sánchez ◽  
M. Emreol ◽  
P. Weidler ◽  
K. Emmerich
Keyword(s):  
Microwave Irradiation ◽  
Physicochemical Properties ◽  
Structural Changes ◽  
Thermal Analyses ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ageing Processes ◽  
Pillared Montmorillonites ◽  
Scanning Electron ◽  
Sem Analyses

AbstractIn this study, a new procedure for the synthesis of pillared clays is proposed. Ageing processes and intercalation reactions were carried out using microwave irradiation in order to decrease the consumption of three industrially-important parameters; time, water consumption and energy. The effects of microwave irradiation, the amount of Al and the Al3+/clay ratio on the physicochemical properties of Al-pillared montmorillonites were investigated. The structural changes, depending on the intercalation and microwave irradiation, were characterized using X-ray diffraction (XRD), Fourier-transform infrared (FTIR) and scanning electron microscopy (SEM) analyses and by measuring the specific surface area and pore-size distribution. Additionally, simultaneous thermal analyses (STA) and zeta potential measurements were carried out to determine physicochemical properties. According to the XRD measurements, the d001 value of microwave-irradiated samples is not affected by the amount of Al and the Al3+/clay ratio; microwave irradiation causes a 0.20 nm contraction in the d001 value in comparison to that of a conventionally pillared sample. The results of FTIR analyses reveal that the intensity of peaks assigned to Keggin-OH and Keggin-H2O stretches is diminished in the case of microwave-irradiated samples. The STA analyses indicate that the amount of water released during dehydroxylation is decreased in the case of microwave-irradiated samples. By considering the contraction in d001 values and the decreases in Keggin-stretching bands and also in the amount of dehydroxylation water, it was concluded that microwave irradiation has a calcination effect.

Copper-Indium-Boron-Diselenide Absorber Materials

2007 ◽  
Vol 1012 ◽  
Author(s):  
Natale J. Ianno ◽  
Rodney J. Soukup ◽  
Tobin Santero ◽  
Chad Kamler ◽  
James Huguenin-Love ◽  
...  
Keyword(s):  
Thin Film ◽  
Spectroscopic Analysis ◽  
New Materials ◽  
X Ray Diffraction ◽  
X Ray ◽  
Copper Indium

AbstractAttempts to fabricate new CuIn1-xBxSe2 (CIBS) and CuBSe2 (CBS) thin-film materials have been complicated by the formation of interfering crystallites and by the loss of boron from the magnetron sputtered precursor alloys during the selenization and annealing processes. Raman and Auger spectroscopic analysis as well as x-ray diffraction studies show that the formation of boron selenide may be contributing to the difficulty in creating these new materials.

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