Zirconium Titanate: Synthesis and Processing of Fine Powders Prepared by Chemical Route

2006 ◽  
Vol 530-531 ◽  
pp. 683-688 ◽  
Author(s):  
Valter Ussui ◽  
Dolores Ribeiro Ricci Lazar ◽  
Nelson Batista de Lima ◽  
Ana Helena A. Bressiani ◽  
José Octavio A. Pascoal

A process for synthesis of fine zirconium titanate powders by chemical route is described. Zirconium/titanium molar ratio was varied from 0.67 to 1.5 and the powders produced were analyzed. The precipitation process comprises the mixture of zirconium and titanium metal salt solutions to ammonium hydroxide solution, followed by washing of the precipitate, calcination and grinding to result in zirconium titanate. The ceramic powder is then uniaxially pressed as cylindrical samples and sintered at 1400°C for 5 hours. The microstructure of fractured and thermally etched ceramic was observed by scanning electron microscopy, and crystal phase identifications were done by X-ray diffraction. At least two different zirconium titanate phases, ZrTiO4 and Zr5Ti7O24, were identified. Ceramic hardness was measured by Vickers indentation.

Author(s):  
Valter Ussui ◽  
Dolores R.R. Lazar ◽  
Nelson Batista de Lima ◽  
A.H.A. Bressiani ◽  
José Octavio A. Pascoal

2021 ◽  
Vol 3 (1) ◽  
pp. 8-11
Author(s):  
Yelmida Azis ◽  
Cory Dian Alfarisi ◽  
Komalasari Komalasari ◽  
Khairat Khairat ◽  
Yusnimar Sahan

Hydroxyapatite (HAp, Ca10(PO4)6(OH)2) is the most stable form of calcium phosphate and widely used in various medical applications, mainly in orthopedics and dentistry due to its close similarities with the inorganic mineral component of bone and teeth. This study aims to synthesize hydroxyapatite from duck eggshell using the precipitation method. The duck eggshell was calcined, hydrated (slaking) and underwent carbonation to form Precipitated Calcium Carbonate (PCC).  Afterwards, (NH4)2HPO4 was added to produce HAp by varying the molar ratio of Ca/P by 1.67, 1.77 and 1.87 and stirring speed by 200, 250, 300rpm under basic condition (pH 10 – 11). The best results were obtained at a molar ratio of 1.77 with 200rpm stirring speed. Furthermore, the X-ray Diffraction (XRD) analysis showed that its crystals were hexagonal with sizes of 23.062nm, in the absence of other crystalline phases. Therefore, the hydroxyapatite was obtained in the agglomerates form with a specific surface area of ??55.929m2/g.


2017 ◽  
Vol 76 (12) ◽  
pp. 3220-3226 ◽  
Author(s):  
Wenmin Cai ◽  
Jiajun Chen ◽  
Qingwei Wang ◽  
Meng Wei

Abstract Presently, the large amount of industrial leaded wastewater creates a great challenge to both environmental governance and wastewater recycling. Lead complexes in washed water must be removed mostly before the washed water can be recycled. This paper reports the mechanism and factors of removing Pb complexes in simulated washed water by the sulfide precipitation method. The reaction time, sodium sulfide dosage, pH, and polymeric aluminum chloride (PAC) dosage were analyzed and the optimal conditions were explored. The composition of the reaction products was also verified by scanning electron microscopy (SEM) and X-ray diffraction (XRD). Additionally, the kinetics of the precipitation reaction of sodium sulfide and Pb-EDTA were studied. These results showed that the Pb removal efficiency reached 91.7% under the optimal process conditions which were as follows: the dosages of Na2S and PAC were 188 mg/L (Na2S/Pb2+ molar ratio of 5:1) and 30 mg/L, respectively, the reaction time was 40 min, and the pH was 9. It was demonstrated using SEM and XRD that the reaction product in the separation process was PbS and the precipitation process was fitted to the following first-order reaction kinetics equation: Ct = 89.1e−0.1047t + 10.1 (R2 = 0.9929; Ct is Pb concentration at reaction time t).


Polymers ◽  
2019 ◽  
Vol 11 (7) ◽  
pp. 1224 ◽  
Author(s):  
Dalila Rocco ◽  
Alessandro Prescimone ◽  
Y. Klein ◽  
Dariusz Gawryluk ◽  
Edwin Constable ◽  
...  

The synthesis and characterization of 4′-(4-methoxyphenyl)-3,2′:6′,3″-terpyridine (2) (IUPAC PIN 24-(4-methoxyphenyl)-12,22:26,32-terpyridine) are described, and its coordination behaviour with cobalt(II) thiocyanate has been investigated. In a series of experiments, crystals were grown at room temperature by layering a MeOH solution of Co(NCS)2 over a CHCl3 solution of 2 using 1:1, 1:2 or 2:1 molar ratios of metal salt-to-ligand. Crystals harvested within 2–3 weeks proved to be the 1D-coordination polymer [Co(2)(NCS)2(MeOH)2]n and powder X-ray diffraction (PXRD) confirmed that the crystals selected for single-crystal X-ray diffraction were representative of the bulk samples. Longer crystallization times with a Co(NCS)2 to 2 molar ratio of 1:1 yielded crystals of [Co(2)(NCS)2(MeOH)2]n (1D-chain) and the pseudopolymorphs [{Co(2)2(NCS)2}·3MeOH]n and [{Co(2)2(NCS)2}·2.2CHCl3]n ((4,4)-nets), each type of crystal originating from a different zone in the crystallization tube. PXRD for this last experiment confirmed that the dominant product in the bulk sample was the 1D-coordination polymer.


Author(s):  
T. J. Beveridge

The Bacillus subtilis cell wall provides a protective sacculus about the vital constituents of the bacterium and consists of a collection of anionic hetero- and homopolymers which are mainly polysaccharidic. We recently demonstrated that unfixed walls were able to trap and retain substantial amounts of metal when suspended in aqueous metal salt solutions. These walls were briefly mixed with low concentration metal solutions (5mM for 10 min at 22°C), were well washed with deionized distilled water, and the quantity of metal uptake (atomic absorption and X-ray fluorescence), the type of staining response (electron scattering profile of thin-sections), and the crystallinity of the deposition product (X-ray diffraction of embedded specimens) determined.Since most biological material possesses little electron scattering ability electron microscopists have been forced to depend on heavy metal impregnation of the specimen before obtaining thin-section data. Our experience with these walls suggested that they may provide a suitable model system with which to study the sites of reaction for this metal deposition.


2000 ◽  
Vol 628 ◽  
Author(s):  
G. González ◽  
P. J. Retuert ◽  
S. Fuentes

ABSTRACTBlending the biopolymer chitosan (CHI) with poly (aminopropilsiloxane) oligomers (pAPS), and poly (ethylene oxide) (PEO) in the presence of lithium perchlorate lead to ion conducting products whose conductivity depends on the composition of the mixture. A ternary phase diagram for mixtures containing 0.2 M LiClO4 shows a zone in which the physical properties of the products - transparent, flexible, mechanically robust films - indicate a high degree of molecular compatibilization of the components. Comparison of these films with binary CHI-pAPS nanocomposites as well as the microscopic aspect, thermal behavior, and X-ray diffraction pattern of the product with the composition PEO/CHI/pAPS/LiClO4 1:0.5:0.6:0.2 molar ratio indicates that these films may be described as a layered nanocomposite. In this composite, lithium species coordinated by PEO and pAPS should be inserted into chitosan layers. Electrochemical impedance spectroscopy measurements indicate the films are pure ionic conductors with a maximal bulk conductivity of 1.7*10-5 Scm-1 at 40 °C and a sample-electrode interface capacitance of about 1.2*10-9 F.


2018 ◽  
Author(s):  
Tasneem Siddiquee ◽  
Abdul Goni

Chemical treatment of CoX<sub>2</sub><b><sup>. </sup></b>6H<sub>2</sub>O (X = Cl, Br, I) with the potentially tridentate PNP pincer ligand 2,6-bis(di-<i>tert</i>-butylphosphinomethyl)pyridine in 1:1 molar ratio results in cobalt(II) halide-PNP pincer complexes. The effect of the hydrated metal source on molecular structure and geometry of the complexes was studied by single crystal X-ray diffraction analysis. The complexes are neutral and the cobalt center adopts a penta-coordinate system with potential atropisomerization. Within the unit cell there are two distinct molecules per asymmetric unit. One of the two phosphorus atoms in the PNP ligand was observed to be partially oxidized to phosphinoxide. Disorder in the structure reflects a mixture of square pyramidal and distorted tetrahedral geometry.


2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Robert Christie

Abstract This paper presents an overview of the general chemical principles underlying the structures, synthesis and technical performance of azo pigments, the dominant chemical class of industrial organic pigments in the yellow, orange, and red shade areas, both numerically and in terms of tonnage manufactured. A description of the most significant historical features in this group of pigments is provided, starting from the discovery of the chemistry on which azo colorants are based by Griess in the mid-nineteenth century, through the commercial introduction of the most important classical azo pigments in the early twentieth century, including products known as the Hansa Yellows, β-naphthol reds, including metal salt pigments, and the diarylide yellows and oranges, to the development in the 1950s and 1960s of two classes of azo pigments that exhibit high performance, disazo condensation pigments and benzimidazolone-based azo pigments. A feature that complicates the description of the chemical structures of azo pigments is that they exist in the solid state as the ketohydrazone rather than the hydroxyazo form, in which they have been traditionally been illustrated. Numerous structural studies conducted over the years on an extensive range of azo pigments have demonstrated this feature. In this text, they are referred to throughout as azo (hydrazone) pigments. Since a common synthetic procedure is used in the manufacture of virtually all azo (hydrazone) pigments, this is discussed in some detail, including practical aspects. The procedure brings together two organic components as the fundamental starting materials, a diazo component and a coupling component. An important reason for the dominance of azo (hydrazone) pigments is that they are highly cost-effective. The syntheses generally involve low cost, commodity organic starting materials and are carried out in water as the reaction solvent, which offers obvious economic and environmental advantages. The versatility of the approach means that an immense number of products may be prepared, so that they have been adapted structurally to meet the requirements of many applications. On an industrial scale, the processes are straightforward, making use of simple, multi-purpose chemical plant. Azo pigments may be produced in virtually quantitative yields and the processes are carried out at or below ambient temperatures, thus presenting low energy requirements. Finally, provided that careful control of the reaction conditions is maintained, azo pigments may be prepared directly by an aqueous precipitation process that can optimise physical form, with control of particle size distribution, crystalline structure, and surface character. The applications of azo pigments are outlined, with more detail reserved for subsequent papers on individual products.


Catalysts ◽  
2021 ◽  
Vol 11 (3) ◽  
pp. 346
Author(s):  
Sonam Goyal ◽  
Maizatul Shima Shaharun ◽  
Ganaga Suriya Jayabal ◽  
Chong Fai Kait ◽  
Bawadi Abdullah ◽  
...  

A set of novel photocatalysts, i.e., copper-zirconia imidazolate (CuZrIm) frameworks, were synthesized using different zirconia molar ratios (i.e., 0.5, 1, and 1.5 mmol). The photoreduction process of CO2 to methanol in a continuous-flow stirred photoreactor at pressure and temperature of 1 atm and 25 °C, respectively, was studied. The physicochemical properties of the synthesized catalysts were studied using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and photoluminescence (PL) spectroscopy. The highest methanol activity of 818.59 µmol/L.g was recorded when the CuZrIm1 catalyst with Cu/Zr/Im/NH4OH molar ratio of 2:1:4:2 (mmol/mmol/mmol/M) was employed. The enhanced yield is attributed to the presence of Cu2+ oxidation state and the uniformly dispersed active metals. The response surface methodology (RSM) was used to optimize the reaction parameters. The predicted results agreed well with the experimental ones with the correlation coefficient (R2) of 0.99. The optimization results showed that the highest methanol activity of 1054 µmol/L.g was recorded when the optimum parameters were employed, i.e., stirring rate (540 rpm), intensity of light (275 W/m2) and photocatalyst loading (1.3 g/L). The redox potential value for the CuZrIm1 shows that the reduction potential is −1.70 V and the oxidation potential is +1.28 V for the photoreduction of CO2 to methanol. The current work has established the potential utilization of the imidazolate framework as catalyst support for the photoreduction of CO2 to methanol.


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.


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