scholarly journals An accelerated and effective synthesis of zinc borate from zinc sulfate using sonochemistry

2020 ◽  
Vol 43 (1) ◽  
pp. 7-14
Author(s):  
Ali Can Ersan ◽  
Azmi Seyhun Kipcak ◽  
Meral Yildirim Ozen ◽  
Nurcan Tugrul
Keyword(s):  
Inorganic Compounds ◽  
Zinc Borate ◽  
High Yield ◽  
X Ray Diffraction ◽  
Ultrasonic Probe ◽  
Minimum Particle Size ◽  
Effective Synthesis ◽  
Ft Ir ◽  
Lower Temperature ◽  
Borate Compound

AbstractRecently, sonochemistry has been used for the synthesis of inorganic compounds, such as zinc borates. In this study using zinc sulphate heptahydrate (ZnSO4·7H2O) and boric acid (H3BO3) as starting materials, a zinc borate compound in the form of Zn3B6O12·3.5H2O was synthesized using an ultrasonic probe. Product’s characterization was carried out with using X-ray diffraction (XRD), Scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR) and Raman spectroscopy. Zinc borate compound’s chemical bond structure was observed with Raman and FTIR. From the XRD results it was seen that Zn3B6O12·3.5H2O can be quickly synthesized upon heating at 80°C and 85°C (55 min) or 90°C (45 min) in very high yield (>90%). The minimum particle size obtained was ~143 μm from the SEM results. Zinc borate compound was synthesized at a lower temperature in less time than other synthesized zinc metal compound in literature.

Ultrasonic-Assisted Synthesis of Zinc Borates: Effect of Boron Sources

2020 ◽  
Vol 42 (6) ◽  
pp. 839-839
Author(s):  
Fatma Tugce Senberber Dumanli Fatma Tugce Senberber Dumanli ◽  
Azmi Seyhun Kipcak Azmi Seyhun Kipcak ◽  
Duygu Sena Vardar and Nurcan Tugrul Duygu Sena Vardar and Nurcan Tugrul
Keyword(s):  
Raw Materials ◽  
Inorganic Compounds ◽  
Zinc Borate ◽  
X Ray Diffraction ◽  
Ultrasonic Probe ◽  
Total Mass Loss ◽  
Minimum Particle Size ◽  
Ir And Raman Spectroscopies ◽  
Ultrasonic Assisted ◽  
Ft Ir

Sonochemistry meaning ultrasound-assisted chemistry plays an important role in the synthesis of inorganic compounds. Among these inorganic compounds, zinc borates are used for the flame-retarding agent. In this study using zinc chloride (ZnCl2), boric acid (H3BO3), Na2B4O7and#183;10H2O, Na2B4O7and#183;5H2O and NaOH as raw materials, a zinc borate compound in the formulae of Zn3B6O12and#183;3.5H2O was obtained using an ultrasonic probe. Crystal structures of samples were identified using X-ray diffraction (XRD). The symmetric and asymmetric stretching between boron and oxygen atoms were searched by Fourier-transform infrared (FT-IR) and Raman spectroscopies. The effects of boron sources on sample morphology were examined by scanning electron microscopy (SEM). From the results, it was seen that Zn3B6O12and#183;3.5H2O can easily be produced from these raw materials with the synthesis parameters of 80-90and#176;C and 40-55 min. From the SEM results, it was seen that the minimum particle size obtained was 172 nm. Reaction efficiencies were calculated between 79.6 and 94.0 and#177; 0.5%. Thermal feature of the obtained pure phase, investigated with the thermogravimetric analyses. The dehydration of the synthesized Zn3B6O12and#183;3.5H2O was seen between 262 and 413and#176;C with a total mass loss of 13.25%.

scholarly journals Carbothermal Reduction Nitridation of Fly Ash, Diatomite and Raw Illite: Formation of Nitride Powders with Different Morphology and Photoluminescence Properties

Crystals ◽  
2020 ◽  
Vol 10 (5) ◽  
pp. 409
Author(s):  
Kuizhou Dou ◽  
Yinshan Jiang ◽  
Bing Xue ◽  
Cundi Wei ◽  
Fangfei Li
Keyword(s):  
Fly Ash ◽  
Alkali Metals ◽  
Blue Shift ◽  
Pulverized Coal ◽  
Photoluminescence Properties ◽  
X Ray Diffraction ◽  
Nitridation Process ◽  
Ft Ir ◽  
Lower Temperature ◽  
Rare Earth Doped

Rare-earth-doped SiAlON and Si3N4 materials from aluminosilicate starting materials have been reported to show superior photoluminescence (PL) properties. Three different starting materials, including pulverized coal furnace fly ash, diatomite and raw illite, were used for synthesis of nitride materials. The phase and morphology evolution of these products were carefully monitored at the low temperature range of 1350 °C to 1450 °C by X-ray diffraction (XRD), scanning electronic microscopy (SEM) and Fourier-transform infrared spectroscopy (FT-IR). The PL properties of Eu-doped nitride products were also comparatively characterized. The results show that the type of starting material affects the phase composition and the photoluminescence properties of products. The existence of aluminum and alkali metals could effectively promote nitridation reactions. Aluminum in the starting materials led to the formation of different aluminum-rich nitride phases. Thus, β-SiAlON could be achieved at a much lower temperature (1350 °C) using raw illite or fly ash containing the proper amount of aluminum. Additionally, excess aluminum led to the formation of corundum and 15R-SiAlON. The products from pulverized coal furnace fly ash had more prismatic particles, and the products from diatomite had more fibrous particles. With the progress of the nitridation process, the fibers were increased, becoming longer and straighter, and the prismatic particles were more obvious. The presence of aluminum in the starting materials led to a blue shift in the photoluminescence spectrum.

Synthesis of Biodegradable Composite for Knee Cartilage Prosthesis Joint

2012 ◽  
Vol 1376 ◽  
Author(s):  
J.C. Pérez-Reyes ◽  
G. Carbajal-De la Torre ◽  
M. A. Espinosa-Medina ◽  
L. A. Ibarra-Bracamontes ◽  
M. Villagómez-Galindo ◽  
...  
Keyword(s):  
Composite Materials ◽  
Calcium Phosphates ◽  
Inorganic Compounds ◽  
X Ray Diffraction ◽  
Biodegradable Composite ◽  
Hard Particles ◽  
Biological Implants ◽  
Ft Ir ◽  
Degradation Time

ABSTRACTOsteoarthritis is a very complex illness of the joints that affects cartilage and subcondral bone. At the last years, researching has been focused in the development and characterization of composite materials, evaluating their structural properties. Some o those composite materials are constituted by organic and inorganic compounds forming hybrids. These materials can improve their properties due to the interaction of reinforcement hard particles in the polymeric matrix. The interest on the composite biomaterials has been increased on the biomedical applications such as tissue regenerating based in synthetic polymers with biodegradable and biocompatible properties whose can be reinforced by calcium phosphates. In this sense, hydroxyapatite [Ca10(PO4)6(OH)2] is often used for biological implants due its mineral phase similitude with bone microstructure and tissue compatibility. Similarly, polylactic acid (PLA) is a used polymer for implant applications due physicochemical and biocompatibility properties, and short degradation time also. In order to obtain a composite that can be used as a regenerating material on the osteoarthritis problem, in this work a (90/10 wt.%) polylactic/hydroxyapatite hybrid composite was produced by chemical synthesis and characterized by X-ray diffraction, SEM, FT-IR and TGA/DSC techniques.

scholarly journals Synthesis of pyrroles catalyzed by MIL-53(Al) via Paal-Knorr reaction under mild condition

2018 ◽  
Vol 1 (T5) ◽  
pp. 116-125
Author(s):  
Hai Truong Nguyen ◽  
Phuong Hoang Tran
Keyword(s):  
Catalytic Activity ◽  
Metal Organic Framework ◽  
Organic Ligand ◽  
Molar Ratio ◽  
High Yield ◽  
X Ray Diffraction ◽  
Benzenedicarboxylic Acid ◽  
Metal Organic ◽  
Ft Ir ◽  
Good Catalytic Activity

Metal-organic framework MIL-53(Al) was synthesized by a solvothermal method using aluminium nitrate as the aluminium source and 1,4- benzenedicarboxylic acid (H2BDC) as the organic ligand. The structure of MIL-53(Al) was characterized by X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). The catalytic activity and recyclability of MIL-53(Al) catalyst were evaluated based on the Paal-Knorr reaction between aniline and acetonylacetone. The reaction conditions were optimized and the results showed that the MIL-53(Al) catalyst exhibited good catalytic activity and recyclability based on the PaalKnorr reaction. With the molar ratio of MIL-53(Al) catalyst of 10 mol %, the molar ratio of aniline and acetonylacetone of 1:1.2, and without solvents, the conversion of aniline could reach 100 % and the selectivity of 2,5-dimethyl-1-phenyl-1H-pyrrole has high yield (95-100 %) after 2 hours by ultrasound activation. The MIL-53(Al) catalyst can be reused five times without significant degradation in the catalytic activity.

scholarly journals Ag2O/GO/TiO2 Composite Nanostructure: an efficient heterogeneous catalyst for one pot synthesis of Bis (dihydropyrimidinone) and tetrahydro-4H-chromenes derivatives

2021 ◽  
Author(s):  
Fatemeh Samandi Zadeh ◽  
Mohammad Kazem Mohammadi ◽  
Ayeh Raeiatzadeh ◽  
Neda Hasanzadeh
Keyword(s):  
Condensation Reaction ◽  
Aromatic Aldehydes ◽  
Synthesis Methods ◽  
X Ray Diffraction ◽  
One Pot ◽  
Transmission Electron ◽  
One Pot Condensation ◽  
Effective Synthesis ◽  
Ft Ir ◽  
Biginelli Condensation

Abstract The simple and efficient synthesis reaction was used for preparing Bis (dihydropyrimidinone) derivatives through Biginelli condensation reaction of terephthalic aldehyde, 1, 3-dicarbonyl compounds and (thio) urea or guanidine and tetrahydro-4H-chromenes via one pot condensation of aromatic aldehydes, malononitrile and dimedone with Ag2O/GO/TiO2 composite nanostructures as a catalyst. The structural functionalities and morphological observations of catalyst were obtained using characterization techniques of field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), Fourier transfer infrared (FT-IR) spectroscopy and transmission electron microscope (TEM). The structures of Bis (dihydropyrimidinone) and tetrahydro-4H-chromenes confirmed by FT- IR, NMR and mass spectroscopy. Excellent yields of the products, simple reaction process and simple work-up are attractive features of these effective synthesis methods.

scholarly journals Ag2O/GO/TiO2 Composite Nanostructure: An Efficient Heterogeneous Catalyst for one Pot Synthesis of Bis (Dihydropyrimidinone) and Tetrahydro-4H-chromenes Derivatives

2020 ◽  
Author(s):  
Fatemeh Samandi Zadeh ◽  
Mohammad Kazem Mohammadi ◽  
Ayeh Rayatzadeh ◽  
Neda Hasanzadeh
Keyword(s):  
Condensation Reaction ◽  
Aromatic Aldehydes ◽  
Synthesis Methods ◽  
X Ray Diffraction ◽  
One Pot ◽  
Transmission Electron ◽  
One Pot Condensation ◽  
Effective Synthesis ◽  
Ft Ir ◽  
Biginelli Condensation

Abstract The simple and efficient synthesis reaction was used for preparing Bis (dihydropyrimidinone) derivatives through Biginelli condensation reaction of terephthalic aldehyde, 1, 3-dicarbonyl compounds and (thio) urea or guanidine and tetrahydro-4H-chromenes via one pot condensation of aromatic aldehydes, malononitrile and dimedone with Ag2O/GO/TiO2 composite nanostructures as a catalyst. The structural functionalities and morphological observations of catalyst were obtained using characterization techniques of field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD), Fourier transfer infrared (FT-IR) spectroscopy and transmission electron microscope (TEM). The structures of Bis (dihydropyrimidinone) and tetrahydro-4H-chromenes confirmed by FT- IR, NMR and mass spectroscopy. Excellent yields of the products, simple reaction process and simple work-up are attractive features of these effective synthesis methods.

A 2D coordination polymer assembled from a nickel(II) tetraazamacrocyclic cation and 4,4′-(dimethylsilanediyl)diphthalate(3–) linker

2020 ◽  
Vol 76 (5) ◽  
pp. 419-426 ◽  
Author(s):  
Sergey P. Gavrish ◽  
Sergiu Shova ◽  
Maria Cazacu ◽  
Yaroslaw D. Lampeka
Keyword(s):  
Diffuse Reflectance ◽  
Diffuse Reflectance Spectroscopy ◽  
Macrocyclic Ligand ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylic Acid Groups ◽  
Structural Differences ◽  
Ft Ir ◽  
Lower Temperature ◽  
Oriented Parallel

The preformed nickel(II) complex of the 14-membered macrocyclic ligand 1,4,8,11-tetraazacyclotetradecane (cyclam, L), when treated with 4,4′-(dimethylsilanediyl)diphthalic acid (H4A) in a DMF/H2O mixture (4:1 v/v) under heating, leads to [Ni(L)]3(HA)2·3DMF (I·DMF). Redissolution of this compound in a DMF/H2O/MeOH mixture (4:1:30 v/v/v) with mild acidification under gentle heating results in the formation of a similar compound but containing water and methanol molecules of crystallization, [Ni(L)]3(HA)2·5H2O·2MeOH (II·H2O). At lower temperature and concentration of reactants and longer reaction time, single crystals of composition {[{Ni(L)}3(HA)2]·4CH3OH} n (II·MeOH) were isolated. Single-crystal X-ray diffraction analysis of this compound, which, according to PXRD is isostructural with II·H2O but different from I·DMF, revealed its two-dimensional (2D) polymeric structure, i.e. poly[[bis{μ3-4-[(4-carboxy-3-carboxylatophenyl)dimethylsilyl]benzene-1,2-dicarboxylato-κ3 O 1:O 2:O 3′}tris(1,4,8,11-tetraazacyclotetradecane-κ4 N)trinickel(II)] methanol tetrasolvate], {[Ni3(C18H13O8Si)2(C10H24N4)3]·4CH3OH} n . It is built up of the monoprotonated tricarboxylate HA3− ligand coordinated in a monodentate manner in the axial positions of two crystallographically independent NiII cations, one of which is located on a crystallographic inversion centre. Both metal ions adopt a slightly tetragonally elongated trans-N4O2 octahedral geometry. The compound has a lamellar structure with polymeric layers oriented parallel to the (10\overline{2}) plane, which are in turn linked via hydrogen bonds involving protonated carboxylic acid groups of the ligand. Bulk compounds I·DMF and II·H2O were characterized by FT–IR and diffuse reflectance spectroscopy and thermogravimetry, which provide evidence of their structural differences.

scholarly journals Synthesis of pure potassium pentaborate (KB5) from potassium dihydrogen phosphate (KH2PO4) and colemanite

2021 ◽  
Author(s):  
Özlem Karagöz ◽  
Soner Kuşlu
Keyword(s):  
Solution Method ◽  
Potassium Dihydrogen Phosphate ◽  
Dihydrogen Phosphate ◽  
X Ray Diffraction ◽  
Reaction Conditions ◽  
Potassium Dihydrogen ◽  
Ft Ir ◽  
Lower Temperature ◽  
The Cost ◽  
Sem Analyses

Abstract In this study, after specifying theoretical reaction conditions required for chemical reaction, potassium pentaborate (KB5) was synthesized from the potassium dihydrogen phosphate (KH2PO4) solution and the raw colemanite (Ca2B6O11.5H2O) ore. The slow evaporation solution method was used at 25 ℃. The effect of time (6-18 hours) on crystallization was studied. Synthesized minerals were characterized by X-ray diffraction (XRD), Fourier transform infrared (FT-IR), RAMAN spectroscopies, and scanning electron microscopy (SEM). The results according to the XRD, FT-IR, RAMAN, and SEM analyses proved that the synthesized product was the potassium pentaborate (KB5O8.4H2O) mineral having the ICSD: 96-026-1927 pdf code. As a result, the cost was reduced by using raw boron ore, colemanite and KB5 could be obtained in a shorter time and at a lower temperature.

scholarly journals One pot three component synthesis of substituted 3,4,6,7-tetrahydro-3,3,6,6-tetramethyl-9,10-diphenylacridine-1,8(2H,5H,9H,10H)-diones catalyzed by efficient In2O3-SiO2

2021 ◽  
Author(s):  
Deepak Totaram Tayde ◽  
Madhukar E. Navgire ◽  
Machhindra K. Lande
Keyword(s):  
High Yield ◽  
Reusable Catalyst ◽  
X Ray Diffraction ◽  
One Pot ◽  
Synthetic Strategy ◽  
Transmission Electron ◽  
Catalytic Material ◽  
Ir Transmission ◽  
Ft Ir ◽  
Temperature Programmed

Abstract A convenient, One pot synthesis of heterocyclic nucleous acridine derivative compound has been achieved those are having very much attention in medicinal chemistry because of their extensive application in biology. The mixture of dimedone, substituted benzaldehyde and aniline were catalyzed by efficient In2O3-SiO2 heterogeneous reusable catalyst in ethanol to obtain the desired acridine derivatives with good yield. Hydrothermal method used to synthesize In2O3-SiO2 catalytic material. This catalytic material were characterized by using X-ray diffraction spectroscopy (XRD), scanning electron microscopy (SEM), Energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FT-IR), Transmission electron microscope (TEM), Temperature-programmed desorption (NH3-TPD) and Brunauer-Emmett-Teller (BET). Our synthetic strategy features high yield, simple work up procedure, non-toxic, clean, and easy recovery and reusability of the catalytic system.

Ten-Vertex Polyhedral Monocarbaborane Chemistry. The Novel High-Yield Formation of the Ten-Vertex closo Compound [6-(PMe2Ph)-closo-1-CB9H9] from the Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11]

1993 ◽  
Vol 58 (12) ◽  
pp. 2924-2935 ◽  
Author(s):  
Jane H. Jones ◽  
Bohumil Štíbr ◽  
John D. Kennedy ◽  
Mark Thornton-Pett
Keyword(s):  
Nmr Spectroscopy ◽  
Diffraction Analysis ◽  
High Yield ◽  
Monoclinic Space Group ◽  
The Novel ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
X Ray ◽  
Yield Formation ◽  
Boiling Toluene

Thermolysis of [8,8-(PMe2Ph)2-nido-8,7-PtCB9H11] in boiling toluene solution results in an elimination of the platinum centre and cluster closure to give the ten-vertex closo species [6-(PMe2Ph)-closo-1-CB9H9] in 85% yield as a colourles air stable solid. The product is characterized by NMR spectroscopy and single-crystal X-ray diffraction analysis. Crystals (from hexane-dichloromethane) are monoclinic, space group P21/c, with a = 903.20(9), b = 1 481.86(11), c = 2 320.0(2) pm, β = 97.860(7)° and Z = 8, and the structure has been refined to R(Rw) = 0.045(0.051) for 3 281 observed reflections with Fo > 2.0σ(Fo). The clean high-yield elimination of a metal centre from a polyhedral metallaborane or metallaheteroborane species is very rare.

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