Synthesis Of Phosphate Research Articles

Synthesis and luminescent properties of Mn-doped alpha-tricalcium phosphate

In this work, a series of Mn2+-doped α-tricalcium phosphate (α-TCP) powders was synthesized by wet co-precipitation method followed by high-temperature annealing and thermal quenching. It was shown that Mn2+-doped α-TCP polymorph can be successfully synthesized with a doping level up to 1 mol%. All Mn-doped samples exhibited a broadband emission in the range from 525 to 825 nm with a maximum centered at around 630 nm. The highest emission intensity was observed for the sample with the highest content of Mn. The crystal structure and purity were evaluated by powder X-ray diffraction (XRD), Fourier-transform infrared (FTIR) and electron paramagnetic resonance (EPR) spectroscopies. Scanning electron microscopy (SEM) was used to investigate the morphological features of the synthesized products. Optical properties were investigated by means of photoluminescence measurements. Excitation spectra, emission spectra and decay curves of the samples were studied. Temperature-dependent photoluminescence measurements were performed as well.

Synthesis, crystal growth and characterizations of 4-fluorobenzyl ammonium dihydrogen phosphate of NLO single crystal [PFBADP

Good quality single crystal of p-fluorobenzyl ammonium dihydrogen phosphate [PFBADP], a compound has been successfully grown from aqueous solution by slow evaporation solution growth method. The crystal system and lattice parameters are confirmed by the single crystal X-Ray diffraction analysis. An optical absorption study on the sample shows that the material is well suitable for optical applications. The functional groups of the compound are confirmed qualitatively by FT-IR spectral analysis. The photoluminescence studies indicate that the grown crystals have a green fluorescence emission. Dielectric studies have been carried out for the grown crystal and the results were discussed in detail.

Facile sonochemical synthesis of strontium phosphate based materials for potential application in supercapattery devices

Among hybrid energy storage devices, supercapattery gained profound research interest due to its ability to give high energy density while maintaining the power density and cyclic stability. Herein, novel low-cost strontium based materials are synthesized by controlled sonochemical method and subsequently calcined at various temperatures. The multiple phases of the material synergistically contributed in the electrochemical charge storage process and give high specific capacity of 220 C g−1 (as-prepared material) and 213 C g−1 (calcined at 200 °C) at 0.5 A g−1. A thorough electrochemical performance of optimized material is investigated as an electrode in asymmetric device. The supercapattery (SP2//AC) exhibits a specific capacity of 103.4 C g−1 at 0.5 A g−1 in the voltage range of 0–1.7 V. Furthermore, supercapattery offers a considerably high specific energy of 24.4 Wh kg−1 at a specific power of 425 W kg−1 and an excellent specific power of 1870 W kg−1 by maintaining specific energy at 14.5 Wh kg−1. In addition, the device retained its specific capacity to 90% after 3000 charging/discharging cycles at 1 A g−1. Strontium based materials could be proposed as an appropriate electrode material for energy storage systems.

Wet synthesis of high purity crystalline urea phosphate from untreated Moroccan industrial phosphoric acid

The phosphorus-nitrogen fertilizer family improves the availability of phosphorus and nitrogen for efficient crop growth. Urea phosphate 17-44-0 (N-P 2 O 5 -K 2 O%) is considered as a binary fertilizer characterized by its high purity and it is easily soluble in water. In addition, urea phosphate can be used in other fields as a high-quality food additive, finishing agent for metals and fermentation food. As a fertilizer, it is suitable for alkaline soils. In this work, a new process for the synthesis of urea phosphate by the wet route is developed. It consists in directly producing crystalline urea phosphate by the chemical reaction between Moroccan industrial phosphoric acid (54 % P 2 O 5 ) and solid urea (46 %). The synthesis is carried out by mixing the solid urea with a stoichiometric amount of untreated Moroccan industrial phosphoric acid. The chemical reaction is complete for optimal conditions which are a temperature of 50 °C and a duration of 90 min. After cooling, the urea phosphate crystals are formed without any additional treatment and are easily recovered. Analysis of the residual liquor after recovery of the urea phosphate crystals confirms that the majority of impurities which may be harmful to the environment pass into the liquid phase

Electrochemical crystallization for phosphate recovery from an electronic industry wastewater effluent using sacrificial iron anodes

With the circular economy in mind, recovery of iron phosphate, i.e., ferric phosphate or ferrous phosphate, from industrial wastewater is realized and the products recovered could be used in the synthesis of lithium iron phosphate for Li-ion secondary batteries. The formation of iron phosphate highly depends on pH and dissolved oxygen (DO) level. The present study focused on the phosphorus removal and recovery from the industrial wastewater effluent of a semiconductor plant by crystallization of iron phosphate. P recovery as iron phosphate was explored by means of electrochemical crystallization using a sacrificial iron anode under various DO levels (air sparging, mechanical mixing, and N2 purging) and pH values (both initial and fixed pH). Under the nitrogen purging condition, the P removal linearly increased with increasing of the Fe:P molar ratios, reaching 100% when the Fe:P molar ratio equals 1.5, which is the stoichiometric molar ratio of ferrous phosphate. The ferrous phosphate particles quickly settled and the crystalline structure was confirmed as vivianite. The final product obtained at pH 6.0 was composed of 82 wt% of vivianite. The operational cost of the electrochemical process was estimated to be only 23.5% of the costs required by the fluidized chemical crystallization process reported in the literature.

Template Synthesis of Calcium Phosphates in Nanoporous Polyolefin Films Obtained via Crazing Mechanism

Template Synthesis of Calcium Phosphates in Nanoporous Polyolefin Films Obtained via Crazing Mechanism

A novel environment-friendly synthesis of high purity micron iron phosphate and its application as a precursor of lithium iron phosphate

This essay studies a novel environment-friendly synthesis method for the high purity micron iron phosphate. Compared with traditional synthesis method, this new method can greatly reduce the amount of industrial sewage, hence it is an environment-friendly production technology which can effectively improve the products’ purity, structure stability and morphological consistency. This new method includes two-step reactions: first, phosphoric acid, iron powder and hydrogen peroxide are used as raw materials to obtain iron phosphate dihydrate intermediate, which is then calcined at high temperature to obtain anhydrous iron phosphate. The results show that the iron phosphate prepared for this new method is a hexagonal system-structured iron orthophosphate with high purity and without any impurities, exhibiting a regular and primary spherical particle morphology, at the average size of 3.096μm in particle and the specific surface area reaching 39.1765 m2 g−1. With these excellent characteristics, it has better application potentials in the field of electrode material preparation. The electrochemical performance of lithium iron phosphate anode materials synthesized with it as the precursor is superior to those synthesized with the iron phosphate prepared by the traditional method as precursor. The first specific capacity of discharge at 0.5C and 10C can be as high as 154.3989 or 102.9326 mAh g−1, increasing by 2.74% and 8.03%, respectively.

A systematic study of the synthesis of transition metal phosphides and their activity for hydrodeoxygenation of phenol

Five different unsupported transition metal phosphides were synthesized and tested for hydrodeoxygenation of phenol in gas phase at 300 °C and atmospheric pressure. The metal phosphide phases were synthesized in two steps: synthesis of phosphates and temperature programmed reduction. In situ X-ray diffraction and temperature programmed reduction revealed the formation of the phosphide phases: Ni2P, MoP, CoP/CoP2, FeP and WP. The in situ diffractograms showed that the metal phosphate precursor is decomposed during reduction, producing metal oxide (Molybdenum) or pyrophosphate (Nickel, Iron) phases, without the formation of a metallic phase. All catalysts showed high selectivity to direct deoxygenation products, indicating that the phosphide phases promoted the direct cleavage of CO bond. However, product distribution varied significantly depending on the metal phosphide phase. Ni2P catalyst exhibited the highest selectivity to benzene, whereas CoP, FeP and WP showed a significant formation of cyclohexene. FeP also produced cyclohexane, while a large amount of C5 – C6 hydrocarbons was formed over MoP. Product distribution was correlated to the type of crystal structure of transition metal phosphides.

Protective roles of salicylic acid in maintaining integrity and functions of photosynthetic photosystems for alfalfa (Medicago sativa L.) tolerance to aluminum toxicity

Aluminum (Al) can be detrimental to plant growth in areas with Al contamination. The objective of this study was to determine whether salicylic acid (SA) can improve plant tolerance to Al stress by mitigating Al toxicity for chloroplasts and photosynthetic systems in alfalfa (Medicago sativa L.). Plants were treated with Al (100 μM) for 3 d in a hydroponic system. The content of Al increased in leaves treated with Al, resulting in damage and deformation of chloroplasts. In Al-damaged leaves, chloroplast envelopes and starch granules disappeared; the lamellae and stroma lamella were loosely arranged and indistinguishable, and the number of grana was reduced; a large number of small plastoglobules appeared. Foliar spraying of 15 μM SA reduced Al content in roots and leaves and alleviated Al damages in chloroplasts. With 15 μM SA treatments, the chloroplast shape returned to a flat ellipsoid, thylakoids were arranged closely and regularly, chloroplasts had intact starch granules, and small plastoglobules disappeared. SA-treated plants had significantly higher aboveground biomass than the untreated control exposed to Al stress. Photosynthetic index and gene expression analyses demonstrated that SA could alleviate adverse effects of Al toxicity by increasing light capture efficiency, promoting electron transport in the photosynthetic electron transport chain and thylakoid lumen deacidification, and promoting synthesis of aenosine triphosphate (ATP) and nicotinamide adenine dinucleotide phosphate (NADPH). SA played protective roles in maintaining integrity and functions of photosystems in photosynthesis for plant tolerance to Al stress.

Evaluation of the Behavior in Water of a Biomaterial Composed of Different Phases of Calcium Phosphate

The synthesis of calcium phosphates of biological interest has been one of the strategies studied in the field of tissue regeneration due to its similarity to the inorganic components of bone. One of the aspects studied has been the process of dissolution of calcium phosphates in water and physiological serum, with the aim of being able to know everything related to the behavior of these materials during the bone regeneration process. The objective of this work was to evaluate the behavior in the water of a biomaterial composed of a three-phase mixture of calcium phosphate for use in tissue regeneration. Three phases of calcium phosphate were synthesized. A biomaterial with a mixture of these phases was elaborated and placed in water at 37ºC. The amount of calcium and phosphorus released was determined over time. The treated samples were evaluated by X-ray diffractometry and infrared spectrometry. The results of this study demonstrated that for calcium, the release overtime was not significant due to the reaction of these ions in solution with phosphate ions and the subsequent precipitation in the studied material. While for phosphorus, the release over time was significant. The results corroborate that the use of a triphasic mixture of calcium phosphates allows us to produce a biomaterial suitable for use as a material in tissue regeneration.

Synthesis of Tricalcium Phosphate From Eggshells with Precipitation Method

Calcium phosphate compounds are one of the biomaterials that are widely used for bone reconstruction because they are biocompatible and have a chemical composition that is close to the inorganic components present in the bone. Two types of calcium phosphate that are widely applied to the bone reconstruction process are hydroxyapatite (Ca10 (PO4) 6 (OH) 2) and β-Tricalcium Phosphate (Ca3 (PO4)2). This research develops the manufacture of β-Tricalcium Phosphate by reacting calcium compounds derived from chicken eggshells and phosphate sources derived from dinatrium phosphate (Na2HPO4) using precipitation method which is carried out with variations in sintering temperature 600 to 1000 °C and sintering time of 1 to 5 h. The results of X-Ray fluorescence (XRF) analysis showed that the Ca / P ratio obtained was 1.74, at the sintering temperature of 1000 °C and the sintering time for 5 h. These results have approached a standard where the ratio of Ca / P on Tricalcium Phosphate is 1.5. While based on the results of X-Ray Diffraction (XRD) analysis that in the sample formed two types of Calcium Phosphate namely β-Tricalcium Phosphate and Hydroxyapatite so that it can be said that the product produced is Biphase Calcium Phosphate. The high percentage of β-Tricalcium Phosphate is 81.9% with the 3 highest peaks, namely at the angle 2θ of 27.83; 31.03; 34.42 is obtained at the sintering temperature of 1000 °C and at the sintering time is 5 h.

Continuous synthesis of tributyl phosphate in microreactor

Tributyl phosphate (TBP) is the most widely used extractant in the nuclear fuel cycle. It is used both in the front-end and back-end of the nuclear fuel cycle for separation and purification of nuclear materials. It is also used for solvent extraction of other metal ions such as lithium, cobalt and nickel. Synthesis of TBP involves highly exothermic reaction of n-butanol with phosphorus oxychloride. It is conventionally carried out using a batch/semi-batch process. We report, for the first time, a continuous method to synthesize TBP in a microreactor. The product yield was observed to increase with an increase in the residence time and the reaction temperature.100% yield was obtained for a residence time of 44 min at reaction temperature of 60 °C in the microreactor having a T-junction micromixer. The space-time-yield and production rate at these conditions were 13270.67 kg/day-m3 and 41.02 gm/day, respectively. Two different types of micromixers (T-junction micromixer and split-and-recombine micromixer) were compared. CFD simulations to quantify mixing in micromixers were also performed to have more insights into the experimental trends.

Synthesis of Amorphous Calcium Phosphate: A Review

The aim of this study is to summarize various synthesis routes of amorphous calcium phosphate (ACP), focusing on properties, especially Ca/P molar ratio and specific surface area (SSA) of obtained ACP. The effects of synthesis conditions on properties of final products are analysed and discussed.

Synthesis, crystal structure, physical and catalytic oxidation studies of a new hybrid phosphate [(N2H5)2Co(HPO4)2

A new one-dimensional coordination polymer [(N2H5)2Co(HPO4)2] was synthesized by slow evaporation method and characterized by means of single-crystal X-ray diffraction, Fourier Transform Infrared Spectroscopy (FTIR) and Thermogravimetric Analysis (TGA). Its catalytic activity was tested using UV–visible absorption measurements. The compound crystallizes in the monoclinic system (S.G: P21/c) with the cell parameters (Å, °): a = 5.3665(3), b = 11.1271(6), c = 7.7017(4), β = 104.843(4), V = 444.55(4) Å3 and Z = 2. The crystal structure, consisting of a linear chain, is made of rings of [CoN2O4] octahedra and [PO3(OH)] tetrahedra sharing vertices via oxygen atoms coordinated to cobalt centers. The rings are linked to chains running along [100] and form thereby polymeric chains that are connected by hydrogen bonds in a three-dimensional arrangement. The FTIR spectroscopy shows the expected bands of hydrazine and phosphate groups. The thermal behavior consists mainly of the loss of hydrazine moieties leading thus to the formation of anhydrous cobalt phosphate. The phosphate complex exhibits efficiency in catalytic oxidation and degradation of methylene blue dye. The ac magnetic susceptibility shows a peak indicating antiferromagnetic order with a Néel temperature of 5.5 K. Fitting the Curie-Weiss equation to the ac magnetic susceptibility above 50 K gives the average Curie-Weiss Constant to be −11.8 K.

Synthesis and Thermal Stability of Si-Containing Calcium Phosphates

Si-containing calcium phosphates have been synthesized. The synthesized solid phases have been investigated by X-ray diffraction analysis, IR spectroscopy, and optical microscopy. SThe specific surface areas of the samples are determined by the Brunauer–Emmett–Teller (BET) method. It is shown that an increase in the concentration of silicate ions in the starting reaction solution decreases the content of phosphate ions in the composition of synthesized samples (which is indicative of possible isomorphic substitution by silicate ions). Dynamic dissolution is carried out, and the dissolution rates of solid phases with different contents of silicate ions before and after thermal treatment are compared. It is established that heat treatment of the samples leads to the formation of a mixture of Si-containing hydroxylapatite and β-tricalcium phosphate.

Solvo-hydrothermal synthesis of calcium phosphate nanostructures from calcium inositol hexakisphosphate precursor in water-ethanol mixed solutions

We report the synthesis and characterization of crystalline calcium phosphate (CaP) nanostructures from calcium inositol hexakisphosphate (CaIP6) precursor in water-ethanol mixed solutions. We show how these CaPs can be prepared by a solvo-hydrothermal reaction and determined their compositions and structures using a battery of material characterization techniques. Our results show that only the hydroxyapatite (HAP) and dicalcium phosphate anhydrous (DCPA) phases of CaP were present in the nanostructures produced in water-ethanol mixtures, and that HAP/DCPA ratio of the rod- and plate-shaped CaP nanostructures produced were affected by the amount of ethanol present in these mixtures. The described method can be used to improve morphological control of CaP-based biomate-rials and has potential use in bone regenerative medicine.

Synthesis of (R)-3-(tert-Butoxycarbonylamino)-4-(2,4,5-trifluorophenyl)butanoic Acid, a Key Intermediate, and the Formal Synthesis of Sitagliptin Phosphate.

An alternate formal synthesis of Sitagliptin phosphate is disclosed from 2,4,5-trifluorobenzadehyde in 8 linear steps with an overall yield of 31%. The chiral β-amino acid moiety present in sitaglitpin is installed via an asymmetric hydrogenation followed by a stereoselective Hofmann rearrangement as the key steps. The key chiral intermediate Boc-amino acid 1 prepared by this novel route was further converted to Sitagliptin phosphate following the known literature protocol.

Synthesis of bioactive calcium phosphate from cockle shell for biomedical applications

The present work reports the synthesis of bioactive calcium phosphate from cockle shell via the combination of calcination and hydrothermal process. The raw cockle shells were pre-treated with 30 % of hydrogen peroxide for 4 days to eliminate the impurities. Afterward, the dried cockle shells were crushed and calcined at various temperatures ranging from 300 to 1100 °C. Subsequently, the calcined powders underwent hydrothermal process in di-ammonium hydrogen phosphate and distilled water at pH of 10.5 for 30 minutes. Lastly, the hydrothermal treated powders were dried in oven at 50 °C for 3 days. The results showed that the mixture of aragonite, calcite, hydroxyapatite, and calcium hydroxide was successfully synthesized at a calcination temperature of 900 °C and 1100 °C. In addition, the nanorods in the length of 80-300 nm were formed. The findings of this work indicate that the cockle shell could be transformed into valuable bioactive materials for biomedical applications.

Synthesis, Characterization, and Stability of Americium Phosphate, AmPO4.

AmPO4 was prepared by a solid-state reaction method, and its crystal structure at room temperature was solved by powder X-ray diffraction combined with Rietveld refinement. The purity of the monazite-like phase was confirmed by spectroscopic (high-resolution solid-state 31P NMR and Raman) and microscopic (SEM-EDX and TEM) techniques. The thermal and self-irradiation stability have been studied. The compound is stable under argon and air atmosphere at least up to 1773 K. It remains crystalline under self-irradiation for circa two months, with a crystallographic volume swelling of ∼1.5%, and then is amorphizing over a year. However, microcrystals are present in the amorphous material even after a two year period of time. All these characteristics are discussed in relation to the potential application of AmPO4 as a stable form of Am in radioisotope power sources for space exploration and of behavior of the monazites under irradiation.

The Synthesis and Thermal Expansion Behavior of Sodium and Calcium Zirconium Copper Phosphates

The crystal-chemical approach has been applied to design materials with regulated thermal expansion. To that end, model simulations have been performed for compositions of phosphates that yield solid solutions of the following type Na1 + 2xZr2 –xCux(PO4)3 and Ca0.5 +xZr2 –xCux(PO4)3, 0.1 ≤ x ≤ 0.5 with the expected structure of NaZr2(PO4)3 (NZP). The new phosphates have been prepared by solid-state reactions and characterized by X‑ray diffraction, IR spectroscopy, and scanning electron microscopy. The compounds have been shown to crystallize in the NZP structure, with a particle size from 0.1 to 1 μm. The thermal expansion of the compounds has been studied by high-temperature X-ray diffraction in the temperature range from 25 to 700°C. Linear, average, and volume coefficients of thermal expansion and anisotropy of thermal expansion have been calculated and analyzed in relation to composition of Na, Zr, Cu and Ca, Zr, Cu phosphates in the studied sets.