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Correlation between structure, chromaticity, and dielectric properties of calcium copper pyrophosphates, Ca2−xCu xP2O7
(2022-12-01)
Baitahe, Rattanai
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Sronsri, Chuchai
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Thompho, Somphob
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Chaiseeda, Kittichai
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Montri, Nattaya
The solid-state reaction was employed to synthesize Ca<inf>2−x</inf>Cu<inf>x</inf>P<inf>2</inf>O<inf>7</inf> by varying the mole ratio between Ca and Cu. The structure and crystallography of the pyrophosphate compounds were identified and confirmed by using X-ray diffraction (XRD). The Rietveld refinement method and the extended X-ray absorption fine structure (EXAFS) least-squares fitting technique were also applied to refine the sample crystal structure. The single phases of the obtained Ca<inf>2</inf>P<inf>2</inf>O<inf>7</inf>, CaCuP<inf>2</inf>O<inf>7</inf>, and Cu<inf>2</inf>P<inf>2</inf>O<inf>7</inf> samples and the mixing phases of the obtained Ca<inf>1.5</inf>Cu<inf>0.5</inf>P<inf>2</inf>O<inf>7</inf> and Ca<inf>0.5</inf>Cu<inf>1.5</inf>P<inf>2</inf>O<inf>7</inf> samples were identified, and then only a single phase of the samples was subjected to structural and dielectrical analyses. The structural results exhibit the tetragonal crystal system with the P4<inf>1</inf> space group for β-Ca<inf>2</inf>P<inf>2</inf>O<inf>7</inf>, the monoclinic crystal system with the P2<inf>1</inf>/c space group for CaCuP<inf>2</inf>O<inf>7</inf>, and the C2/c space group for α-Cu<inf>2</inf>P<inf>2</inf>O<inf>7</inf>. The dielectric constant (ε<inf>r</inf>) of the single metal pyrophosphates (Ca<inf>2</inf>P<inf>2</inf>O<inf>7</inf> and Cu<inf>2</inf>P<inf>2</inf>O<inf>7</inf>) was higher than that of binary metal pyrophosphates (CaCuP<inf>2</inf>O<inf>7</inf>). The image sensor result of the Cu<inf>2</inf>P<inf>2</inf>O<inf>7</inf> sample (x = 2.00) illustrated a yellowish-green color, while other compounds (x = 0.50−1.50) presented color tones that changed from blue-green to bluish-green. Raman and Fourier transform infrared (FTIR) spectrophotometers were employed to characterize and confirm the vibrational characteristics of the P<inf>2</inf>O<inf>7</inf>4− group, which contains the O–P–O radical ([PO<inf>2</inf>]-) and the P–O–P bride ([OPO]-) and approximate M–O stretching modes. Furthermore, this work reports for the first time that the change in the crystal structure of Ca<inf>2−x</inf>Cu<inf>x</inf>P<inf>2</inf>O<inf>7</inf> (i.e., bond angle of P−O−P in P<inf>2</inf>O<inf>7</inf>4− and distortion phenomena in the M−O<inf>6</inf> octahedral site) are cause the correlation between the structure, chromaticity, and dielectric properties of calcium copper pyrophosphates, Ca<inf>2−x</inf>Cu<inf>x</inf>P<inf>2</inf>O<inf>7</inf>.
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Economical and Environmentally Friendly Track of Biowaste Recycling of Scallop Shells to Calcium Lactate
(2022-05-03)
Seesanong, Somkiat
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Wongchompoo, Yok
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Boonchom, Banjong
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Sronsri, Chuchai
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Laohavisuti, Nongnuch
The scallop shell waste (Pectinidae, one of saltwater clams) was used as a raw material (precursor) to prepare calcium lactate (Ca(C<inf>2</inf>H<inf>4</inf>OHCOO)<inf>2</inf>), and the physicochemical properties of scallop-derived calcium lactate were then investigated. The scallop waste was first ground to obtain calcium carbonate (CaCO<inf>3</inf>) powder, and the calcium lactate compounds were successfully synthesized by the reactions between shell-derived CaCO<inf>3</inf>and lactic acid (C<inf>2</inf>H<inf>4</inf>OHCOOH). The short preparation time, high percentage yield, and low-cost production are the preferred manners, and, in this research, it was the reaction of 70 wt % lactic acid and scallop-derived CaCO<inf>3</inf>. The thermal decompositions of both CaCO<inf>3</inf>precursor and all prepared calcium lactates resulted in the formation of calcium oxide (CaO), which is widely used as a catalyst for biodiesel production. By comparing with the literature, the results obtained from the characterization instruments (infrared spectrophotometer, X-ray diffractometer, thermogravimetric analyzer, and scanning electron microscope) confirmed the formation and crystal structure of both CaCO<inf>3</inf>and its calcium lactate product. The morphologies of calcium lactate show different sizes depending on the acid concentration used in the reaction process. Consequently, this work reports an easy, uncomplicated, low-cost technique to change the cheap calcium compound product (scallop CaCO<inf>3</inf>) derived from shellfish waste to the valuable compound (calcium lactate), which can be used in many industries.
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Recrystallization of Triple Superphosphate Produced from Oyster Shell Waste for Agronomic Performance and Environmental Issues
(2022-02-01)
Seesanong, Somkiat
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Seangarun, Chaowared
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Boonchom, Banjong
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Sronsri, Chuchai
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Laohavisuti, Nongnuch
Calcium dihydrogen phosphate monohydrate (Ca(H<inf>2</inf>PO<inf>4</inf>)<inf>2</inf>·H<inf>2</inf>O) (a fertilizer) was successfully synthesized through a recrystallization process using prepared triple superphosphate (TSP) derived from oyster shell waste as the starting material. This bio-green, eco-friendly process to produce an important fertilizer can promote a sustainable society. The shell-waste-derived TSP was dissolved in distilled water and kept at 30, 50, and 80◦C. Non-soluble powder and TSP solution were obtained. The TSP solution fractions were then dried, and the recrystallized products (RCP30, RCP50, and RCP80) were obtained and confirmed as Ca(H<inf>2</inf>PO<inf>4</inf>)<inf>2</inf>·H<inf>2</inf>O. Conversely, the non-soluble products (NSP30, NSP50, and NSP80) were observed as calcium hydrogen phosphate dihydrate (CaHPO<inf>4</inf>·2H<inf>2</inf>O). The recrystallized yields of RCP30, RCP50, and RCP80 were found to be 51.0%, 49.6%, and 46.3%, whereas the soluble percentages were 98.72%, 99.16%, and 96.63%, respectively. RCP30 shows different morphological plate sizes, while RCP50 and RCP80 present the coagulate crystal plates. X-ray diffractograms confirmed the formation of both the NSP and RCP. The infrared adsorption spectra confirmed the vibrational characteristics of HPO<inf>4</inf>2−, H<inf>2</inf>PO<inf>4</inf>−, and H<inf>2</inf>O existed in CaHPO<inf>4</inf>·2H<inf>2</inf>O and Ca(H<inf>2</inf>PO<inf>4</inf>)<inf>2</inf>·H<inf>2</inf>O. Three thermal dehydration steps of Ca(H<inf>2</inf>PO<inf>4</inf>)<inf>2</inf>·H<inf>2</inf>O (physisorbed water, polycondensation, and re-polycondensation) were observed. Ca(H<inf>2</inf>PO<inf>4</inf>)<inf>2</inf> and CaH<inf>2</inf>P<inf>2</inf>O<inf>7</inf> are the thermodecomposed products from the first and second steps, whereas the final product is CaP<inf>2</inf>O<inf>6</inf>.
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Simple recycling of biowaste eggshells to various calcium phosphates for specific industries
(2021-12-01)
Laohavisuti, Nongnuch
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Boonchom, Banjong
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Boonmee, Wimonmat
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Chaiseeda, Kittichai
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Seesanong, Somkiat
Egg consumption is very high throughout the world and with it comes enormous amount of waste eggshells. To reduce and utilize these wastes, eggshell wastes were simply transformed to low- or high-purity calcium carbonate grades by washing, crushing, and drying to use as raw materials for producing highly valuable calcium phosphate products. Low-purity calcium carbonate grade was used to prepare triple superphosphate for using in fertilizer industry, whereas high-purity calcium carbonate grade was used to produce dicalcium phosphate dihydrate, monocalcium phosphate monohydrate, and tricalcium phosphate for using in mineral feed and food additive industries. All calcium phosphate samples obtained by simple, rapid, cheap, and environmentally safe method using eggshells and phosphoric acid were identified and their structural phases and impurities were determined by XRF, XRD and FTIR techniques. Thermal behaviors of raw materials and the prepared calcium phosphates excepted tricalcium phosphate were investigated by TG/DTG techniques. The methodologies described here will be useful to manage eggshells by converting them to highly valuable products, which can solve eggshell wastes problem from industries and communities. This finding supports the viewpoint of zero waste operation to produce value-added products for obtaining sustainable development, which may be selected as an alternative way for material recycling and waste management in the future.
1
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Composition and Properties of Triple Superphosphate Obtained from Oyster Shells and Various Concentrations of Phosphoric Acid
(2021-08-31)
Seesanong, Somkiat
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Seangarun, Chaowared
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Boonchom, Banjong
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Laohavisuti, Nongnuch
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Chaiseeda, Kittichai
Triple superphosphates [TSPs, Ca(H2PO4)2·H2O] were produced by exothermic reactions of oyster shells and different concentrations of phosphoric acid (10, 20, 30, 40, 50, 60, and 70% w/w) in a molar ratio of 1:2. The percentage yields, P2O5 and CaO contents, metal impurities, and thermal behaviors of all the as-prepared products are dependent on the concentrations of phosphoric acid added during the production processes, which confirm to get the best optimum of 60% w/w phosphoric acid. All the as-prepared products were characterized by several characterization methods [X-ray fluorescence, thermal gravimetric/derivative thermal gravimetric analysis, powder X-ray diffraction, Fourier-transform infrared spectroscopy, and scanning electron microscopy], verifying that all the obtained compounds are TSP that can be used as fertilizers without metal toxic contaminants. From the successful results, the method for TSP production can be applied in the fertilizer industry based on starting waste materials of oyster shells that can replace the use of unsustainable phosphate or calcium minerals obtained from nonliving things.
1
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Conversion of bivalve shells to monocalcium and tricalcium phosphates: An approach to recycle seafood wastes
(2021-08-02)
Seesanong, Somkiat
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Boonchom, Banjong
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Chaiseeda, Kittichai
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Boonmee, Wimonmat
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Laohavisuti, Nongnuch
The search for sustainable resources remains a subject of global interest and the conversion of the abundantly available bivalve shell wastes to advanced materials is an intriguing method. By grinding, calcium carbonate (CaCO<inf>3</inf>) powder was obtained from each shell of bivalves (cockle, mussel, and oyster) as revealed by FTIR and XRD results. Each individual shell powder was reacted with H<inf>3</inf>PO<inf>4</inf> and H<inf>2</inf>O to prepare Ca(H<inf>2</inf>PO<inf>4</inf>)<inf>2</inf>·H<inf>2</inf>O giving an anorthic crystal structure. The calcination of the mixture of each shell powder and its produced Ca(H<inf>2</inf>PO<inf>4</inf>)<inf>2</inf>·H<inf>2</inf>O, at 900 °C for 3 h, resulted in rhombohedral crystal β-Ca<inf>3</inf>(PO<inf>4</inf>)<inf>2</inf> powder. The FTIR and XRD data of the CaCO<inf>3</inf>, Ca(H<inf>2</inf>PO<inf>4</inf>)<inf>2</inf>·H<inf>2</inf>O, and Ca<inf>3</inf>(PO<inf>4</inf>)<inf>2</inf> prepared from each shell powder are quite similar, showing no impurities. The thermal behaviors of CaCO<inf>3</inf> and Ca(H<inf>2</inf>PO<inf>4</inf>)<inf>2</inf>·H<inf>2</inf>O produced from each shell were slightly different. However, particle sizes and morphologies of the same products obtained from different shells were slightly different—but those are significantly different for the kind of the obtained products. Overall, the products (CaCO<inf>3</inf>, Ca(H<inf>2</inf>PO<inf>4</inf>)<inf>2</inf>·H<inf>2</inf>O, and Ca<inf>3</inf>(PO<inf>4</inf>)<inf>2</inf>) were obtained from the bivalve shell wastes by a rapidly simple, environmentally benign, and low-cost approach, which shows huge potential in many industries providing both economic and ecological benefits.
2
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Simple and Rapid Synthesis of Calcium Acetate from Scallop Shells to Reduce Environmental Issues
(2021-01-01)
Thongkam, Montree
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Saelim, Jinnaput
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Boonchom, Banjong
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Seesanong, Somkiat
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Chaiseeda, Kittichai
The search for sustainable resources remains a subject of global interest. Calcium acetate used in many fields was prepared using waste scallop shell as a raw material, and its physicochemical properties were investigated. The waste scallop shells were transformed to calcium acetate compounds by reactions with four acetic acid concentrations at ambient temperature until the completely dried powder is obtained. The maximum yield of 87% with short reaction time at a low temperature was observed in the reaction of 60%w/w acetic acid with scallop shells. Thermal transformation reactions of all prepared calcium acetate samples revealed temperature conditions for heating to produce other advanced materials. FTIR and XRD results confirmed the purity and solid phase of all prepared calcium acetate samples, and they were compared with those of literatures and found to be well consistent. The obtained timber-like particles have different sizes depending on the acetic acid concentration. This work reports an easy and low-cost method with no environmental effect to produce cheap calcium products to be used in the industry.
1
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Simple synthesis, kinetics and thermodynamics of rod-like Cu2(OH)PO4 microparticles and rod-like Cu4O(PO4)2 nanoparticles
(2020-08-01)
Kullyakool, Saifon
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Boonchom, Banjong
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Chaiseeda, Kittichai
Rod-like Cu<inf>2</inf>(OH)PO<inf>4</inf> microparticles were synthesized via a simple wet chemical reaction by mixing the solutions of CuSO<inf>4</inf>·5H<inf>2</inf>O and Na<inf>3</inf>PO<inf>4</inf>·12H<inf>2</inf>O at 90 °C for 24 h. Thermal transformation of the prepared Cu<inf>2</inf>(OH)PO<inf>4</inf> microparticles were related to endothermic dehydroxylation and its final decomposed product rod-like Cu<inf>4</inf>O(PO<inf>4</inf>)<inf>2</inf> nanoparticles were obtained. The XRD results indicated that Cu<inf>2</inf>(OH)PO<inf>4</inf> and Cu<inf>4</inf>O(PO<inf>4</inf>)<inf>2</inf> crystallize orthorhombic (space group Pnnm, D<inf>2h</inf> 12) and triclinic (space group P1‾, C<inf>i</inf> 1) phases, respectively. The thermal transformation mechanisms from Cu<inf>2</inf>(OH)PO<inf>4</inf> to Cu<inf>4</inf>O(PO<inf>4</inf>)<inf>2</inf> were expressed thought the relation of the graphical shape of isothermal combined with the non-isothermal multi-heating rate equation and kinetic models (P<inf>3/2</inf> and R<inf>2</inf>) to discuss the change of morphologies from microparticles to nanoparticles. Kinetic parameters and triplet thermodynamic functions of activated compound were determined and fully discussed. The obtained data will be useful for academic scientists and industrial researchers to apply these copper phosphates for special applications.

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