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.

Waste oyster shells were utilized to produce calcium carbonate (CaCO₃) by grinding. This CaCO₃ was then reacted with acetic acid to yield calcium acetate monohydrate (Ca(CH₃COO)₂·H₂O). Both CaCO₃ and Ca(CH₃COO)₂·H₂O were used as precursors for synthesizing calcium oxide (CaO) through thermal decomposition at 900 °C and 750 °C, respectively. The yields of CaO from both precursors, determined through calcination experiments and thermogravimetric analysis (TGA), exceeded 100% due to the high purity of the raw agents and the formation of calcium hydroxide (Ca(OH)₂). X-ray fluorescence (XRF) analysis revealed a CaO content of 87.8% for CaO-CC and 91.5% for CaO-CA, indicating the purity and contamination levels. X-ray diffraction (XRD) patterns confirmed the presence of CaO and minor peaks of Ca(OH)₂, attributed to moisture adsorption. Fourier-transform infrared (FTIR) spectroscopy identified the vibrational characteristics of the Ca-O bond. Scanning electron microscopy (SEM) showed similar morphologies for both CaO-CC and CaO-CA, with CaO-CA displaying a significant amount of rod-like crystals. Based on these results, calcium acetate monohydrate (CA) is recommended as the superior precursor for synthesizing high-purity CaO, offering advantages for various applications.

Calcium dihydrogen phosphate monohydrate (Ca(H₂PO₄)₂·H₂O) (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(H₂PO₄)₂·H₂O. Conversely, the non-soluble products (NSP30, NSP50, and NSP80) were observed as calcium hydrogen phosphate dihydrate (CaHPO₄·2H₂O). 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 HPO₄²⁻, H₂PO₄⁻, and H₂O existed in CaHPO₄·2H₂O and Ca(H₂PO₄)₂·H₂O. Three thermal dehydration steps of Ca(H₂PO₄)₂·H₂O (physisorbed water, polycondensation, and re-polycondensation) were observed. Ca(H₂PO₄)₂ and CaH₂P₂O₇ are the thermodecomposed products from the first and second steps, whereas the final product is CaP₂O₆.

A green and mild chemical reaction of calcium citrate (CC) was successfully prepared from reactions between mussel shell waste and citric acid in the presence of acetone (AC), ethanol (Et), and isopropyl alcohol (IPA). All the synthesized CCs contained the same functional groups such as citrate (C₆H₅O₇³⁻), water (H₂O), and calcium–oxygen (Ca–O). However, the differences in the spectra pointed out the differences in the crystal environment and structure of CCs. CC-AC and CC-IPA mainly crystallized in the monoclinic [Ca₃(C₆H₅O₇)₂(H₂O)₂]·2H₂O crystal system, whereas CC-Et mainly crystallized in the triclinic Ca₃(C₆H₅O₇)₂∙(H₂O)₄ structure. The molecular alignments of triclinic CC-Et were different from monoclinic CC-AC and CC-IPA, resulting in differences in thermal behaviors. Two dehydration steps were observed for the monoclinic CC-AC and CC-IPA, whereas the triclinic CC-Et showed a single dehydration process. The TG mass losses further demonstrated that anhydrous Ca₃(C₆H₅O₇)₂ phase, in addition to the Ca₃(C₆H₅O₇)₂∙4H₂O, was also observed for CC-AC and CC-IPA, whereas CC-Et contained a single Ca₃(C₆H₅O₇)₂∙(H₂O)₄ phase. The morphologies of CC-AC and CC-IPA also differed from that of CC-Et. The differences in some properties of the synthesized CCs could be attributed to the change in the supersaturation state of the reaction solution. Due to the superior polarity, ethanol is more compatible with citric acid. The presence of ethanol could suppress the supersaturation rate of the reaction solution, causing the modulation of the precipitation mechanisms and reducing the particle growth rate of CC-Et, thereby explaining the difference in vibrational, structural, thermal, and morphological characteristics of CC-Et, compared to CC-AC and CC-IPA.

Aragonite calcium carbonate (CaCO₃), derived from cockle shell waste, was successfully used as a renewable calcium source to synthesize calcium citrate (CCT) using citric acid (C₆H₈O₇). The three CCT products (CCT-2, CCT-3, and CCT-4) were prepared using three different acid concentrations: 2, 3, and 4 M. The physicochemical characteristics of the newly synthesized CCT were investigated. Fourier-transform infrared (FTIR) spectra revealed the vibrational modes of the citrate anionic group (C₆H₅O₇³⁻), which preliminarily confirmed the characteristics of CCT. However, X-ray diffraction (XRD) revealed that the concentration of citric acid altered the structural property and the chemical formula of the synthesized CCT. Employing 2 M citric acid, a pure tetra-hydrated phase (Ca₃(C₆H₅O₇)₂·4H₂O, earlandite mineral) was obtained. However, a mixture of hydrated (Ca₃(C₆H₅O₇)₂·4H₂O) and anhydrous (Ca₃(C₆H₅O₇)₂) phases was precipitated when 3 and 4 M citric acid was used in the preparation process. The lower mass loss observed in the thermogravimetric analysis (TGA) of CCT-3 and CCT-4 compared to that of CCT-2 further confirmed that CCT-3 and CCT-4 were composed of hydrated and anhydrous CCTs. The synthesized CCT decomposed in four major processes: the first dehydration, the second dehydration, CaCO₃ formation, and decarbonization, generating calcium oxide (CaO) as the final product. X-ray fluorescence (XRF) results showed that the CCT mainly consisted of CaO with a quantity of >98%. The scanning electron microscopic (SEM) image revealed the irregular plate-like CCT crystallites. The concentration of citric acid is a key factor that influences the productive parameters of CCT, including production yield, reaction time, and solubility. 2 M citric acid provided the optimal balance between productivity and cost-effectiveness, with the highest yield and soluble fraction and the lowest reaction time. The results suggest that the preparation of CCT from cockle shell waste can potentially replace the use of commercial calcite from mining, which is a limited and non-renewable resource.

In this paper, mussel shells were used to produce chitin, chitosan, and calcium acetate using chemical processes, searching for an alternative environmentally friendly biopolymer and calcium source. Mussel shells were treated with acetic acid as a demineralizing agent, resulting in separate solid fractions and calcium solution. The solid was further purified to produce chitin by deproteinization and decolorization processes, and then the deacetylation process was used to obtain chitosan. The calcium solution was evaporated to produce calcium acetate powder. The yields of extracted chitin, chitosan, and calcium acetate from 100 g of mussel shells were 2.98, 2.70, and 165.23 g, respectively. The prepared chitin, chitosan, and calcium acetate were analyzed by Fourier transform infrared (FTIR) spectrophotometry, X-ray diffraction (XRD), thermogravimetric analysis (TGA), and scanning electron microscope (SEM) to confirm the chemical and physical properties. The analysis results of chitin and chitosan revealed the similarity to chitosan derived from crustaceans and insects in terms of functional group, structure and morphologies. The prepared calcium acetate shows FTIR and XRD data corresponding to calcium acetate monohydrate (Ca(CH₃COO)₂·H₂O) similar to synthesized calcium acetate in previous research. In addition, the mineral contents of calcium acetate identified by X-ray fluorescence (XRF) analysis exhibit 97.8% CaO with non-toxic impurities. This work demonstrated the potential of the production process of chitin, chitosan, and calcium acetate for the development of a sustainable industrial process with competitive functional performance against the commercial chitin and chitosan production process using crustacean shells and supported the implementation of a circular economy.