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    Extraction of Chitin, Chitosan, and Calcium Acetate from Mussel Shells for Sustainable Waste Management
    (2025-08-01)
    Seangarun, Chaowared
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    ; ;
    Laohavisuti, Nongnuch
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    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(CH<inf>3</inf>COO)<inf>2</inf>·H<inf>2</inf>O) 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.
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    Green Ca-source of cockle shells converted to calcium acetate for environmental sustainability
    (2024-06-15) ;
    Seangarun, Chaowared
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    Ohpasee, Natee
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    Laohavisuti, Nongnuch
    This work aimed to synthesize and characterize the calcium acetate monohydrate (Ca(CH<inf>3</inf>COO)<inf>2</inf>·H<inf>2</inf>O) from the exothermic reaction between CaCO<inf>3</inf> powder derived from cockle shells with three different acetic acids (8, 10, and 12 mol L<sup>−1</sup>) concentrations by the rapid and easy process without pH and temperature control to lead to cheap chemical production. The physicochemical characteristics of all synthesized Ca(CH<inf>3</inf>COO)<inf>2</inf>·H<inf>2</inf>O samples are investigated based on the chemical compositions, crystal structures, vibrational characteristics, morphologies, and thermal behavior to confirm the target compound. A suitable concentration of 10 mol L<sup>−1</sup> CH<inf>3</inf>COOH was chosen to produce Ca(CH<inf>3</inf>COO)<inf>2</inf>·H<inf>2</inf>O with the highest yield (96.30 %), maximum calcium content (96.2 % CaO) with lower impurities, and time consumption of 17 h. The calcium acetate product obtained from cockle shells in this work shows differences in thermal stability, morphological structure purity, %yield, and metal contamination with those reported obtained from other sources and another shell type in the previous work. This research investigates the transformation of cockle shell waste into CaCO<inf>3</inf> for the production of calcium acetate, aiming to address environmental sustainability concerns by reducing the use of calcium ore resources and greenhouse gas emissions.
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    A Facile Method to Synthesize b-Oriented Silicalite-1 Thin Film
    (2022-05-01) ;
    Woramongkolchai, Somsak
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    Saowsupa, Sairoong
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    Silicalite-1 thin film was prepared with the following batch composition—3TPAOH:25TEOS: 1450H<inf>2</inf> O:100EtOH—and synthesized using the hydrothermal technique. Silicalite-1 colloidal crystals were successfully coated on the surface of the silica substrate by the dip-coating method. The investigation of silicalite-1 thin film with organic structure-directing agents (SDA), using a seeding technique with various colloidal seed concentrations, number of dip-coating steps, and crystallization time, were systematically discussed and obtained interesting results. Silicalite-1 powder and Silicalite-1 membrane, the patterns of which showed a unique characteristic crystallography of MFI topology, were characterized by XRD, which indicated the preferred orientation along the b-axis perpendicular to the substrate surface. The morphology and crystal size aspect of Silicalite-1 were also examined by a scanning electron microscope (SEM).
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    Crystal growth of AlPO-5, AlPO-15, and AlPO-21 from aluminum foil
    (2008-03-01) ;
    Wang, Xiqu
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    Jacobson, Allan J.
    Single crystals of AlPO-n (AlPO-5, AlPO-15 and AlPO-21) have been grown using Al metal as the aluminum source and appropriate organic amines as templates. The influence of synthesis conditions on the crystal size has been studied by systematically changing temperature, the organic template and the gel composition. © 2007 Elsevier Inc. All rights reserved.
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    Vitrimer-like of poly (glycerol sebacate) by using zinc acetate, zinc oxide and Amberlyst as catalysts
    (2023-01-01) ;
    Saowsupa, Sairoong
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    Polyglycerol sebacate (PGS) is elastomeric biodegradable polymer with potential biomedical and green packaging applications. This study focuses on the synthesis of vitrimer-like PGS utilizing various catalysts, including Zinc acetate, Zinc oxide and Amberlyst-15. The investigation of vitrimer-like of PGS polymer by polycondensation of glycerol and sebacic acid with various molar ratio of 1:1, 1:1.25 and 1:1.5 will be studied. The synthetic time and temperature were controlled at 72 h, 120 <sup>°</sup>C, respectively. The prepolymer of PGS had a weight-average molecular weight (Mw.) of 1743. The result of functional group was confirmed by Fourier transforms Infrared spectroscopy (FTIR). The intense C[dbnd]O stretch at 1737 cm<sup>−1</sup> confirms the formation of ester bonds. The intense OH stretch at 3454 cm<sup>−1</sup> indicated hydroxyl groups from hydrogen bonded. When the quantity of catalyst is increased, the results of hardness are rising but swelling (%) becomes lower. The results showed a polymer network has higher cross-link when the catalyst increases. In addition, the proton nuclear magnetic resonance spectroscopy (<sup>1</sup>H NMR) analysis found that PGS using catalyst does not have peaks of glycerol.
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    Influence of Organic Solvent on the Physicochemical Characteristics of Calcium Citrate Prepared from Mussel Shell Waste
    (2025-06-01)
    Punthipayanon, Sirichet
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    Chanwetprasat, Pantita
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    ; ;
    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 (C<inf>6</inf>H<inf>5</inf>O<inf>7</inf><sup>3−</sup>), water (H<inf>2</inf>O), 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 [Ca<inf>3</inf>(C<inf>6</inf>H<inf>5</inf>O<inf>7</inf>)<inf>2</inf>(H<inf>2</inf>O)<inf>2</inf>]·2H<inf>2</inf>O crystal system, whereas CC-Et mainly crystallized in the triclinic Ca<inf>3</inf>(C<inf>6</inf>H<inf>5</inf>O<inf>7</inf>)<inf>2</inf>∙(H<inf>2</inf>O)<inf>4</inf> 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 Ca<inf>3</inf>(C<inf>6</inf>H<inf>5</inf>O<inf>7</inf>)<inf>2</inf> phase, in addition to the Ca<inf>3</inf>(C<inf>6</inf>H<inf>5</inf>O<inf>7</inf>)<inf>2</inf>∙4H<inf>2</inf>O, was also observed for CC-AC and CC-IPA, whereas CC-Et contained a single Ca<inf>3</inf>(C<inf>6</inf>H<inf>5</inf>O<inf>7</inf>)<inf>2</inf>∙(H<inf>2</inf>O)<inf>4</inf> 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.
      1
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    Characterization, Kinetic Using Deconvolution Techniques and Thermodynamic Study of Synthetic MgHPO4·3H2O
    (2023-04-01)
    Kullyakool, Saifon
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    Thompho, Somphob
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    MgHPO<inf>4</inf>·3H<inf>2</inf>O was synthesized via a simple wet reaction and transformed to its final decomposed product, Mg<inf>2</inf>P<inf>2</inf>O<inf>7</inf> at 873 K. The thermal properties, vibrational modes of block units, and solid phases of the synthetic compounds have been investigated by TG/DTG/DTA, FTIR, and XRD techniques. The temperature dependence of thermodynamic properties estimated from the DSC data occurred in two regions (before and after the dehydration reaction) indicating a characteristic of the prepared MgHPO<inf>4</inf>·3H<inf>2</inf>O sample. The dehydration reactions of 3.5 mol of water molecules in the structure overlapped in the temperature of 363–823 K and showed the phase transition at 921 K as revealed by TG/DTG/DTA. The deconvolution technique using the newly modified co-mathematical functions was used to separate the overlapped dehydration steps in the DTG curve, which obtained the three steps. Only the first and second steps were estimated using kinetic triplet parameters (E<inf>a</inf>, A, and model), which indicate the single dehydration mechanism with the A<inf>1.25</inf> model and the multi-step of a parallel mechanism with the A<inf>1.6</inf> model, respectively. The data of kinetics and thermodynamics play key points in theoretical study, application development, and industrial production of magnesium phosphates as a theoretical basis.
      1
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    Simple Rapid Production of Calcium Acetate Lactate from Scallop Shell Waste for Agricultural Application
    (2025-05-01)
    Mongkol, Sorakit
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    ; ;
    Laohavisuti, Nongnuch
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    Calcium acetate lactate (CAL) was rapidly synthesized for the first time using the reaction between the scallop shell-derived calcium carbonate (CaCO<inf>3</inf>) and the binary phase of acetic and lactic acids. Calcium acetate (CA) and calcium lactate (CL) synthesized from the reaction of scallop shell-derived CaCO<inf>3</inf> with each acid by similarity routes are compared with the obtained CAL product. The production yields are 88.24, 79.17, and 96.44%, whereas the solubilities are 93.77, 90.18, and 95.08% for CA, CL, and CAL, respectively. All the synthesized CA, CL, and CAL samples were characterized and confirmed by X-ray fluorescence (XRF) to examine the calcium main element and other impurities of minor elements, X-ray diffraction (XRD) to investigate the crystallography, Fourier transform infrared (FTIR) to characterize the vibrational characteristics of the functional groups, scanning electron microscope (SEM) to observe the sample morphologies, and the thermogravimetric analysis (TGA) to investigate the thermal decomposition processes of samples. The experimental results pointed out that the synthesized CA, CL, and CAL were the monohydrate, pentahydrate, and dihydrate forms with chemical formulae of Ca(CH<inf>3</inf>COO)<inf>2</inf>·H<inf>2</inf>O, Ca(CH<inf>3</inf>CHOHCOO)<inf>2</inf>·5H<inf>2</inf>O, and Ca(CH<inf>3</inf>COO)(CH<inf>3</inf>CHOHCOO)·2H<inf>2</inf>O, respectively. The final thermal decomposition product of all calcium compounds was calcium oxide (CaO). The CAL sample’s vibrational characteristics, crystal phases, and morphologies show the binary acetate and lactate anion phases, confirming the new binary anionic calcium acetate lactate obtained. In conclusion, this research proposes an easy and low-cost technique to prepare a new valuable CAL compound using scallop shell waste as a cheap and renewable calcium source.
      1
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    Sustainable Synthesis of Calcium Propionate from Cockle Shell Biowaste for Food Additive Production
    (2026-06-01)
    Seangarun, Chaowared
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    ; ; ;
    Punthipayanon, Sirichet
    Calcium propionate (Ca(CH<inf>3</inf>CH<inf>2</inf>COO)<inf>2</inf>) was successfully synthesized from cockle shell biowaste through a reaction with propionic acid at concentrations of 80%, 90%, and 99%, valorizing seafood processing biowaste as a renewable calcium source in support of circular economy principles. The synthesis was conducted at ambient temperature with a fixed CaCO<inf>3</inf>: propionic acid molar ratio of 1:2, enabling rapid reaction completion without external heating or complex purification steps. The prepared samples were characterized by FTIR, XRD, TGA, and SEM techniques, which confirmed the formation of calcium propionate monohydrate (Ca(CH<inf>3</inf>CH<inf>2</inf>COO)<inf>2</inf>·H<inf>2</inf>O), while XRF confirmed more than 97 wt% CaO across all samples with non-toxic impurities corresponding to compositional requirements for food additive calcium propionate (E282). The sample prepared using 80% propionic acid exhibited the highest yield (90.24%) and soluble percentage (98.23%). The proposed approach demonstrates an effective valorization of cockle shell waste into a food additive, calcium propionate, offering advantages in terms of sustainability, cost efficiency, and scalability, and highlighting its strong potential for industrial food additive production within a circular economy framework.
      2
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    Low-Cost and Rapid Production of Calcium Formate from Cockle Shell Waste for Sustainable Waste Recycling
    (2026-04-01)
    Seangarun, Chaowared
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    ; ; ;
    Punthipayanon, Sirichet
    Calcium formate (Ca(HCOO)<inf>2</inf>) is an important industrial chemical widely used in construction, feed additives, and various chemical processes. In this work, calcium formate was synthesized from cockle shell waste and concentrated formic acid (50%, 60%, and 70% w/w) by a simple, rapid, low-cost, and environmentally friendly process, denoted as CF50, CF60, and CF70, respectively. The chemical and physical properties of as-synthesized calcium formate using cockle shells as a renewable calcium source were investigated by Fourier transform infrared (FT-IR), X-ray diffraction (XRD), X-ray fluorescence (XRF), Thermal gravimetric analysis (TGA), and scanning electron microscopy (SEM) techniques. The FTIR and XRD results revealed that the samples prepared using 50% and 60% formic acid produced well-crystallized α-calcium formate. In contrast, the reaction using 70% formic acid generated a strongly exothermic reaction, which hindered the complete conversion of calcium carbonate and resulted in the presence of residual CaCO<inf>3</inf> in the final product. Similarly, the SEM images of the CF50 and CF60 samples show the slick surface of orthorhombic crystals of calcium formate; on the other hand, the SEM image of CF70 shows some small particles of aragonite on the surface of the calcium formate crystals. The 60% formic acid provided the optimal synthesis condition, yielding pure calcium formate with the shortest synthesis time. Overall, the proposed approach provides a simple, rapid, and cost-effective route for producing calcium formate from shell waste. Furthermore, the utilization of cockle shell waste as a renewable calcium source contributes to waste valorization, reduces environmental impacts associated with shell disposal, and minimizes dependence on mined limestone resources, supporting sustainable resource utilization within a circular economy.
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