Phosphorus Research Bulletin

Editorial Board

2022 年 38 巻 p. i
発行日: 2022年
公開日: 2022/01/12

DOIhttps://doi.org/10.3363/prb.38.i

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ION RELEASE BEHAVIOR OF SILICOPHOSPHATE GLASSES CONTAINING SIX-FOLD COORDINATED SILICON STRUCTURE

Atsuhiro Miura, Akiko Obata, Toshihiro Kasuga

2022 年 38 巻 p. 1-4
発行日: 2022年
公開日: 2022/01/12

DOIhttps://doi.org/10.3363/prb.38.1

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To facilitate the efficient use of phosphate-based glasses in various biomedical applications, it is essential to understand the effects of ion-releasing in the living body. In this work, the ion-releasing behavior of silicophosphate glass, designed as a supply source of silicate and phosphate ions that are effective for bone formation, was investigated. Two types of P₂O₅-SiO₂-CaO-Na₂O glasses containing 45–50 mol% of P₂O₅ with both four- and six-fold coordinated silicon structures were prepared. The glass with ~50 mol% of P₂O₅ content had a higher proportion of six-fold coordinated silicon structure, and it showed a lower ionic release to a simulated body fluid than that with ~45 mol% P₂O₅ content. The release of the therapeutic ions from the silicophosphate glass can be effectively controlled by choosing their composition.

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REVISITING WET-CHEMICALLY SYNTHESIZED β-TRICALCIUM PHOSPHATE: SOLID-STATE NMR STUDY OF LOCAL STRUCTURE

Toshiisa Konishi

2022 年 38 巻 p. 5-17
発行日: 2022年
公開日: 2022/04/21

DOIhttps://doi.org/10.3363/prb.38.5

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Several parameters, including the pH, ripening time, temperature, and Ca/P molar ratio, affect the crystal phase of wet-chemically synthesized beta-tricalcium phosphate (β-TCP). In previous studies, optimal synthesis conditions for β-TCP have been established. However, the local structure and dissolution of β-TCP remain unclear. As such, we investigated the effects of the ripening time on the local structure and dissolution of β-TCP. Wet-chemical synthesis at 25 °C, a pH of 7.0, and a Ca/P molar ratio of 1.50 over a ripening time of 48 h resulted in the formation of single-phase β-TCP. A solid-state nuclear magnetic resonance analysis revealed two distinct local structures of β-TCP: the conventionally reported broad resonances’ local structure under a ripening time of 48 h and 16 narrow-linewidth resonances’ local structure over a ripening time of 48 h. The narrow-linewidth resonances indicated the ordered vacancies of Ca(4) sites in the β-TCP structure, in contrast to previously reported randomly ordered Ca(4) vacancies. In a buffer solution with a pH of 5.5, the dissolution was higher and heterogeneous for β-TCP with ordered Ca(4) vacancies than for β-TCP with randomly ordered Ca(4) vacancies, and in a buffer solution with a pH of 7.3, the opposite was observed.

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COPPER WHITLOCKITE SYNTHESIZED VIA HYDROTHERMAL TRANSFORMATION OF CALCIUM HYDROGEN PHOSPHATE DIHYDRATE

Toshiisa Konishi, Sadayuki Watanabe

2022 年 38 巻 p. 18-24
発行日: 2022年
公開日: 2022/04/21

DOIhttps://doi.org/10.3363/prb.38.18

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Metal ion substitution in calcium phosphate provides a vehicle for therapeutic delivery of metal ions at low cost and with a long shelf life. The whitlockite structure can incorporate metal ions, which enables the introduction of antibacterial and antiviral agents such as copper ions. The present study describes the synthesis of copper whitlockite (CuWH) via a single-step hydrothermal transformation of calcium hydrogen phosphate dihydrate in the presence of copper ions. Hexahedral morphology of single-phase CuWH was synthesized at 220 °C for 12 h at pH 2.0 in the presence of 5 to 7 mol% Cu²⁺ ions, suggesting that CuWH precipitation was both dose- and pH-dependent. The CuWH structure contained protonated phosphate, which also suggests that Cu²⁺ ions were incorporated not only into the Ca(5) site but also the Ca(4) site. The dissolution test mimicking a bioresorption environment created by osteoclasts showed similar dissolution characteristics of Ca²⁺ and Cu²⁺ ions in acetic acid–sodium acetate buffer solution containing potassium nitrate at pH 5.5.

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EFFECT OF BALL-MILLING TREATMENT ON SINTERABILITY OF HYDROXYAPATITE CERAMICS INCLUDING BONE MINERALS

SHOTA OKITSU, TOMOHIRO YOKOTA, MAMORU AIZAWA

2022 年 38 巻 p. 25-31
発行日: 2022年
公開日: 2022/04/21

DOIhttps://doi.org/10.3363/prb.38.25

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Biological apatite found in the bone and teeth of mammals contains various ions, such as Na⁺, K⁺, Mg²⁺, F^- and CO₃^2-. We have previously developed porous hydroxyapatite ceramics, containing bone minerals (bone HAp). These ceramics showed great bone-forming ability and bio-resorbability; however, their mechanical strengths were in sufficient for clinical application. Thus, we focused on the refinement of raw material powder to improve the strength of the resulting bone HAp ceramics. In particular, we clarified the effect of ball milling time on sinterability of the bone HAp powder. Among the prepared samples, the most easily sinterable powder was prepared after ball milling for 1 hour. This powder showed the smallest particle size with a particle size distribution that was close to a uniform distribution. The compressive strengths of Bone HAp ceramics from powders prepared by ball-milling for 30 minutes and 1 hour were of 55.7 MPa and 63.1 MPa, respectively.

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PREPARATION OF POROUS β-TRICALICUM PHOSPHATE BY FOAMING METHOD USING CELLULOSE NANOFIBERS WITH DIFFERENT MANUFACTURING METHODS AS FOAM STABILIZER

Gai Toyota, Hirobumi Shibata, Kazuaki Hashimoto

2022 年 38 巻 p. 32-36
発行日: 2022年
公開日: 2022/04/21

DOIhttps://doi.org/10.3363/prb.38.32

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In this study, we found that the use of phosphite esterified cellulose nanofibers (CNF-P) in combination with the foaming method can produce porous bodies due to the interaction between nonionic surfactants and hydrophobic/hydrophilic CNF-P. When the foaming method was applied to the water-based slurry, the hydrophilic-lipophilic balance of the nonionic surfactant used was about 11-14.5, indicating that the foam was stable during preparation. Furthermore, it was shown that the addition of CNF-P promoted the formation of both micron-sized pores and macro-sized pores (100-400 μm).

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RESEARCH AND DEVELOPMENTS OF INORGANIC PHOSPHATE MATERIALS WITH HIGH PERFORMANCE

Kiyoshi Itatani

2022 年 38 巻 p. 37-46
発行日: 2022年
公開日: 2022/05/10

DOIhttps://doi.org/10.3363/prb.38.37

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The present author and coworkers have engaged in the research and developments of inorganic phosphate materials with high performance, utilizing the characteristic properties of inorganic phosphates in the forms of crystals and glasses. The present review described our previous research regarding (i) the preparation of fibrous octacalcium phosphate (Ca₈H₂(PO₄)₆∙5H₂O) and hydroxyapatite (Ca₁₀(PO₄)₆(OH)₂; HAp) particles due to the anisotropic crystal growth, (ii) the superplastic deformation of HAp ceramics due to the tensile force applied at high temperatures and (iii) the preparation of phosphors with variety of light emission colors (alkaline earth zirconium phosphates and alkaline earth (oxy)nitrides) and glass encapsulant (M₂O-ZnO-B₂O₃-P₂O₅(-CaF₂) system; M=Li and Na) for the designing of novel light emitting diodes. The present research and developments of phosphate materials in the forms of powder, sintered body and glass could be successfully conducted by the assistance of advanced preparation and analytical techniques.

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ELUTION BEHAVIOR OF DEPHOSPHORAZATION SLAG TO VARIOUS ACIDS AND EFFECT OF ADDITION OF AQUEOUS ALKALI TO ACID ELUATE

Shigeru Sugiyama, Kenta Imanishi, Takeru Ishimoto, Miku Hisai, Naohiro ...

2022 年 38 巻 p. 47-52
発行日: 2022年
公開日: 2022/05/11

DOIhttps://doi.org/10.3363/prb.38.47

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We recently developed a method for efficiently recovering phosphoric acid from dephosphorization slag. The most important processes in this recovery technique involve elution of the dephosphorization slag into an acid solution (acid-elution process) and the addition of an alkali to the acid eluate to form a precipitate (alkali-precipitation process). Ultimately, we settled the use of an aqueous nitric acid solution for the acid-elution step, while an aqueous ammonia solution proved to be the optimal choice to accomplish alkali precipitation. Herein, we describe the procedures used to compare the utility of nitric acid with that of hydrochloric acid, sulfuric acid, and citric acid in the acid-elution process, and describe our comparison of an aqueous sodium hydroxide with that of an aqueous ammonia in the alkali-precipitation process. Finally, we summarize our findings on the acids and alkalis that proved to be suitable for this technology.

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UPTAKE AND RELEASE OF SODIUM DIPHOSPHATE BY A CHLORIDE-TYPE LAYERED DOUBLE HYDROXIDE

Aki Hayashi, Sawako Otsu, Hitomi Kamiji, Aki Yoshioka, Shin Ando, Chie ...

2022 年 38 巻 p. 53-59
発行日: 2022年
公開日: 2022/09/13

DOIhttps://doi.org/10.3363/prb.38.53

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In this study, we investigated the uptake and release of sodium diphosphate (Na₄P₂O₇, P2) by a chloride-type layered double hydroxide (LDH-Cl) with good anion exchange properties. The pH of the P2 aqueous solution produced the strongest effect on the P2 uptake. At pH 5, the maximum uptake was 1.9 mmol/g (LDH-P2(1.9)), and the minimum uptake amount obtained at pH 11 was 0.8 mmol/g (LDH-P2(0.8)). The maximum release rate of P2 determined for LDH-P2(0.8) in a NaCl aqueous solution at a NaCl(aq) concentration of 4 M, temperature of 24 °C, and reaction time of 1 h was 12%. After repeating the release process four times under these conditions, the cumulative P2 release rate increased to 22%. Meanwhile, the cumulative release rate of P2 in a Na2CO3 aqueous solution determined for LDH-P2(0.8) was 90%, which exceeded the value obtained for the NaCl aqueous solution.

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PHOSPHORUS RECOVERY FROM SEWAGE-SLUDGE MOLTEN SLAG USING A COMBINATION OF ACID-DISSOLUTION, ALKALI-PRECIPITATION, AND ION-EXCHANGE

Shigeru Sugiyama, Li-Hao Hsiao, Taizo Tokunaga, Takumi Hashimoto, Masa ...

2022 年 38 巻 p. 60-66
発行日: 2022年
公開日: 2023/02/21

DOIhttps://doi.org/10.3363/prb.38.60

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We recently reported an efficient procedure for recovering phosphoric acid from dephosphorization slag. This recovery procedure consists of a combination of the following four processes: (1) A first dissolution process of slag in a nitric acid solution; (2) a precipitation process then adds ammonia to the obtained eluate; (3) a second dissolution process dissolves the precipitation from the nitric acid eluate; and, (4) the final process involves ion exchange in which the obtained eluate is passed through an ion exchange resin. In the present study, this recovery procedure was applied to concentrate and recover phosphorus from sewage-sludge molten slag, which is an unused resource that should be considered a new resource for phosphorus. As a result, our procedure for recovery from dephosphorization slag was viable following two revisions. Initially, the time for the first dissolution process was extended from 0.2 h to 1 h, but 0.2 h proved to be the optimum time for dephosphorization slag. Next, we discovered it was better to perform the filtration one day after adding the ammonia instead of immediately after adding it. The other two processes could be treated under substantially the same conditions as in the case of dephosphorization slag, and high-purity phosphorus was obtained.

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