Phosphorus Research Bulletin

INTERCALATION OF ORGANIC MOLELECULES INTO LAYERED PHOSPHATES

CORRELATION BETWEEN STRUCTUE AND FUNCTION

Hirokazu Nakayama

2009 Volume 23 Pages 1-9
Published: 2009
Released on J-STAGE: May 02, 2009

DOIhttps://doi.org/10.3363/prb.23.1

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Precise investigation of intercalation compounds of layered phosphates by solid state NMR could explore the microscopic picture of intercalation phenomena. By ³¹P solid state NMR experiment, type of layered phosphate and existence of various phosphates, H₂PO₄^-, HPO₄^2-, and PO₄^3- groups, can be distinguished. The microscopic picture of diethylenetriamine-intercalated α-zirconium phosphate, and its mechanism can be obtained by ¹³C and ³¹P solid state NMR. Furthermore, the adsorption of carboxylic acids by diethylenetriamine-intercalated α-zirconium phosphate and the exchange of methylene blue with butylamine in butylamine-intercalated α-zirconium phosphate can be clarified microscopically.

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MECHANOCHEMICAL PROPERTIES OF OCTACALCIUM PHOSPHATE AND BRUSHITE

Hideki Monma, Toshinori Okura, Yoshihiro Hara, Yusuke Moriyoshi

2009 Volume 23 Pages 10-14
Published: 2009
Released on J-STAGE: May 02, 2009

DOIhttps://doi.org/10.3363/prb.23.10

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Crystalline layer-structured octacalcium phosphate (Ca₈(HPO₄)₂(PO₄)₄ 5H₂O, OCP) and brushite (CaHPO₄ 2H₂O, DCPD) were mechanochemically ground. The crystalline XRD pattern of OCP was weakened with grinding and reached almost amorphously after 72 h. However, the amorphously ground OCP possessed IR spectroscopic and thermogravimetric characteristics of OCP. On the other hand, DCPD was dehydrated to monetite (CaHPO₄) by grinding above 4 h. As-prepared OCP particles consisting of aggregates of fine primary thin blade crystals changed to amorphous-like sub-micron spherical particles by grinding. DCPD platy crystals changed to aggregates of very fine primary particles.

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REMOVAL OF AQUEOUS AMMONIUM FROM INDUSTRIAL WASTEWATER WITH MAGNESIUM HYDROGEN PHOSPHATE

Shigeru Sugiyama, Tomoyuki Manabe, Dai Ioka, Keizo Nakagawa, Ken-Ichir ...

2009 Volume 23 Pages 15-19
Published: 2009
Released on J-STAGE: May 02, 2009

DOIhttps://doi.org/10.3363/prb.23.15

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In the present study, it is described that the removal of aqueous ammonium in wastewater released from the steel industry and thermal power plant is possible in using powder MgHPO₄ while the removal nature depends on the solution pH and various contaminant in the wastewater. The removal rate of aqueous ammonium increased with increase of an initial solution pH. Although apparent removal rate increased upon adding phenol that was contained in wastewater from steel industry, it was found that an addition of an excess amount of NaOH into the solution but not phenol directly contributed to the increase of the removal rate. The removal amount decreased upon adding SO₄^2- and Ca²⁺ that were in wastewater from the thermal power plant.

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SYNTHESIS AND ELECTRICAL CONDUCTIVITY OF TETRA-VALENT CERIUM POLYPHOSPHATE BULKS

Hiroaki Onoda, Yousuke Inagaki, Akihide Kuwabara, Naoto Kitamura, Koji ...

2009 Volume 23 Pages 20-24
Published: 2009
Released on J-STAGE: May 02, 2009

DOIhttps://doi.org/10.3363/prb.23.20

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Tetra-valent cerium phosphate was synthesized from cerium oxide and phosphoric acid by heating. The sintering processes, pressure-less sintering (PLS), spark plasma sintering (SPS), and hydrothermal hot pressing (HHP), were tried to obtain polyphosphate bulks. Furthermore, the electrical conductivity of cerium polyphosphate bulks was investigated. Tetra-valent cerium phosphate was synthesized by heating at 700 °C for 20 hours. The hydrothermal hot pressing process was the suitable method to synthesize the tetra-valent cerium phosphate bulk. Y doped Ce(PO₃)₄ had higher conductivity than other rare earth phosphates. A part of tetra-valent cerium cation was considered to reduce tri-valent cerium cation and then to work as a dopant.

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HYDROXYAPATITE CERAMICS FOR MEDICAL APPLICATION PREPARED BY HYDROTHEMAL METHOD

Koji Ioku, Masanobu Kamitakahara

2009 Volume 23 Pages 25-30
Published: 2009
Released on J-STAGE: May 02, 2009

DOIhttps://doi.org/10.3363/prb.23.25

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The hydrothermal method enables us to prepare well crystallized, compositionally homogeneous, uniform and easily sinterable powders due to the effects of the high temperature-high pressure aqueous solutions. This method was applied for preparation of hydroxyapatite ceramics as biomaterials. Hydroxyapatite dense ceramics prepared by the sintering method using HIP or SPS from nano-sized single crystals showed transparency. Transparent hydroxyapatite ceramics enabled the direct observation of living cells. Hydroxyapatite porous ceramics and granules with tailored crystal surface were prepared by the hydrothermal vapor exposure method at temperatures below 200 °C. Porous ceramics and granules of hydroxyapatite with controlled crystal surface should be suitable for bone-repairing materials, for scaffold of cultured bone, for bone graft material and for drug delivery system (DDS). They should have the advantage of adsorptive activity and osteoconductivity in comparison with the conventional sintered hydroxyapatite materials with random crystal surface.

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TRANSITORY NATURE OF OCTACALCIUM PHOSPHATE IN PHYSIOLOGICAL MILIEU AND ITS OSTEOCONDUCTIVE PROPERTY

Osamu Suzuki

2009 Volume 23 Pages 31-34
Published: 2009
Released on J-STAGE: May 02, 2009

DOIhttps://doi.org/10.3363/prb.23.31

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Octacalcium phosphate (OCP) is a metastable salt in physiological pH which tends to convert to hydroxyapatite (HA). Conversion from OCP to HA is also observed if OCP is implanted in various bony sites. From a quantitative viewpoint, the implantation of OCP granules enhances bone regeneration more than that of non-sintered HA or sintered HA granules in rabbit bone marrow spaces or the subperiosteal area of mouse calvaria; in addition, OCP is biodegraded by osteoclast-like cells. OCP promotes differentiation of bone marrow stromal cells to osteoblastic cells. These osteoconductive characteristics may be acquired by the dissolution process associated with the progressive OCP-HA conversion. The biodegradability and osteoconductive characteristics are summarized in relation to the solubility of OCP.

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PREPARATION OF AMMONIUM POLYPHOSPHATE AND ITS APPLICATION TO FLAME RETARDANT

Makoto Watanabe, Makoto Sakurai, Mioko Maeda

2009 Volume 23 Pages 35-44
Published: 2009
Released on J-STAGE: May 02, 2009

DOIhttps://doi.org/10.3363/prb.23.35

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Ammonium polyphosphate forms II, V, and VI have been prepared by new preparation processes using ammonium orthophosphate, urea and/or phosphorus pentaoxide as starting materials. The preparation processes are very useful for a large scale preparation in a factory. These crystal phases of APP showed flame retardant effect to organic polymer materials. The order of flame retardation effect among the phases was V > II > VI ≥ I.

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FABRICATION OF FLUORAPATITE CERAMIC MATERIAL WITH SUBMICROME -45- TER-SIZED GRAINS AND ITS HIGH-TEMPERATURE PLASTIC DEFORMATION

Daisuke Watane, Yoshio Sakka, Ian J. Davies, Seiichiro Koda, Kiyoshi I ...

2009 Volume 23 Pages 45-51
Published: 2009
Released on J-STAGE: May 02, 2009

DOIhttps://doi.org/10.3363/prb.23.45

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The fabrication conditions of high-density fluorapatite (Ca₁₀(PO₄)₆F₂: FAp) ceramic material with submicrometer sized grains were examined by two different techniques, namely pressureless firing and pulse-current pressure firing. Firstly, FAp compact was pressurelessly fired at a temperature between 1000 and 1200 °C for 10 h. The relative density and grain size of the FAp compact fired at 1200 °C achieved 92.6% and 1.8 μm, respectively. In order to enhance the relative density but restrict the grain size below 1 μm, FAp compact was pulse-current pressure fired at a temperature between 900 and 1100 °C for 10 min. The relative density and grain size of the FAp compact were 98.8% and 0.79 μm, respectively, when the temperature increased to 1100 °C. Owing to the simultaneous achievement of high density and restricted grain growth, the tensile strain of the FAp specimen pulse-current pressure fired at 1100 °C for 10 min was investigated and found to attain 70.6% at a test temperature of 1100 °C and a strain rate of 1.48 × 10^-4 s^-1.

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PHOSPHORYLATION OF POLYAMIDOAMINE DENDRIMERS WITH CYCLO-TRIPHOSPHATE IN AQUEOUS SOLUTION

Hideko Maeda, Mayumi Matsushita, Mitsutomo Tsuhako, Hiroyuki Nariai, H ...

2009 Volume 23 Pages 52-56
Published: 2009
Released on J-STAGE: May 02, 2009

DOIhttps://doi.org/10.3363/prb.23.52

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Phosphorylation of polyamidoamine dendrimers has been achieved using inorganic cyclo-triphosphate in aqueous solution. In the phosphorylation of polyamidoamine dendrimers, triphosphate derivatives of them were synthesized with the yields of more than 95%. For polyamidoamine dendrimer with four terminal amino groups, two phosphorylated products were obtained.

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FORMATION OF POLY-L-ARGININE - HYDROXYAPATITE NANOPARTICLE COMPLEXES AND INTERACTIONS BETWEEN COMPLEXES AND LIPIDBILAYER MEMBRANES.

Satoru Ueno, Saburo Shimabayashi

2009 Volume 23 Pages 57-62
Published: 2009
Released on J-STAGE: May 02, 2009

DOIhttps://doi.org/10.3363/prb.23.57

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A certain molecule permeable to a phospholipid bilayer membranes (cell or endosormal membrane ) is a useful carrier (i.e. vector) for drugs (especially polymeric drugs). We prepared two types of the hydroxyapatite nanoparticle - poly-L-arginine complexes in a different solvent, which were used as the probes for the study on the translocationability through the negatively charged phospholipid bilayer membranes by means of a confocal laser scanning microscope (CLSM). CLSM observation and secondary structure of poly-L-arginine moieties which estimated by FT-IR measurement showed the transformation of the polypeptide secondary structure on the surface of liposome is on important key step of membrane transfer of the these complexes.

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SYNTHESIS OF PLATE-LIKE CERIUM PHOSPHATES AND THEIR PHOTOCHEMICAL PROPERTIES VIA SOFT CHEMICAL REACTIONS

Tsugio Sato, Midori Saito, Chigusa Sato, Shu Yin

2009 Volume 23 Pages 63-66
Published: 2009
Released on J-STAGE: May 02, 2009

DOIhttps://doi.org/10.3363/prb.23.63

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Plate-like cerium phosphates have attracted attention because of their unique UV-shielding ability with low photocatalytic activity and excellent comfort when applied on skin. Plate-like hydrated cerium phosphate, Ce₂(PO₄)₂HPO₄·H₂O, ca 3 μm in diameter, was obtained by the hydrothermal reaction of Ce(SO₄)₂ in H₃PO₄ aqueous solution at 200 °C for 3 h. Ce₂(PO₄)₂HPO₄·H₂O transformed to CeP₂O₇-CePO₄, mixture around 700 °C with the transcription of plate-like morphology. Plate-like CePO₄ and CeP₂O₇ were also synthesized as single phase by heating plate-like Ce₂(PO₄)₂HPO₄·H₂O with cerium hydroxide and NH₄H₂PO₄, respectively. Plate-like cerium phosphates showed excellent comfort, absorption ability of UV-light and lower oxidation catalytic activity than undoped ceria. The UV-shielding ability of them was in the order Ce₂(PO₄)₂HPO₄·H₂O > CeP₂O₇ > CeP₂O₇-CePO₄ mixture > CePO₄ > K_0.8Li_0.266Ti_1.734O4.

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CHEMICAL PREPARATION, THERMAL BEHAVIOR, KINETIC AND INFRARED STUDIES AND QUANTUM CHEMICAL CALCULATIONS OF Ba₃(P₃O₉)₂6H₂O

S. Belaaouad, Y. Lahrir, S. Sarhane, M. Tridane

2009 Volume 23 Pages 67-75
Published: 2009
Released on J-STAGE: May 02, 2009

DOIhttps://doi.org/10.3363/prb.23.67

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Chemical preparation, thermal behavior, kinetic and IR studies and quantum chemical calculations are given for the cyclotriphosphate Ba₃(P₃O₉)₂6H₂O. Ba₃(P₃O₉)₂6H₂O is triclinic P-1 with the following unit-cell dimensions : a = 7.547(4)Å, b = 11.975(6))Å, c = 13.068(8))Å, α= 108.58(8)°, β= 100.35(8)°, γ= 95.54(8)°, Z = 2. Ba₃(P₃O₉)₂6H₂O has never been studied except its crystallographic characterization. Ba₃(P₃O₉)₂6H₂O is stable, in the conditions of temperature and pressure of our laboratory, until 80°C. It is impossible to dehydrate Ba₃(P₃O₉)₂6H₂O without breaking its rings P₃O₉^3- and leading to amorphous compounds in X-ray diffraction and IR absorption spectrometry. The final product of the dehydration and calcination of Ba₃(P₃O₉)₂6H₂O, under atmospheric pressure, is its long chain polyphosphate form β, β [Ba(PO₃)₂]_∞. β [Ba(PO₃)₂]_∞ is stable until its melting point at 870°C. β [Ba(PO₃)₂]_∞ is prepared otherwise by dry way. β [Ba(PO₃)₂]_∞ has many applications in industry such as corrosion inhibitor.

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Editorial Board

2009 Volume 23 Pages i
Published: 2009
Released on J-STAGE: May 02, 2009

DOIhttps://doi.org/10.3363/prb.23.i

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Erratum: FABRICATION OF FLUORAPATITE CERAMIC MATERIAL WITH SUBMICRO -45- METER-SIZED GRAINS AND ITS HIGH-TEMPERATURE PLASTIC DEFORMATION [Phosphorus Research Bulletin 23, 45-51 (2009)]

Daisuke Watanabe, Yoshio Sakka, Ian J. Davies, Seiichiro Koda, Kiyoshi ...

2009 Volume 23 Pages 76-82
Published: 2009
Released on J-STAGE: May 20, 2009

DOIhttps://doi.org/10.3363/prb.23.76

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The title and one of authors of the article [Phosphorus Research Bulletin 23, 45-51 (2009)] were incorrect because of the editor's mistakes. The corrected name of the author is 'Daisuke Watanabe', and the corrected title is "FABRICATION OF FLUORAPATITE CERAMIC MATERIAL WITH SUBMICROMETER-SIZED GRAINS AND ITS HIGH-TEMPERATURE PLASTIC DEFORMATION".

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SYNTHESIS AND CHARACTERIZATION OF EXPANDED LAYER-SPACING ZIRCONIUM PHOSPHATE BY ION-EXCHANGE AND INTERCALATION PROCESSES

Adly A. Hanna, Ashraf F. Ali, Alaa E. Gad

2009 Volume 23 Pages 83-89
Published: 2009
Released on J-STAGE: August 27, 2009

DOIhttps://doi.org/10.3363/prb.23.83

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In a previous work¹, we prepared α-Zr(HPO₄)₂·2H₂O (ZrP) by direct precipitation, reflux, and by sol-gel method. The results of characterization indicated that the properties of the resultant ZrP samples depended on the method and conditions of preparation as well as on the nature of precursor used. As an important factor governing the use of such layered phosphates, various modifications were done to enlarge the interlayer spacing of α-ZrP (7.6 Å) to be suitable for exchange of large cations. This work aims to modify the interlayer spacing of α-ZrP prepared from zirconium acetylacetonate complex and phosphoric acid. Two routes were used to achieve this goal; the first is by intercalation of acid α-ZrP with n-butyl amine in its vapor-saturated atmosphere. The second route is by performing ion-exchange of the α-ZrP protons by different cations.

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PREPARATION, CHARACTERIZATION AND ELECTRICAL CONDUCTIVITY OF CONDENSED SODIUM PHOSPHATES

Adly A. Hanna, Marwa A. Sherief, Reham M. M. Morsi

2009 Volume 23 Pages 90-93
Published: 2009
Released on J-STAGE: August 27, 2009

DOIhttps://doi.org/10.3363/prb.23.90

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Condensed phosphates are generally prepared from their simple phosphates by heating at high temperature. The formation, structure and the morphology of the resultant condensed phosphates depend on the kind of inorganic cations as well as the conditions of preparation, temperature, heating time, and cooling rate of the melt. Condensed sodium phosphates were prepared by thermal treatment of NaH₂PO₄, the effect of calcinated temperature, also was studied. The products were characterized by X-ray diffraction, IR spectrum, Transmission electron microscope(TEM).The results indicate that the produced phosphate depends on the heat of calcinations. The electrical conductivity of the product was measured in range from room temperature up to 300 °C. The measurements show that the condensed phosphates tend to be a semiconductor material. The calculation of the activation energies indicates that the mechanism of conductivity is photonic or electronic conduction at low temperatures and ionic mechanism at high temperatures.

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INTERFACE BONDING OF α-TRICALCIUM PHOSPHATE CERAMIC COUPLE SOAKED IN WATER AND SIMULATED BODY FLUID

Hideki Monma, Yusuke Moriyoshi, Toshinori Okura

2009 Volume 23 Pages 94-97
Published: 2009
Released on J-STAGE: October 30, 2009

DOIhttps://doi.org/10.3363/prb.23.94

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The interface bonding of α-tricalcium phosphate (αT) porous ceramic couple in H₂O and SBF was investigated. The bonding occurred with the entanglements of HAp microcrystals formed in the interface narrow space between αT ceramic couple. The HAp had calcium-deficient compositions with HPO₄^2- and/or CO₃^2-. The HAp formation extent was in the order, open free surface « interface narrow space, which was assumed to depend on how ease the supersaturated solution conditions with respect to HAp was realized.

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