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1.
Calcium hydroxoaluminate hydrates were precipitated from different sodium hydroxoaluminate and hydroxoaluminate-excess hydroxide solutions at ambient temperature (at CAl = 0.1 to 0.3 M and at XS OH/Al = 0 to above 8). The precipitations were monitored by potentiometric (pH) measurements. Precipitate morphologies were examined by optical microscopy and precipitate compositions were determine by chemical analysis, infra-red spectrophotometry and thermal analysis. Generally at OH/Al ratios of 4 to 4.5 (XS OH/Al = 1 to 1.5), the compound 2 CaO · · Al2O3 · 8 H2O (C2AH8) was precipitated with some aluminium hydroxide; then at OH/Al ratios of 5 to above 11 (XS OH/Al = 2 to above 8), the compound 2 CaO · Al2O3 · 8 H2O was precipitated with increasing amounts of the compound 4 CaO · Al2O3 · 13 H2O (C4AH13).  相似文献   

2.
Magnesium hydroxoaluminate hydrates were precipitated from different sodium hydroxoaluminate and hydroxoaluminate-hydroxide solutions at ambient temperature, at CAl = 0.1 M, OH/Al ratios = 4–9 and XS OH/Al ratios = 1–6. The precipitations were monitored by potentiometric (pH) measurements while the final precipitate compositions were examined by chemical analysis, infra-red spectrophotometry and thermal analysis. At solution OH/Al ratio = 4, the main precipitate phase at 20°C was Mg(H2O)n[Al(OH)4]2 admixed with some Al(OH)3; at solution OH/Al ratio = 5, the main phase was Mg2(H2O)4[Al2(OH)10]; at solution OH/Al ratio = 7, the main phase was Mg4(H2O)n(OH)4[Al2(OH)10] while at solution OH/Al ratio = 9, the main phase was Mg6(H2O)n(OH)8[Al2(OH)10] admixed with some Mg(OH)2. These hydrates were dehydrated at 60–100°C probably to the compounds Mg2[Al2O3(OH)4], Mg4(OH)4[Al2O3(OH)4] and Mg6(OH)8[Al2O3(OH)4], respectively.  相似文献   

3.
Calcium aluminium hydroxides were coprecipitated from different mixed metal cation solutions — at total CM = 0.1 M and Ca/Al2 ratios from 1 to 4 — with sodium hydroxide solution at ambient temperature. The coprecipitations were monitored by potentiometric (pH) titration and the final coprecipitate compositions were examined by chemical analysis, infra-red spectrophotometry and thermal analysis Generally, microcrystalline aluminium hydroxide was first precipitated at pH about 4; this then redissolved on further addition of sodium hydroxide to form hydroxoaluminate anion and polyanion and calcium aluminium hydroxide coprecipitates were formed continuously at pHs from about 9 to above 12. Their compositions were similar to the calcium hydroxoaluminate hydrates formed by direct precipitation from high pH sodium hydroxoaluminate solutions. At Ca/Al2 ratio = 1, the main phase was probably Ca2(H2O)h[Al2(OH)4]2 with some Al(OH)3; At Ca/Al2 ratio = 2, the main phase was probably Ca2(H2O)h[Al2(OH)10] dehydrating to Ca2[Al2O(OH)8]; At Ca/Al2 ratios = 3–4, the main phase was Ca2(H2O)h[Al2(OH)10] with increasing amounts of Ca4(H2O)h(OH)4[Al2(OH)10] and 5–10 percent adsorbed or post-precipitated Ca(OH)2.  相似文献   

4.
Magnesium hydroxoaluminate hydrates were coprecipitated from different mixed metal cation solutions at Mg/Al2 ratios from 1 to 4 by ammonium hydroxide. The coprecipitations were monitored by potentiometric titration and the final precipitate compositions were examined by chemical analysis, X-ray diffraction, infra-red spectrophotometry and thermal analysis. The process of coprecipitation was similar to that for coprecipitation with sodium hydroxide but large excess of ammonium hydroxide was required for complete reaction at pHs from about 8 to 10.
  • At Mg/Al2 = 1, the main phase was probably Mg(H2O)h [Al(OH)4]2;
  • at Mg/Al2 = 2, the main phase was probably Mg2(H2O)h [Al2(OH)10];
  • at Mg/Al2 = 4, the main phase was probably (MgOH4) (H2O)h [Al2(OH)10].
  相似文献   

5.
Zine aluminium hydroxides were coprecipitated from different mixed metal cation solutions, at CM tot = 0.1 M and at Zn/Al2 ratios from 1 to 4, with sodium hydroxide solution. The coprecipitations were monitored by potentiometrie (pH) titration and the final coprecipitate compositions were examined by chemical analysis, infra-red spectrophotometry and thermal analysis. Generally, microcrystalline aluminium hydroxide was first precipitated at pH about 4; this then partially redissolved on further addition of sodium hydroxide (to form hydroxoaluminate anion) and zinc aluminium hydroxide coprecipitates were formed continuously at pHs from 5.5–6 to above 9. Their compositions were similar to the magnesium hydroxoaluminate coprecipitated from magnesium aluminium solutions. At Zn/Al2 ratio = 1, the main phase was probably Zn(H2O)n [Al(OH)4]2; at Zn/Al2 ratio = 2, the main phase was probably Zn2(H2O)n [Al2(OH)10], whereas at Zn/Al2 ratio = 4, the main phase was probably Zn(H2O)n(OH)4[Al2(OH)10].  相似文献   

6.
The precipitation of barium, strontium, calcium and magnesium polymetaphosphate hydrates was studied from aqueous solutions of initial metal salt concentrations from 0.001 to 3 M at 20 °C; equivalent sodium polymetaphosphate solutions were added to the alkaline-earth metal chloride solutions. Precipitate compositions were determined by chemical analysis, paper chromatography, potentiometric analysis, thermogravimetric and differential thermal analysis and infra-red spectrophotometry; final crystallite morphologies and sizes were studied by scanning electron microscopy and X-ray powder diffraction. Nucleation rates and nucleus numbers (at the end of the induction periods) were very high; crystal numbers varied from 1014 to 1015 at the critical concentrations to above 1017 per 1. solution. Crystal growth rates were also very high and varied as the fourth power of the initial metal salt concentration. High molecular-weight metal polymetaphosphate hydrates were precipitated from the more dilute solutions (0.001 to 0.025 M) while increasing amounts of the more soluble intermediate and low molecular-weight products were precipitated from the more concentrated solutions. Washing with cold water removed the tri- and tetralinear and cyclic phosphate products. The magnesium salts were not precipitated even from 3 M aqueous solutions. The precipitates from aqueous (NaPO3(I))n (n = 12) solutions had the compositions (BaP2O6 · 2.5 H2O)6, (SrP2O6 · 3 H2O)n and (CaP2O6 · 4 H2O)n while the magnesium salt precipitate from 20 percent aqueous acetone solution had the composition (MgP2O6 · 4 H2O)n, the precipitate n values varied from 19 to 13. The precipitates from aqueous (NaPO3(II))n (n = 20) solutions contained 0.5n to n additional adsorbed water molecules; these precipitate n values varied in turn from 40 to 26. The final precipitate powders consisted of ‘spherules’ of highly microcrystalline or amorphous polymer glass; the spherule diameters were about 0.2 μm at the critical concentrations and decreased to below 0.05 μm with increasing solution concentrations.  相似文献   

7.
The precipitation of different calcium phosphates in gelatine gels was studied by diffusion of disodium hydrogen phosphate solutions into ten percent gels containing calcium cation at liquid gel pHs from 6 to 11. At pHs 6.0 to 7.5, calcium hydrogen phosphate dihydrate (CaHPO4 · 2 H2O) was deposited as a continuous precipitate and then as rings of precipitate (the Liesegang phenomenon): their spacing coefficients varied with the reciprocal initial anion concentrations according to the Packter-Matalon relation. At liquid gel pHs 8.0, 8.5, tretacalcium phosphate (Ca4H(PO4)3) was deposited as a continuous precipitate. At liquid gel pHs from 8.5 to 11, hydroxyapatite (Ca10(PO4)6(OH)2, Ca/P ratios = 1.50 to 1.67) was deposited as a continuous precipitate. The mechanisms of precipitation of the different calcium phosphates (in gelatine gels) is briefly discussed.  相似文献   

8.
Zinc aluminium hydroxide hydrates were coprecipitated from different mixed cation solutions at Zn/Al2 ratios from 1/2 to 4/1. The coprecipitations were monitored by potentiometric titrations and the final coprecipitate compositions were examined by chemical analysis and atomic absorption spectrophotometry, X-ray diffraction and preliminary thermal analysis. The product from Zn/Al2 = 1/2 solution was amorphous: at Zn/Al2 = 1/1.5, the main phase (after drying at 95 °C) was a zinc hydroxoaluminate Zn[Al(OH)4]2 together with some gibbsite: at Zn/Al2 = 1, the main phase was probably a solid solution (of Zn[Al(OH)4]2 with Zn2[Al2(OH)10]) together with Zn2[Al2(OH)10]: at Zn/Al2 = 2, the main phase was a mixture of Zn2[Al2(OH)10] with (ZnOH)4 [Al2(OH)10] and some gibbsite: at Zn/Al2 = 4, the main phase was (ZnOH)4 [Al2(OH)10] with some zinc hydroxide.  相似文献   

9.
The crystallization conditions for the NaH2PO4, NaH2PO4 · H2O, and NaH2PO4 · 2H2O solid phases have been established from the analysis of the phase diagram of solubility of the ternary Na2O-P2O5-H2O system in the temperature range from 0 to 100°C. Based on these data, the methods for growing sodium dihydrogenphosphate single crystals of the above compositions are developed. The initial components for preparing mother solutions were H3PO4 and NaOH solutions taken in certain weight ratios. For the first time, NaDP, NaDP · H2O, and NaDP · 2H2O single crystals were grown on a seed by the method of temperature decrease. The habits of the NaDP and NaDP · H2O single crystals are determined. __________ Translated from Kristallografiya, Vol. 47, No. 5, 2002, pp. 937–944. Original Russian Text Copyright ? 2002 by Soboleva, Voloshin.  相似文献   

10.
A new hexaborate, Ba0.975[B6O9(OH)(O0.975Br0.025) · B2O(OH)3], was synthesized under hydrothermal conditions. This compound is structurally similar to tunnelite and the synthetic borates Pb[B6O10(OH) · B2O(OH)3], Pr[B6O10(OH) · B2O(OH)4], and Nd[B6O10 · B3O3(OH)4] · H2O studied earlier. In the new hexaborate and the refined pentaborate Ba2[B5O8(OH)2]OH, in which the polyanions adopt an orientation in layers unusual for pentaborates, thermal vibrations of the terminal groups were revealed. This fact reflects the real crystal structure. The nonlinear optical properties of the crystals of the polar pentaborate Na4Ba4[B20O34(OH)4] were determined. The crystal structure of the related pentaborate Ba5[B20O33(OH)4]H2O was considered. The factors most likely responsible for the difference in the second-harmonic generation signal for this pair were revealed.  相似文献   

11.
A new polar representative of the hilgardite structural family, Na0.5Pb2[B5O9](OH)1.5 · 0.5H2O (space group Pnn2), is synthesized under hydrothermal conditions. The crystal structure of the compound synthesized is similar to the structure of the previously studied polar compound Na0.5Pb2[B5O9]Cl(OH)0.5 and is intermediate between the latter compound and the centrosymmetric hydrate Pb2[B5O9](OH) · 0.5H2O. The additional peak revealed in the electron density in the vicinity of the Pb(1) atom is attributed to the stereochemically active lone electron pair of this atom. The lone electron pair is oriented toward the two most distant oxygen atoms involved in the Pb(1) coordination environment, namely, O(7) and O(2), which are located in a boron-oxygen framework layer in the ac plane, not toward the (00z) channel occupied by water molecules. The nonequivalence in the stereochemical activity of two lead atoms [Pb(1) > Pb(2)] is similar to that observed in the nonlinear optical borate Pb2[B4O5(OH)4](OH)2 · H2O related to BiB3O6.  相似文献   

12.
Magnesium aluminium hydroxides were coprecipitated from different mixed metal cation solutions — at total CM = 0.1 M and Mg/Al2 ratios from 1 to 6 — with sodium hydroxide solution at ambient temperature, with different pre-ageing conditions for the aluminium hydroxide pre-precipitate. The coprecipitations were monitored by potentiometric (pH) titration and the final precipitate compositions were examined by chemical analysis, infrared spectrophotometry and thermal analysis. Magnesium hydroxide was coprecipitated onto completely recrystallised aluminium hydroxide as a simple mixture. Generally, with no to three days pre-ageing, microcrystalline aluminium hydroxide was first precipitated at pH about 4; this then partially redissolved on further addition of sodium hydroxide (to form hydroxoaluminate anion) and magnesium aluminium hydroxide coprecipitates were formed continuously at pHs from 8.0–8.7 to 12.0–12.5. Their compositions were similar to the magnesium hydroxoaluminate hydrates formed by direct precipitation from high pH sodium hydroxoaluminate solutions.   相似文献   

13.
D‐optimal experimental design with three levels of SiO2/Al2O3, template/SiO2, H2O/SiO2, SiO2/Na2O and TPABr/TPAOH ratio parameters was used to optimize the experimental parameters by the analysis of variance (ANOVA). The effects of above mentioned ratios in the initial synthetic mixture on the crystallinity of the ZSM‐5 zeolite were studied. The synthesized samples were characterized by XRD, FE‐SEM, and TEM analysis. Fischer test results showed that SiO2/Al2O3 and H2O/SiO2 molar ratios are the most and least effective parameters, respectively, in the range studied. The most important two‐way interaction variable was that of template/SiO2 and Na2O/SiO2 molar ratios. The optimum composition of the gel compound to achieve relative maximum crystallinity is SiO2/Al2O3 = 99.96, template/SiO2 = 0.16, H2O/SiO2 = 34.68, Na2O/SiO2 = 0.02 and TPABr/TPAOH = 1.44.  相似文献   

14.
《Journal of Non》2005,351(43-45):3483-3489
Glasses in the system BaO/Al2O3/B2O3 with and without the addition of platinum were melted. In one sample series, the BaO-concentration was varied while the ratio [Al2O3]/[B2O3] was kept constant. In another sample series, the [BaO]/[Al2O3]-ratio (= 0.9) was kept constant and the B2O3 concentration was varied. The samples were thermally treated at 720 °C for 24 h and subsequently at 780 °C for 4 h. In most thermally treated samples, the crystalline phase BaO · Al2O3 · B2O3 occurred. At some compositions, the platinum-doped samples showed larger concentrations of the crystalline phases. The most remarkable property of the obtained glass–ceramics is their zero or negative thermal expansion coefficient. Here, notable differences were observed: samples with fine grained microstructures showed thermal expansion coefficients approximately zero up to temperatures of around 80 °C. By contrast, samples with coarser microstructures and large spheroidal crystals exhibit negative expansion coefficients up to temperatures of around 280–375 °C. The thermal expansions of these samples were close to those of the mean thermal expansion of the unit cell of the BaO · Al2O3 · B2O3 phase. The thermal expansion of the fine grained samples was approximately equal to that of the crystallographic a-axis of the BaO · Al2O3 · B2O3 phase.  相似文献   

15.
Calcium phosphates are precipitated at 25 °C from solutions of medium (Ca = P = 50 mM) and low (Ca = P = 10 mM) concentrations in the presence of magnesium. Experiments are also performed with solutions in which Ca + Mg = P = 50 mM and Ca + Mg = P = 10 mM. An amorphous calcium phosphate, Ca3 (PO4)2 · nH2O, and brushite, CaHPO4 · 2 H2O, are the phases first nucleated. The phases occurring one year later are brushite in the more concentrated solutions, hydroxyapatite (Ca5OH(PO4)3) and whitlockite (Ca9MgH(PO4)7) in the others. Octacalciumphosphate, Ca8H2 (PO4)6 · 5H2O, occurs as transitory phase. The effects of concentration, pH, supersaturation and magnesium on the precipitation and evolution of calcium phosphates, and the conditions for phase stability are discussed.  相似文献   

16.
We examined the solid-state water-soluble amorphous precursors that are formed by partial thermal decomposition of Al(NO3)3·9H2O (aluminum nitrate nonahydrate: ANN) using Raman and FTIR and solid-state magic-angle spinning NMR spectroscopy. We also studied the species formed in the aqueous alumosols formed by dissolution of the pre-ceramic precursors using 27Al NMR spectroscopy. Species identified in the alumosols included the Al3+(H2O)6 monomer, the [AlO4Al12(OH)24(H2O)12]7+(Al13) Keggin ion, and the Al30 polycation, [Al30O8(OH)56(H2O)24]18+, as well as various other oligomers or nanoparticles containing IV-, V- and VI-coordinated Al3+ ions.  相似文献   

17.
Crystallization was examined for glasses having chemical composition of 2(Ca,Sr,Ba)O-TiO2-2SiO2 in which the CaO/SrO/BaO molar ratio varied. Powdered glass samples were pelleted into disks and sintered at 950 °C for 2 h. The major phase precipitated in the sintered samples was (Ca,Sr,Ba)2TiSi2O8 and minor phase of perovskite such as CaTiO3 or SrTiO3 increased with CaO content in the samples containing more than 40 mol% of CaO in total CaO+SrO+BaO. Three regions having different slopes were found in linear relationships between SrO mol% and exothermal peak temperature on DSC curves or d[0 0 2] values determined by powder XRD method. These facts suggested that the major phase precipitated in each region was a solid solution containing a different amount of CaO, SrO, BaO and that these compositions varied depending on SrO content in the sample. The micro-crystalline structure, which could be useful in fabricating a dielectric dense body, was observed for samples containing 30-70 mol% of SrO.  相似文献   

18.
The structure of a new modification of the barium pentaborate β-Ba[B5O8(OH)] · H2O synthesized under hydrothermal conditions is investigated. This structure differs from the previously studied structure of the α-Ba[B5O8(OH)] · H2O compound by a shorter interlayer spacing and a higher degree of filling of the intersheet space with water molecules and barium atoms (the space group P is retained). The structure of the Ba2[B5O9] Cl · 0.5H2O pentaborate from the family of orthorhombic hilgardites (space group Pnn2) is refined, and the property of this crystal to generate the second optical harmonic is revealed. It is found that the previously studied pentaborate Ba5[B20O33(OH)4]H2O exhibits a nonlinear optical activity. The relationship between the structure and properties of hydrous and anhydrous pentaborates is discussed. Original Russian Text ? E.L. Belokoneva, S.Yu. Stefanovich, M.A. Erilov, O.V. Dimitrova, N.N. Mochenova, 2008, published in Kristallografiya, 2008, Vol. 53, No. 2, pp. 255–263.  相似文献   

19.
The precipitation of barium, strontium, calcium and magnexium polyacryate hydrates was studied from equivalent aqueous solutions of initial concentrations 0.03 M to 0.30 M at ambient temperature: sodium polyacrylate (m. wt = 30,000 to 300,000) was added to metal chloride solution. The final yields of precipitate increased with decreasing solubility and/or peptisation (Ba > Sr > Ca > Mg) and increasing molecular weight of the polyacrylate; the precipitates had the compositions [BaA(COO)2 · 1–2H2O]n, [SrA(COO)2 · 1–2 H2O]n, [CaA(COO)2 · 2 H2O]n and [MgA(COO)2 · 2 H2O]n. The final yields of the precipitates from sodium polyacrylate solutions were far lower and these had the compositions [NaM1-αCA(COO)2 · 2 H2O]n; A =  CH CH2 CH . The metal polyacrylate hydrate powders consisted of microcrystalline ‘spherules’; their average diameters were from 0.03–0.05 μm (for lower m. wt products) to 0.01 to 0.02 μ,m (for higher m. wt products).  相似文献   

20.
Magnesium aluminium hydroxocarbonate hydrates were coprecipitated from mixed metal nitrate solutions, at total CM = 0.2 M and Mg/Al2 = 1 ratio, with four sodium hydrogen carbonate-sodium carbonate solutions (of pH 8.1 to 11.5) at ambient temperature. The course of precipitation was monitored by potentiometric (pH) titration, and the compositions of the primary and final precipitates were determined by chemical analysis, infrared spectrophotometry and X-ray diffraction. Precipitation generally occurred through three stages, primary precipitation (of low CO3 aluminium hydroxocarbonates) at low pH with evolution of carbon dioxide, their dissolution by complexing to form hydroxocarbonatoaluminate anions and then secondary precipitation of the final coprecipitate at higher pHs. The final product from coprecipitation by sodium hydrogen carbonate solution (pH 8.1) was mainly the magnesium hydroxocarbonatoaluminate ‘MAHC I’; the final products from coprecipitation by sodium hydrogen carbonate-sodium carbonate solutions (pH 9.4 and 10.3) were ‘MAHC I’/‘MAHC II’ mixture and ‘MAHC II’/‘MAHC I’ mixture whereas the final product from coprecipitation by sodium carbonate solution (pH 11.5) was a complex mixture if ‘MAHC II’ with ‘MAHC I’ and ‘MAHC III’;
  • ‘MAHC I’ was probably Mg2[Al4(OH)10(CO3)3] · hH2O,
  • ‘MAHC II’ was probably Mg[Al2(OH)4(CO3)2] · h H2O whereas
  • ‘MAHC III’ was probably Mg[Al2(OH)6CO3] · h H2O.
  相似文献   

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