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1.
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   

2.
A series of aluminium hydroxocarbonate hydrates were prepared by precipitation from aluminium nitrate solution, with five sodium hydrogen carbonate-sodium carbonate solutions of different pH, at ambient temperature. The course of precipitation was monitored by pH measurement and the final precipitate compositions were determined by chemical analysis, infra-red spectrophotometry, X-ray diffraction and thermal analysis. Precipitation generally occurred through three stages, primary precipitation of materials with low carbonate content at low pH with evolution of carbon dioxide, their dissolution to form hydroxcarbonato anions and then secondary reprecipitation of the final products at higher pH. These materials were mixtures of polyhydroxoaluminium carbonate hydrates of general composition Aln(OH)3n-2CO3 · hH2O (where n = 2, 4, 6 and h = 6–8); their CO3 content increased with increasing pH and carbonate anion content of the precipitant solution.  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.
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   

5.
Series of magnesium iron(111) hydroxides were coprecipitated at ambient temperature from different mixed metal cation solutions, at CM tot = 0.1 M and Mg/Fe2 ratios from 4 to 1/4, with sodium hydroxide solution. The relevant single precipitations and the coprecipitations were monitored by potentiometric (pH) titration and the final coprecipitate compositions were examined by chemical analysis, infra-red spectrophotometry and thermal analysis. The coprecipitates onto aged α-FeOOH were simple mixtures of α-FeOOH and Mg(OH)2. The main coprecipitates were either «molecular inclusion mixtures» of microcrystalline α-FeOOH with excess Mg(OH)2 or similar mixtures of Mg(OH)2 with excess α-FeOOH and some ten-twenty percent (relative to the Mg content) of magnesium hydroxo-ferrate(III) hydrate Mg[Fe(OH)4]2 · h H2O. The coprecipitates aged in alkaline magnesium hydroxide suspension at 20 °C and 40 °C were mixtures of Mg(OH)2, α-FeOOH and forty to ninety percent (relative to the Mg content) of Mg[Fe(OH)4]2 · h H2O. The related α-FeOOH NaOH and α-FeOOH Mg(OH)2 equilibria and the different coprecipitation mechanisms are discussed.  相似文献   

6.
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   

7.
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   

8.
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   

9.
Magnesium chromium (III) hydroxides were coprecipitated at ambient temperature from different mixed metal cation solutions — at CMtot = 0.1 M and Mg/Cr2 ratios varying from 1 to 4 — with sodium hydroxide solution. The coprecipitations were monitored by potentiometric (pH) titration and the final precipitate compositions were examined by chemical analysis, i.r. spectrophotometry and thermal analysis. Generally, microcrystalline chromium(III) hydroxide was first precipitated at pH about 5; this material then redissolved on further addition of hydroxyl ion to form hydroxochromate(III) anion and magnesium chromium hydroxide coprecipitates were then formed continuously (at OH/Cr ratios from 4 to 10) at pHs from 9.5–10 to about 11. The coprecipitates from Mg/Cr2 = 1 systems was predominately magnesium hydroxochromate hydrate. The coprecipitates from Mg/Cr2 = 2 to 4 systems were mixture or solid solutions of magnesium hydroxochromate hydrate with increasing amounts of magnesium hydroxide. The ionic equilibria involved in different coprecipitations are discussed.  相似文献   

10.
Crystals of a new lead carbonate, NaPb2(CO3)2(OH), sp. gr. P31c, were prepared by hydrothermal synthesis. The crystal structure was established by the heavy-atom method without knowing the exact chemical formula of the compound. The polar structure of the carbonate and the distortion of the pseudosymmetry described by the supergroup P $\bar 3$ 1c are caused by the acentric arrangement of the oxygen atoms providing the satisfactory coordination of Pb and Na atoms. The bonds between a hydroxyl group and two crystallographically independent Pb atoms are directed along the c-axis and have different lengths. The study of the carbonate by the second harmonic generation method in a temperature range of 20–250°C revealed the nonlinear optical properties comparable with the similar properties of quartz. The comparison of the structure of the new carbonate with a number of carbonates demonstrated that the new compound is structurally similar to ewaldite BaCa(CO3)2, diorthosilicate NaBa3[Si2O7](OH), and Ba[AlSiO4]2 containing a double silicon—oxygen layer.  相似文献   

11.
Abstract The title complex [Co2(bte)3(NCS)4(H2O)2] n (bte = 1,2-bis(triazol-1-yl)ethane) has been prepared. Single-crystal X-ray analysis reveals that the complex crystallizes in space group P ī with a = 7.7962(2), b = 8.3407(4), c = 14.7735(5) ?, α = 86.835(2), β = 76.2031(9), γ = 80.583(3)°. The crystal consists of two discrete complexes, [Co(bte)(NCS)2(H2O)2] and [Co(bte)2(NCS)2]. The structure of [Co(bte)(NCS)2(H2O)2] consists of neutral chain containing Co(II) bridged by bte molecules. The six-co-ordination of Co2+ is achieved by means of two trans NCS ions and water molecules. The structure of [Co(bte)2(NCS)2] demonstrates a one-dimensional neutral chain through bte-bridge, in which the Co(II) atom is in a distorted octahedral environment formed by four nitrogen atoms of the triazoles and two nitrogen atoms from two trans thiocyanato liagnds. Index abstract Synthesis and Crystal Structure of a Polymeric Cobalt(II) Complex with 1,2-bis(1,2,4-triazol-1-yl)ethane This paper reports the synthesis and crystal structure of complex [Co2(bte)3(NCS)4(H2O)2]n (bte = 1,2-bis(triazol-1-yl)ethane), which consists two different neutral chains containing Co(II) bridged by bte molecules.   相似文献   

12.
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   

13.
Kernite Na2B4O6(OH)2·3H2O dehydration in air at high temperature and in vacuum at room temperature has been studied. It was found that kernite easily dehydrates forming a new phase‐I both on heating and in vacuum. The chemical formula Na2B4O6(OH)2·1.5H2O of the new phase‐I has been estimated on the basis of thermogravity analysis. It is triclinic with the unit cell parameters a = 7.047(8), b = 8.76(1), c = 13.08(2) Å, α = 93.40(9), β = 95.32(9), γ = 90.28(9)° changing slightly on pressure reduction. Due to the relatively low temperature (353 K) and reversibility of the kernite ⟷ phase‐I transition an anion of the new phase‐I likely consists of the same chains [B4O6(OH)2]2– like in kernite structure. The high anisotropy of kernite thermal expansion was explained by approaching of NaO chains due to the initial removing of water molecules from kernite crystal structure. The behaviour of the new phase‐I at low temperatures in vacuum was also investigated. A formation of an additional new phase II has been detected at the temperature of 93 K. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)  相似文献   

14.
The structures of three acid phosphites of trivalent metals [Al(HPO3H)3(H2O)] · H2O (I), K[Fe(HPO3H4)] (II), and Rb3[Ga(HPO3H)6] (III) have been determined. Structure I is layered, complex anions [Fe(HPO3H)4] form polymer chains in structure II, and structure III is insular.  相似文献   

15.
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   

16.
The electrical conductivity of pure and SrCO3-doped sodium carbonate has been measured in the temperature range 310–800 °C in air using a dc technique. Its concentration dependency is similar to that of the K2CO3–SrCO3 system described recently (GUTH et al. 1986). The maximum conductivity could be observed at ≈ 20 mol.% SrCO3. At temperatures > 440 °C, the conductivity of Na2CO3–SrCO3 mixtures containing up to 80 mol.% SrCO3 is larger than that of pure Na2CO3. X-ray investigations of slowly cooled samples show the mixtures to be heterogeneous. X-ray diffraction patterns of quenched mixtures containing 10 mol.% SrCO3 show reflexes of a high temperature compound. SrCO3, however, could not be detected. The lattice constants of this hexagonal compound Na2Sr4(CO3)5 which is isotyp with Na2Ca2Sr2(CO3)5 described by CHEN and CHAO are a0 = (1066.1 ± 0.4) pm and c0 = (653.2 ± 0.2) pm.  相似文献   

17.
Abstract The reaction of the third-generation, bis(pyrazolyl)methane ligand 1,1,5,5-tetra(1-pyrazolyl)pentane, [CH(pz)2]2(CH2)3 (pz = 1-pyrazolyl), with the dimer [Pt(p-tolyl)2(μ-SEt2)]2 yields the complex {μ-[CH(pz)2]2(CH2)3}[Pt(p-tolyl)2]2. The complex crystallizes in the space group P with unit cell dimensions a = 11.9461(5) ?, b = 12.1475(5) ?, c = 16.0665(7) ?; α = 102.424(1)°, β = 104.413(1)°, γ = 102.140(1)°. The platinum centers adopt a square planar coordination geometry where each bis(pyrazolyl)methyl group binds in a cis bidentate fashion. Index abstract The complex {μ-[CH(pz)2]2(CH2)3}[Pt(p-tolyl)2]2 (pz = 1-pyrazolyl) has been prepared by the reaction between the bis(pyrazolyl)methane ligand [CH(pz)2]2(CH2)3 and [Pt(p-tolyl)2(μ-SEt2)]2. Daniel L. Reger*, Russell P. Watson, and Mark D. Smith Department of Chemistry and Biochemistry, University of South Carolina, Columbia, SC 29208, USA,reger@mail.chem.sc.edu   相似文献   

18.
The crystal structure of a new mineral britvinite Pb7.1Mg4.5(Si4.8Al0.2O14)(BO3)(CO3)[(BO3)0.7(SiO4)0.3](OH, F)6.7 from the Lángban iron-manganese skarn deposit (V?rmland, Sweden) is determined at T = 173 K using X-ray diffraction (Stoe IPDS diffractometer, λMoKα, graphite monochromator, 2θmax = 58.43°, R = 0.052 for 6262 reflections). The main crystal data are as follows: a = 9.3409(8) ?, b = 9.3579(7) ?, c = 18.8333(14) ?, α = 80.365(6)°, β = 75.816(6)°, γ = 59.870(5)°, V = 1378.7(2) ?3, space group P1, Z = 2, and ρcalcd = 5.42 g/cm3. The idealized structural formula of the mineral is represented as [Pb7(OH)3F(BO3)2(CO3)][Mg4.5(OH)3(Si5O14)]. It is demonstrated that the mineral britvinite is a new representative of the group of mica-like layered silicates with structures in which three-layer (2: 1) “sandwiches” composed of tetrahedra and octahedra alternate with blocks of other compositions, such as oxide, oxide-carbonate, oxide-carbonate-sulfate, and other blocks. The tetrahedral networks (Si5O14)∞∞ consisting of twelve-membered rings are fragments of the britvinite structure. Similar networks also form crystal structures of the mineral zeophyllite and the synthetic phase Rb6Si10O23. In the crystal structures under consideration, the tetrahedral networks differ in the rotation of tetrahedra with respect to the layer plane. Original Russian Text ? O.V. Yakubovich, W. Massa, N.V. Chukanov, 2008, published in Kristallografiya, 2008, Vol. 53, No. 2, pp. 233–242.  相似文献   

19.
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   

20.
The high-sodium variety of cancrinite [Si6.3Al5.7O24][Na2(H2O)2][Na5.7(CO3)0.9(SO4)0.1(H2O)0.6] (Kovdor Massif, Kola Peninsula, Russia) and the calcium-containing variety of cancrisilite [Si6.6Al5.4O24][(Na1.2Ca0.4)(H2O)1.6][Na6(CO3)1.3(H2O)1.2] (Khibiny Massif, Kola Peninsula, Russia) are studied. The trigonal unit cell parameters of the crystal structures under investigation are as follows: a = 12.727(4) Å, c = 5.186(2) Å, and space group P3 for the former mineral and a = 12.607(4) Å, c = 5.111(1) Å, and space group P3 for the latter mineral. The reduced symmetry of the new varieties as compared to the symmetry of typical cancrinite and typical cancrisilite is associated with the specific features in the arrangement of the carbonate groups and water molecules in channels. This inference is confirmed by the IR spectroscopic data.  相似文献   

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