Synthesis and characterization of layered zinc hydroxychlorides

Layered material of zinc hydroxychlorides (Zn₅(OH)₈Cl₂·nH₂O: ZHC), which is one of the basic zinc salts (BZS), was synthesized from ZnO nano-particles aged with aqueous ZnCl₂ solutions at different temperatures ranging from 6 to 140 °C for 48 h. X-ray diffraction (XRD) results indicated that the diffraction peaks of ZnO completely disappeared by aging at 6 °C and the ZHC peaks were developed. By increasing the aging temperature, crystallinity of the layered structure was improved. At 6 °C, the ZHC particles were thin hexagonal plate particles with sizes ranging from 1 to 3 μm. The particle size of ZHC was independent of aging temperature. The atomic Cl/Zn ratios of all the ZHC materials were almost 0.2 less than 0.4 of the theoretical ratio, indicating that the synthetic ZHC is Cl-deficient. It seemed that half of Cl atoms in the layer were replaced with HCO₃⁻ and/or OH⁻. The specific surface areas of ZHC estimated from N₂ adsorption isotherms were ca. 10 m² g⁻¹ and were independent of the aging temperature. However, the H₂O monolayer adsorption capacity per unit surface area (n_w) for all the samples was higher than that of ZnO particles, revealing the high affinity of ZHC to H₂O molecules. The n_w values were increased by reducing the crystallinity of ZHC. This enhancement of H₂O adsorption selectivity was thought to be related with less-crystallized parts of the particles.     

Synthesis and characterization of mesoporous zinc layered hydroxide-isoprocarb nanocomposite

The ion exchange method was used to intercalate a poor water-soluble insecticide, isoprocarb into zinc layered hydroxide (ZLH). PXRD analysis indicated the successful intercalation with good crystallinity for the resulting nanocomposite, with a basal spacing of 33.1 Å. FTIR analyses showing the resemblance of an absorption peak of the nanocomposite with the host and the guest anion. The thermal analysis confirmed that the nanocomposite had better thermal stability compared to the pristine isoprocarb. The nanocomposite also characterized by elemental and surface morphology analysis. The surface analyses of the host and nanocomposite showed mesoporous-type material characteristics. On the whole, the intercalation process decreased the pore size of the nanocomposite compared to the pristine host, layered zinc layered hydroxide-sodium dodecyl sulphate (ZLH-SDS). The obtained material is believed has a great potential as an environmentally friendly insecticide.     

Synthesis,characterization and fungicidal activity of zinc diethyldithiocarbamate and phosphate

Monolayers of amphiphilic di-block copolymer, PEO₄₀-b-PMA(Az)₁₉ on water surface and solid surfaces, such as silicon wafer and quartz glass, were analyzed by surface pressure — molecular area (π-A) isotherm, UV-Vis spectroscopy, atomic force microscopy (AFM) and total X-ray reflectivity (TXR). The monolayer prepared at 22 mN m-1 consisted of H aggregated azobezene (Az) moieties, which orientated perpendicular to the solid surface. The monolayer structure, including H aggregated Az and orientation of Az, was stable after annealing at 98°C, at which temperature the hydrophilic PEO domain was the liquid phase and the hydrophobic PMA(Az) was in the smectic A phase.     

Synthesis and structural characterization of a new layered gallium phosphate using triethylenetetramine as structure-directing agent

A new layered gallium phosphate Ga₁₀(PO₄)₂(HPO₄)₁₂(OH)₅2.5N₄C₆H₂₀4.5H₂O was hydrothermally synthesized at 180 °C for 3 days by using triethylenetetramine (teta) as structure-directing agent. Its structure was determined by single-crystal X-ray diffraction with a triclinic cell in the space group P-1 (n^o 2) with a=8.4718(1) Å, b=18.5915(1) Å, c=24.1994(3) Å, α=110.538(1)°, β=93.656(1)°, γ=93.549(1)° and V=3547.45(6) Å³. It consists of [Ga₁₀(PO₄)₂(HPO₄)₁₂(OH)₅]⁵⁻ macroanionic sheets composed of infinite chains of GaO₄(OH)₂ octahedra connected via corner-sharing to PO₄ and GaO₄ tetrahedra. They contain four-, seven- and nine-membered rings. The inorganic layers are held together through hydrogen bond between the terminal PO bondings, the water molecules and the terminal ammonium groups of the intercalated teta molecules.     

Synthesis and characterization of a novel two-dimensional layered vanadate complex containing double helical chains

A novel two-dimensional layered vanadate complex 1 [Ni(phen)H₂O][V₂O₆] has been hydrothermally synthesized and characterized by elemental analyses, i.r., x.p.s., t.g. and single crystal X-ray diffraction. The single crystal X-ray diffraction analysis reveals that compound 1 consists of the chains covalently linked by [Ni(phen)H₂O]²⁺ subunits to form two-dimensional layered polyoxovanadate. It is interesting that the compound 1 consists of left-handed and right-handed helical chains, which are further interconnected to produce the double helical chains. The adjacent two-dimensional layers interact with each other via extensive hydrogen bonds and π–π stacking interactions to form a three-dimensional supramolecular framework.     

Synthesis, characterization and photocatalytic properties of novel zinc germanate nano-materials

We report the first instance of a hydrothermal synthesis of zinc germanate (Zn₂GeO₄) nano-materials having a variety of morphologies and photochemical properties in surfactant, template and catalyst-free conditions. A systematic variation of synthesis conditions and detailed characterization using X-ray diffraction, ultraviolet-visible diffuse reflectance spectroscopy, Raman spectroscopy, electron microscopy, X-ray photoelectron spectroscopy and small angle X-ray scattering led to a better understanding of the growth of these particles from solution. At 140 °C, the zinc germanate particle morphology changes with pH from flower-shaped at pH 6.0, to poly-disperse nano-rods at pH 10 when the Zn to Ge ratio in the synthesis solution is 2. When the Zn to Ge ratio is reduced to 1.25, mono-disperse nano-rods could be prepared at pH 7.5. Nanorod formation is also independent of the addition of cetyltrimethylammonium bromide (CTAB), in contrast to previous reports. Photocatalytic tests show that Zn₂GeO₄ nano-rods (by weight) and flower shaped (by surface area) are the most active for methylene blue dye degradation among the synthesized zinc germanate materials.     

Synthesis and characterization of a new layered lead borate

A new lead borate, Pb[B₈O₁₁(OH)₄], has been hydrothermally synthesized and structurally characterized by single crystal X-ray diffraction, FTIR, powder X-ray diffraction and thermogravimetric analysis. The compound crystallizes in the monoclinic system, space group P2₁/n (No. 14), , , , β=90.327(2)°, , and Z=4. The structure consists of layers of 9-membered borate rings enclosing Pb²⁺ cations. Adjacent borate layers are interconnected via ionic Pb-O bonds and hydrogen bonding to form a 3D supramolecular network.     

Synthesis, characterization and photophysical properties of novel tetrasubstituted phthalocyaninato zinc derivatives

Peripherally tetraimido-substituted phthalocyaninato zinc compounds 1-3 were synthesized through the reaction of tetraamino-substituted phthalocyaninato zinc with 4-Br-1,8-naphthalic anhydride, 4-hexahydropyridine-1,8-naphthalic anhydride and 4-morpholine-1,8-naphthalic anhydride, respectively. The compounds were characterized by MS, ¹H NMR, UV-vis, IR and elemental analysis, the results of which were consistent with the proposed structures. The effects of substitutes, acid/base and solvents on the UV-vis spectra of the new complexes were discussed in detail.     

Synthesis and characterization of chromia-pillared layered tetratitanate

The first chromia-pillared layered tetratitanate was prepared by the reaction of layered tetramethy-lammonium tetratitanate with chromium(Ⅲ) acetate [Cr(OAc)3] aqueous solution and subsequent calcination of the resultant solid product in air at 400℃. The obtained chromia-pillared layered tetratitanate has an interlayer distance of 1.06 nm and a high thermal stabih'ty up to 600℃. It was also found that calcination in N2 led to the chromia-pillared layered tetratitanate with relatively higher Brunauer-Emmett-Teller (BET) specific surface area (93.9 m2·g-1) and smaller average pore diameter (4.44 nm) than that in air (82.0 m2·g-1, 7.61 nm) . Both Bronsted and Lewis acid sites (mainly Lewis type) are present on the chromia-pillared layered tetratitanate (500℃, N2, 8 h) and strong enough to still remain a small proportion of pyridine upon outgassing at 250℃. Moreover, ammonia temperature-programmmed desorption (NH3-TPD) result showed that there were three NH3 desorption peaks at 160, 200and315℃, resp     

Synthesis and characterization of a UV absorbent-intercalated Zn-Al layered double hydroxide

Zn-Al-layered double hydroxides (LDHs) containing the organic anion of 2-hydroxy-4-methoxybenzophenone-5-sulfonic acid (HMBA), a highly efficient UV absorber, have been synthesized by reaction in air of HMBA with an LDH-carbonate precursor obtained by a process involving separate nucleation and aging steps. The structural properties, photo- and thermal stability of the resulting Zn-Al-HMBA-LDHs were characterized by PXRD, FT-IR and UV-visible spectroscopy and laser particle-size analysis. The results obtained indicated that Zn-Al-HMBA-LDHs synthesized by this method were relatively highly crystalline and had a narrow distribution of particle size. Intercalation of HMBA in the LDH interlayer galleries resulted in an enhanced photo- and thermal stability without affecting its UV absorption capacity; this shows that the hybrid HMBA-LDH phase has potential applications as a UV absorber.     

二维层状磷钒多金属氧酸盐的水热合成及晶体结构

利用中温水热技术合成了新型的磷矾铁酸盐(NH3CH2CH2NH3)4[FeV8O12(HPO4)6(PO4)2(H2O)2]·5H2O,通过元素分析、IR光谱、热重分析和X射线衍射确定了晶体结构.该晶体属单斜晶系,P21/n空间群,晶胞参数:a=1.4304(3)nm,b=1.0145(2)nm,c=1.8356(4)nm,β=90.15(3)°,V=2.6637(9)nm3,Z=2,最终偏差因子R1=0.0631,wR2=0.1874.     

Synthesis and crystal structure of a layered cobalt phosphate with a racemic 1,2-Diaminopropane template

A novel layered cobalt phosphate with racemic 1,2-diaminopropane as the templating agent, [CH₂(NH₃)-CH(NH₃)CH₃] [CoPO₄]₂, has been synthesized and structurally characterized by single-crystal X-ray diffraction methods. The compound crystallizes in the monoclinic system, space group P2₁/c with a = 10.457(2), b = 7.849(1), c = 6.692(l)?Å, β = 103.30(1)°, V = 534.5(2)?ų, Z = 2. The interaction of cobalt phosphate anionic layers and doubly protonated 1,2-diaminopropane cations is mainly ionic. The crystal structure is stabilized by a hydrogen bonding network between layers and templating cations.     

Synthesis and characterization of a novel nano-scale magnetic solid base catalyst involving a layered double hydroxide supported on a ferrite core

A nano-scale magnetic solid base catalyst MgAl-OH-LDH/MgFe₂O₄ (where LDH denotes layered double hydroxide) composed of MgAl-OH-LDH Brønsted base catalytic layers coated on MgFe₂O₄ spinel cores has been prepared. A magnetic precursor MgAl-CO₃-LDH/MgFe₂O₄ was prepared by a method involving separate nucleation and aging steps, and subsequently calcined to give a mixed metal oxide composite MgAl(O)/MgFe₂O₄ which was rehydrated to give MgAl-OH-LDH/MgFe₂O₄. The structure and magnetic properties of the nano-scale magnetic solid base MgAl-OH-LDH/MgFe₂O₄, together with those of the magnetic precursor MgAl-CO₃-LDH/MgFe₂O₄ and MgFe₂O₄ were characterized by XRD, XPS, low temperature N₂ adsorption and vibrating sample magnetometry (VSM). The MgAl-OH-LDH/MgFe₂O₄ composite possesses a mesoporous structure with pore size ranging from 2 to 20 nm with particle size mainly in the range 35-130 nm. The catalytic properties of MgAl-OH-LDH/MgFe₂O₄ were evaluated using the self-condensation of acetone at 273 K as a probe reaction. The results showed that the conversion of acetone to diacetone alcohol reached the thermodynamic equilibrium value of 23% at 273 K. The catalyst was easily recovered through application of an external magnetic field, and when the reclaimed catalyst was used in a second run for the same reaction, the reactivity remained unchanged.     

Synthesis, characterization and intercalation property of layered zirconium benzylamino-N,N-dimethylphosphonate phosphate materials

Layered zirconium benzylamino-N,N-dimethylphosphonate phosphate (ZBMPA) was prepared by the reaction of zirconyl chloride with benzylamino-N,N-dimethylphosphonic acid (H₂BMPA) and phosphoric acid in the presence of hydrofluoric acid. The intercalation of n-alkylamines (n-butylamine, n-heptylamine and n-decylamine) into ZBMPA was primarily investigated at room temperature. These materials were characterized by elemental analysis, ICP, XRD, SEM, FT-IR, Raman spectra, TG and DSC. The composition of ZBMPA is Zr(HPO₄)(C₆H₅CH₂N(CH₂PO₃)₂)_0.5 · 2.0H₂O. The interlayer distance of ZBMPA, n-butylamine, n-heptylamine and n-decylamine intercalation compounds is 2.03, 2.58, 2.52 and 3.17 nm, respectively. ZBMPA and the n-alkylamine intercalation compounds are different in the morphology and vibration spectra. Thermogravimetries of all materials obtained reveal three step mass losses at temperatures of up to 1000 °C. These results indicate that n-alkylamines are intercalated into the galleries of host ZBMPA.     

蔗渣木聚糖磷酸酯的合成与表征

以蔗渣木聚糖为主要原料,正磷酸盐(NaH2PO4与Na2 HPO4)为酯化剂,尿素为催化剂,在湿法工艺下合成了蔗渣木聚糖磷酸酯.考察了酯化温度、酯化时间、蔗渣木聚糖与酯化剂和催化剂配比、pH等因素对取代度的影响,采用正交试验设计对合成条件进行优化,运用统计分析方法探讨了各因素影响的主次顺序和显著性,得到较佳的合成条件为...     

Synthesis and characterization of zinc oxide nanoparticles

The research is aimed at synthesis and characterization of nanoscaled zinc oxide particles and their application on linen fibrous supports, for thermal properties. To impart thermal activity to the fibrous nanocomposites, nanoparticles as well as fibrous nanocomposites were produced in different hydrothermal conditions of temperature (90 °C). To characterize the nanoparticles composition, their shape, size, and crystallinity, investigations technique, such as Fourier transformed infrared spectroscopy, scanning electron microscopy, and X-ray powder diffractometry were used. Differential scanning calorimetry analysis profiles were also revealed. The thermal treatment of linen fabrics with nanosized ZnO does not modify significantly their thermal stability.     

Synthesis pretreatment and characterization of a magnetic layered double hydroxides fluorescent probe

Using magnetic layered double hydroxide （MLDH） as carrier of fluorescein （FLU）, a fluorescent composite of MLDH-FLU was prepared via intercalation reaction of ion change. The crystal properties of MLDH-FLU were investigated through XRD, IR, TEM and TG-DSC characterization. It is shown that the crystal type of MLDH-FLU composite matched well with R-hexagonal crystal system of MLDH, with crystal cell parameters of a, c and channel height h equal to 0.3199, 2.411 and 0.3267 nm respectively. The superabundant pigment adsorbed outside the composite should be cleared before interference with cells, but excessive wash would decrease stability and cause crystal phase transformation of MLDH.     

Synthesis and characterization of layered double hydroxides with a high aspect ratio

A new route for synthesis of Mg/Al layered double hydroxide (Mg₆Al₂(OH)₁₆(CO₃)·4H₂O) has been introduced, which can be considered as a modified calcination-rehydration method. Under the hydrothermal conditions, LDHs with a high aspect ratio were synthesized and characterized by inductively coupled plasma-atom emission spectrometer (ICP-AES), X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), thermal measurement (TG-DTG) and scanning electron microscopy (SEM). XRD patterns display the crystalline enhanced with the increase of hydrothermal temperature and aging time. TG-DTG curves show the more stable LDHs were synthesized at higher temperature. SEM images indicate the lateral size of the synthesized LDHs locates at ca. 1-6 μm and the thickness at ca. 35-60 nm. And the particle size depends strongly on the treatment temperature and aging time. A buffer solution consisted of HCO₃⁻ and CO₃²⁻ keeps the pH of reaction system in a certain range and offers a low supersaturated reaction circumstance. This is of high importance for the formation of LDHs with a high aspect ratio.     

Intercalation and photophysical characterization of 1-pyrenemethylamine in zirconium phosphate layered materials

The ion exchange of the luminescent probe 1-pyrenemethylamine (PYMA) into zirconium phosphate (ZrP) layered materials has been accomplished. The matrices used were the hexahydrated 10.3 A phase of ZrP (10.3 A ZrP, where 10.3 A represents the interlayer distance) and butylammonium-exchanged ZrP (BAZrP) with an expanded 18.6 A interlayer distance. The XRPD patterns for the 10.3 A ZrP after PYMA exchange (PYMA-exchanged ZrP), at high PYMA concentrations, show an increase in the interlayer distance from 10.3 A in unexchanged 10.3 A ZrP to 23.5 A in PYMA-exchanged ZrP, indicating PYMA intercalation. The luminescence spectrum for the PYMA-exchanged ZrP exhibits an excimer band at 458 nm that is absent in the luminescence spectrum of PYMA in aqueous solution at low concentrations. The intensity of the excimer emission increased at low PYMA concentrations. These results are in contrast to experiments using the BAZrP matrix. The XRPD patterns for PYMA-exchanged BAZrP do not show changes in the interlayer distance, which suggests that PYMA is not being intercalated and is only surface bound. The luminescence spectrum for PYMA-exchanged BAZrP exhibits a lower emission intensity in its excimer band, at different PYMA concentrations, compared with the PYMA-exchanged ZrP excimer band. For PYMA-exchanged ZrP, we propose a process in which exchange at low PYMA concentrations occurs at external surface sites with clustering promoting excimer formation followed by exchange at high PYMA concentrations occurring at interior sites reducing excimer formation.     

Synthesis of a novel mesoporous tin phosphate,SnPO4

Novel mesoporus tin phosphates have been synthesized using alkyltrimethylammonium bromide (alkyl = C8-C18) as surfactant; the structure of the materials is stable at 500 degrees C. UV-VIS spectra show tetrahedral coordination of tin.