氧化锌纳米棒的制备和生长机理研究

ZnO nanorods are prepared by different assistants (cetyltrimethylammonium bromide，trisodium citrate and ethylene diamine anhydrous) favored hydrothermal synthesis with Zn(OH)₂ colloid as the precursor. The samples are characterized by transmission electron microscopy (TEM) and X-ray diffraction (XRD). The results show that the as-synthesized ZnO nanorods are of uniform size with 25 nm in diameter and 200～300 nm in length. The effects of the different assistants to the morphology, size and mechanism of nano-ZnO are discussed.     

ZnO纳米线的电化学制备研究

High-quality ZnO nanowires have been synthesized at relatively low temperature via one-step electrochemical anodization technique. In this method, Zn sheet acted as the anode and Pb sheet served as the counter electrode, and the complex solution of HF-C₂H₅OH-H₂O was used as electrolyte. ZnO nanowires were characterized by Field Emission Scanning Electron Microscopy (FE-SEM), Transmission Electron Microscopy (TEM) and Selected Area Electron Diffraction (SAED) and X-ray Diffraction (XRD). The results show that the nanowires were wurtzite crystalline ZnO, and the ZnO nanowires with the diameters of 70 nm and 30～40 nm were obtained by adjusting preparation conditions, respectively.     

均一形貌的ZnO纳米棒的制备及其光催化性能研究

ZnO nanorods were synthesized from high purity Zn granule by a vapor phase deposition in the Ar + O₂ gas. The products were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). The ZnO nanorods were typically 1～2 μm in length and 20～30 nm in diameter with an aspect ratio as high as 20. The UV absorption properties were detected and the results show that the ZnO nanorods have an extremely strong absorption at 200～380 nm wavelength. The results were good when the ZnO nanorods were used as photocatalyst.     

单分散超细ZnO粉体的制备与表征

Monodispersed superfine ZnO powders with particle size of about 200～400nm were successfully prepared by the decompressed distillation process with n-butyl alcohol as the solvent. The starting materials were Zn(NO₃)2·6H₂O and NH₃·H₂O. TG-DSC， XRD， TEM and BET surface areas techniques were used to characterize the precursor and as-prepared superfine ZnO powders. In the preparation process of superfine ZnO powders， two techniques including the decompressed distillation with n-butyl alcohol and washing with absolute ethanol were used to avoid agglomeration. It is showed that the decompressed distillation process has a better effect in avoiding ag-glomeration than washing with absolute ethanol. The precursor obtained by the decompressed distillation technique has a lower calcination temperature than the one obtained by washing with absolute ethanol. Zincite phase of ZnO with some impurities was obtained when the precursor was calcined at 200℃ for 2h. After it was calcined at 300℃ for 2h， pure superfine ZnO powder was obtained.     

针状TiO2锐钛矿晶粒溶胶的制备、结构及形成机理研究

The PTA sol was prepared using titanyl sulfate(TiOSO₄), peroxide (H₂O₂) and ammonia (NH₃·H₂O) as raw materials. The semitransparent, light yellow AS(autoclaved sol) with ultra-fine needle-like anatase crystals was synthesized by autoclaving the PTA sol at 80～100 ℃ for different times. The anatase crystals were needle-like and 80 nm in length, 20～30 nm in diameter. The FTIR, XRD, SEM were used to analyse the chemical structure, properties of the AS and influencing factors during the sol preparation. The mechanism model of the AS formation was established based on the inorganic and crystal structural chemistry. The PTA molecules were decomposed to form Ti⁴⁺ under hydrothermal conditions and the Ti⁴⁺ were hydrated with water to get [Ti(OH)₄(OH₂)₂]⁰, a growing units of the anatase crystals. The appearance of the needle-like anatase crystals and the anatase precipitate are also explained in this paper.     

Sr3SiO5∶Eu2+荧光粉的微波合成及性能研究

Silicate orange yellow phosphor used in white-light LED was prepared by microwave method. The structure and optical properties of phosphor were studied. Sr₃SiO₅∶Eu²⁺ phosphor synthesized by microwave method is tetragonal structure of Sr₃SiO₅ with uniform particle distribution. Luminescence spectrum is a broad band spectrum peaking at 575 nm. The peak of excitation is at 532 nm and phosphor can be excited by blue LED. The warm white light was obtained combined phosphor and blue LED. The CIE chromaticity coordinates and correlated color temperature of white light is (x=0.394, y=0.341) and 3 239 K respectively.     

一种制备大量氧化锌纳米管的简单方法(英)

ZnO nanotubes were synthesized in large scale by thermal decomposition of the precursors obtained via chemical reaction between Zn(CH₃COO)₂·2H₂O and NaHCO₃ in the presence of surfactant sodium dodecyl sulfate (SDS). The inner diameters of the tubes were in the range of 80～100 nm, and outer diameters in the range of 160～260 nm with lengths up to a few micrometers. The products were characterized with XRD, TEM, and SEM.     

95 ℃水溶液体系中TiCl4溶胶水解法制备纯金红石纳米粉体(英)

Titanium dioxide (TiO2) nanoparticles of rutile phase were synthesized by hydrolysis of TiCl₄ at 95 ℃ in aqueous solution. The samples as prepared and calcined at 500 ℃ were characterized by XRD, TG-DTA and TEM. The sample as prepared was of imperfect rutile structure, and its morphology was rod-like with a diameter of 10～20 nm, a length of 20～80 nm and an aspect ratio of 2～4. The structure of the sample calcined at 500 ℃ was a perfect rutile one, and its morphology was rod-like with a diameter of 15～25 nm, a length of 25～105 nm and an aspect ratio of 2～4. These results indicate that calcination temperature has a positive effect on the structure and the size of rutile nanocrystals, and has no effect on the aspect ratio of rutile nanocrystal. A model for the formation mechnism of rutile nanocrystal in aqueous solution under hydrolysis conditions has been proposed.     

Synthesis and characterization of yellow water-borne polyurethane using a diol colorant as extender

<正>A novel and facile method toward a series of yellow water-borne polyurethane was developed by using an intrinsically colored diol in this paper.The yellow aqueous dispersion PCLD-HENA-PU was synthesized based on isophorone diisocyanate(IPDI), polycaprolactonediol(PCLD) and 2,2-dimethylol propionic acid(DMPA) using a yellow diol N,N-bis(2-hydroxyethyl)-4-nitroaniline (HENA) as a chain extender.Due to the complete reaction of OH group in colorant HENA with NCO group in diisocyanate,a series of stable yellow polyurethanes could be obtained conveniently and easily.The structure of PCLD-HENA-PUs was confirmed by means of Fourier transform infrared spectroscopy.The UV-visible absorption analysis showed a blue shift effect of about 7 nm when HENA was blocked into polyurethane chain.The absorption intensity of PCLD-HENA-PUs increased with increasing HENA content.It was found that the tensile strength enhanced from 8.6 to 19.6 MPa with HENA content increased from 0 to 18.0%,while the extensibility decreased from 449 to 300%.The thermal gravimetric analysis presented that the initial decompose temperature began from about 250℃,and had a little increase with increasing the HENA content.     

高分子辅助水热制备单晶碲纳米管

Te single-crystal nanotubes were synthesized using Na₂TeO₃ and (NH₂)₂CS as starting materials and pol-yacrymide (PAM) as morphology-director under hydrothermal conditions. The obtained products were characteri-zed by XRD, FESEM, SEM and TEM techniques. The results show that Te nanotubes grow along c axial with the inner diameters of 100～500 nm, wall thickness of 80～160 nm and lengths of 5～10 μm. A possible mechanism for the growth of Te nanotubes was discussed.     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Selective syntheses of 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones via temperature-dependent Rh(II)-carbenoid-mediated 2H-azirine-ring expansion

The Rh(II)-catalyzed reaction of 2-carbonyl-substituted 2H-azirines with ethyl 2-cyano-2-diazoacetate or 2-diazo-3,3,3-trifluoropropionate provides an easy access to 2H-1,3-oxazines and 1H-pyrrol-3(2H)-ones. These compounds can be selectively prepared from the same starting material using temperature as the only varied parameter. The 2-azabuta-1,3-diene intermediate, a common precursor for both heterocyclic products, isomerizes into 2H-1,3-oxazine under kinetic control, while 1H-pyrrol-3(2H)-one is the sole product of the reaction at elevated temperatures. According to DFT-calculations a one-atom oxazine ring contraction involving ring-opening to a 2-azabuta-1,3-diene intermediate, followed by a 1,5- and 1,2-prototropic shift leads to the consecutive formation of imidoylketene and azomethine ylide, which then further undergo cyclization to the pyrrole derivative.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

Copper catalyzed/mediated synthetic methodology for ebselen and related isoselenazolones

Scope of the copper catalyzed/mediated selenium-nitrogen coupling reaction has been studied for the synthesis of isoselenazolones. It is noticed that the 2-chloro, 2-bromo-, and 2-iodo-aryl amides substrates can be exploited in the selenium-nitrogen coupling reaction by employing 25-100 mol % of CuI/1,10-phenanthroline (L) and potassium carbonate as a base in DMF. Furthermore, electron rich 2-chloro-arylamides also underwent selenium-nitrogen coupling reaction to give biologically important selenium-nitrogen heterocycles. Also, copper-catalyzed selenium-nitrogen coupling reaction has been meticulously applied for the synthesis of diaryl diselenides having methoxy, amine, and amide functionality from respective aryl iodides in the presence of stoichiometric amount of succinimide as an external Se-N coupling partner.     

Knoevenagel condensation catalyzed by novel Nmm-based ionic liquids in water

A series of novel N-methyl morpholine (Nmm) based ionic liquids with 1,2-propanediol group were synthesized and used as catalysts for Knoevenagel condensation at room temperature in water. Under the effect of the catalyst, various aldehydes or aliphatic ketones could react with a wide range of activated methylene compounds well, including malononitrile, alkyl cyanoacetate, cyanoacetamide, β-diketone, barbituric acid, 2-arylacetonitrile and thiazolidinedione. Furthermore, most of the products could be separated just by filtrating and washing with water. Additionally, the catalyst is recyclable and applicable for the large-scale synthesis.     

Construction of polyheterocyclic spirotetrahydrothiophene derivatives via sulfa-Michael/aldol cascade reaction

A series of polyheterocyclic spirotetrahydrothiophene derivatives were obtained in moderate to excellent yields via a catalyst-free sulfa-Michael/aldol cascade reaction of chalcones 1 and commercially available 1,4-dithiane-2,5-diol 2 under mild conditions. We also present the first asymmetric sulfa-Michael/aldol cascade reaction of chalcones 1 and commercially available 1,4-dithiane-2,5-diol 2 with moderate to good enantioselectivities catalyzed by readily available chiral phase-transfer catalysts (PTCs).