反相微乳液法合成SrTiO3纳米棒

SrTiO₃ nanorods were synthesized in cetanyl trimethyl ammonium bromide (CTAB) reverse microemulsion containing CTAB, n-hexanol, n-octane and water with Ba(OH)₂ as reactants. The effects of different conditions such as ω₀ [ω₀=n_H2O/ n_CTAB], aging time and the concentration of reactants on the formation of the nanorods were studied. Transmission electron microscope (TEM), electron diffraction (ED) and X-ray diffraction(XRD)were used to characterize the morphology and the structure of the synthesized nanorods. The results show that SrTiO₃ nanorods with a length of 260～2 000 nm and a diameter of 50～100 nm belonging to single crystal are single cubic system. The molar ratio of Sr to Ti of products is 1.0 as determinded by ICP.     

碳酸氢铵与氯化钇反应及结晶产物的组成和晶相类型

The relationships of crystal type, crystallization speed, purity, grain size and shape of rare earth carbonate with precipitation and crystallization conditions are very important for the production of rare earth carbonate with high efficiency, high quality and low cost. It is necessary for us for further understand the crystallization process mechanism and the factors effect on the crystallization. In the present paper, the crystallization characteristic, composition and crystal phase type of yttrium carbonates or ammonium yttrium carbonates precipitated from yttrium chloride solution using ammonium bicarbonate as precipitant were determined by chemical analysis, X-ray powder diffraction and the pH situ-determination. It was found that the crystal phase type was dominated by the feed molar ratio of ammonium bicarbonate to yttrium chloride, and the crystallization speed and the crystal composition were also influenced by temperature, feed manner and aging period etc. When precipitating and aging under lower temperature, crystallization is easy to take place in the high feed molar ratio zone, and when increasing tempera-ture, crystallization will take place both in lower and higher feed molar ratio zones. The results show that spherical yttrium carbonate with tengerite type crystal phase can be formed within the temperature 30～70℃ when feed molar ratio of ammonium bicarbonate to yttrium chloride is less than 4, and that a rhombus flake crystal, which possesses the composition of ammonium yttrium quasi-double carbonate and a new XRD pattern, is formed when the feed molar ratio is over 4. Their compositions can be represented as (NH₄)_aY(CO₃)_b(OH)_c·nH₂O, a< 1, 1< b< 2, c=3+a-2b. A fine crystal of ammonium yttrium double carbonate with the formula of (NH₄)Y(CO₃)₂·H₂O can also be obtained as using an enough amount of ammonium bicarbonate and aging enough time.     

水/油型微乳液中球形及棒状钛酸锶钡纳米粒子的控制合成

Barium strontium titanate nanoparticles with spherical and rod-like morphologies were synthesized in water/Triton X-100/n-hexanol/cyclohexane quaternary reverse microemulsion solution. The influences of the molar ratio of water to surfactant (ω₀) and the concentration of reactants on the morphology and size of barium strontium titanate nanoparticles were studied. The structure, compositions and morphology of the prepared products were characterized by XRD, SAED, ICP, EDS and TEM. The results show that the obtained Ba_0.7Sr_0.3TiO₃ spherical nanoparticles with diameters of 20～100 nm and the Ba_0.7Sr_0.3TiO₃ nanorods with diameters of 70～120 nm and lengths up to 600～800 nm are a single crystal, with a cubic phase. The molar ratio for barium, strontium and titanate in products is about 0.7:0.3:1.     

CaSO4纳米棒(线)的微乳法制备与表征

CaSO₄ Nanorods/wires were synthesized in quaternary W/O microemulsion solution containing triton X-100, cyclohexane and n-pentanol. Transmission electron microscopy (TEM) was utilized to characterize the shape and size of products as-prepared, as well as electron diffraction (ED) pattern was obtained for designated nanorods (wires). It is revealed that ω₀ (molar ratio of water to surfactant),reactants concentration and aging time play an important role in the formation of different morphologies and size of synthesized CaSO₄ nanocrystal.     

低维纳米材料CuI的制备

Low-dimensional CuI nanomaterials were synthesized in microemulsions containing cyclohexane， Triton X-100， n-pentanol and aqueous solution. The redox reaction took place in this system and the final products CuI were obtained. It′s found that the morphology of CuI could be influenced a great deal by the experimental param-eters such as w₀ (the molar ratio of water to surfactant)， reactant concentration and the aging time. Hexagonal or shuttle-like CuI flakes， nanoparticles and nanofibers could be prepared respectively under certain conditions.     

A Novel Cu-Mo／ZSM-5 Catalyst for NOx Catalytic Reduction with Ammonia

The Cu-Mo/ZSM-5 catalysts with different Cu/Mo ratios were prepared by wet impregnation method, and their catalytic performance for selective catalytic reduction of NOx was studied. The results showed that Cu-Mo/ZSM-5 is a very effective catalyst for NOx catalytic reduction with ammonia, especially when Cu/Mo molar ratio is about 1.5. It not only exhibited the extremely high catalytic activity, but also showed good stability for 02. The bulk phase structure of Cu-Mo/ZSM-5 catalysts was determined by XRD technique, and the results indicated that there is a maximum dispersion for Cu species when Cu/Mo molar ratio is 1.5, and an interaction between Cu and Mo along with HZSM-5 may be present in Cu-Mo/ZSM-5, which may possibly result in a special structure favorable for the catalytic reduction of NOx over Cu-Mo/ZSM-5 catalyst.     

噻吩甲酰基吡唑啉酮缩氨基酸稀土配合物的合成、表征及生物活性

A new amino-acid Schiff base, 1-phenyl-3-methyl-4-(2-thenoyl) pyrazolone-5-β-alanine (HL) and its ten rare earth complexes have been synthesized. On the basis of elemental analysis and molar conductance, the general formula of the complexes, [REL₂NO₃]·nH₂O (RE=La, Nd, Eu, Tb, Y, n=2; RE= Pr, Sm, n=1; RE= Dy, Er, Yb, n=3), is given. They were characterized by IR, UV-visible, ¹H NMR, ¹³C NMR and fluorescence. The results show that the rare earth ions exhibit coordination of eight in the complexes.The antibacterial experiments indicate that they have high antibacterial activities against S. Aureus, B. Subtillis, E. Coli, E. Carotovora and C. Flaccumfaciens.     

CeO2-ZrO2复合氧化物的制备及协同抛光性能

Sub-micrometer ultra fine CeO₂-ZrO₂ mixed oxides have been prepared by milling solid cerium carbonate and zirconium oxy-chloride with ammonia and followed by filtering, drying and calcining procedures. The effects of Ce/Zr molar ratio, milling time and calcining temperature on the phase composition, particle size and morphology, surface charge, as well as the polishing property were investigated. The results show that the mixed oxide calcined at 1 000 ℃ is composed of cubic ceria doped with zirconium and tetragonal zirconia doped with cerium, and the phase composition varies with calcination temperature and the Ce/Zr molar ratio. The monoclinic zirconia is observed when decreasing calcination temperature and shortening milling time, demonstrating that milling and calcining can force the phase transformation from monoclinic zirconia to cerium stabilized tetragonal zirconia and zirconium doped cubic ceria solid solutions. The removal rate for the optical glass polishing varies with Ce/Zr molar ratio. A synergetic polishing effect is found when Ce/Zr molar ratio below 4, and the optimal Ce/Zr molar ratio is 1∶1. At the same time, the cubic ceria content, density, particle size and surface charge all increase when calcination temperature increasing from 800 ℃ to 1 100 ℃. However, the particle morphology changes from disperse quasi-sphere to irregular aggregation and the maximal removal rate for optical glass polishing lies at 1 000 ℃.These facts show that the polishing property of the synthesized ceria-zirconia mixed oxide is affected by the particle physical characteristics comprehensively.     

氨基酸水杨醛席夫碱与铜(Ⅱ)配合物的合成及其抗菌活性和稳定性、结构间的关系

n-Salicylideneamino acids and their Cu(Ⅱ) complexes are synthesized. The structures of the compounds are characterized by elementary analysis, molar conductance, magnetic susceptibility, electronic and infrared spectra. The stability constants and the antibacterial activities have been determined. The relativity between antibacterial activities and structures of ligands and stability of complexes has been preliminarily studied.     

混合溶剂前体法制备纳米CuO粉体及其性能表征

Nano-CuO was prepared by heating nano-Cu₂(OH)₂CO₃ precursors in different calcination temperatures. The precursor was synthesized from water-alcohol mixed solution of Cu(Ac)₂ using mixed solution of NaOH and Na₂CO₃as precipitants. XRD, FT-IR, TEM, TG-DTA and surface area measurement techniques were used to investigate the properties of the CuO powder. The results show that the spherical, well dispersed nano-CuO powder with the average size of 15 nm and higher catalytic activity for H₂O₂ decomposition was obtained at 300 ℃. With the increasing of calcination temperature, crystal of CuO grows up, agglomeration of the powder becomes heavier and catalytic activity decreases. FT-IR patterns revealed that the vibration fine structure of Cu-O bond in nano-CuO powder disappears and main absorption is red-shifted with the average size of nano-CuO reducing.     

邻甲基苯磺酸铜催化"一锅法"合成3,4-二氢嘧啶-2(1H)-酮

二氢嘧啶酮(DHPMs)及其衍生物具有广泛的生物活性,如抗病毒、抗肿瘤、抗癌、抗高血压及消炎等作用[1].此外,DHPMs及其衍生物作为钙通道阻滞剂、α1a-对抗剂和神经肽Y的对抗剂,显示出良好的药理活性[2].更重要的是,最近几种含二氢嘧啶酮-5-羧酸盐的海洋生物碱被成功分离出来,并表现出重要的生物学性质[3],某些可以阻止HIVgp-120-CD4键的形成,是一种潜在的HIV抑制剂[4].因此,对DHPMs及其衍生物的研究成为生物活性有机杂环化合物的研究热点之一.     

铜铁二元类水滑石化合物的制备及催化性质研究

利用共沉淀法合成了CuFe二元类水滑石化合物。测定了不同Cu/Fe比混合盐溶液随沉淀剂NaOH与Na₂CO₃加入,混合盐体系pH值变化情况,详细探讨了不同因素对类水滑石化合物制备的影响,得到了合成铜铁二元类水滑石化合物的适宜条件,制备出晶相单一、结晶度高的类水滑石化合物,并利用XRD、FTIR、TG-DTA对合成物进行表征。将合成的催化剂引入苯甲醛与正丙醇反应生成安息香异丙醚反应中, 苯甲醛转化率为58%,安息香异丙醚选择性接近于100%。     

尿素燃烧法制备CuO-ZnO/HZSM-5及其催化CO_2加氢合成二甲醚的性能

以尿素为燃烧剂,先采用燃烧法制备CuO-ZnO催化剂,接着采用研磨法将其与HZSM-5分子筛均匀混合形成CuO-ZnO/HZSM-5双功能催化剂.采用固定床反应器,在反应温度260℃、压力3.0 MPa、空速1 500 h-1条件下,考察了不同Cu/Zn(摩尔比)催化剂在CO_2加氢合成二甲醚反应中的催化性能.通过XRD、N_2等温吸附脱附、H2-TPR、NH3-TPD对催化剂进行表征,研究了不同Cu/Zn对催化剂结构及表面酸性的影响.结果表明:当Cu∶Z n=6∶4时,催化剂对CO_2催化加氢直接合成二甲醚反应的催化活性和选择性最佳,CO_2的转化率、DME的选择性分别为11.95%和28.74%,且在催化剂上具有更多的低温还原Cu和较强的酸中心,从而提高了CO_2加氢活性和二甲醚的选择性.     

A new way to synthesize benzoin isopropyl ether on Cu-Fe-hydrotalcite

An efficient synthesis of benzoin isopropyl ether with benzaldehyde and propanol in the presence of heterogeneous recyclable Cu-Fe-hydrotalcite catalyst has been explored. Cu-Fe-hydrotalcite was firstly successfully synthesized over Jahn-Teller effect of Cu2+. The catalytic test result showed that Cu-Fe-hydrotalcite could be used as a good catalyst in the synthesis of benzoin isopropyl ether. The highest conversion of benzaldehyde was 59.7% and the selectivity of benzoin isopropyl ether was nearly 100%. By ...     

氮杂冠醚接枝壳聚糖的合成及其对金属离子的吸附性能

本文利用壳聚糖Ｃ２位上活泼的氨基先与苯醛反应制备成保护氨基的Ｓｃｈｉｆｆ碱壳聚糖,再将含环氧基的氮杂冠醚接枝到壳聚糖的Ｃ６位上,制得含Ｓｃｈｉｆｆ碱的氮杂冠醚壳聚糖,随后使其在一定条件下脱去苯甲醛,合成了一种含氮杂冠醚功能基的新型壳聚糖衍生物,研究了其重金属离子Ｐｂ＾２＋,Ｃｕ＾２＋、Ｃｒ＾３＋、Ｃｄ＾２＋的静态吸附性能。结果表明,该吸附剂对重金属离子具有较强的吸附能力,在Ｐｈ＾２＋、Ｃｕ＾２＋、     

K-MnO／y-A1203和Cu／SiO2催化剂应用于苯甲酸甲酯连续加氢合成无氯苯甲醇

以K—MnO／F—Al2O3和Cu／SiO2为催化剂，利用固定床串联反应器实现了苯甲酸甲酯连续加氢合成无氯苯甲醇反应过程．K-MnO/y-Al2O3和Cu／SiO2催化剂对于苯甲酸甲酯连续加氢合成苯甲醇具有良好的加氢活性，反应转化率可达89．2％，苯甲醇的选择性为84．1％．在苯甲酸甲酯加氢连续步骤中的氢醛比得到提高，有效地抑制了副产物甲苯的生成．XRD，SEM和TPR表征结果表明：采用吸附沉淀法制备的Cu／SiO2-C15．2催化剂，氧化铜在载体上具有良好的分散性能，并且易于还原，表现出最佳的苯甲醛加氢活性．     

Hyperbranched bisphosphinoamine ligands: synthesis,characterization and application in ethylene oligomerization

Two hyperbranched bisphosphinoamine (PNP) ligands and chromium complexes were synthesized in good yield with 1.0 generation (1.0 G) hyperbranched macromolecules, chlorodiphenylphosphine (Ph₂PCl) and CrCl₃(THF)₃ as raw materials. The hyperbranched PNP ligands and chromium complexes were characterized by FT-IR, ¹H NMR, ³¹P NMR, UV and ESI-MS. Comparing with the chromium complexes, the hyperbranched PNP ligands, in combination with Cr(III), and activation by methylaluminoxane (MAO) in situ generated species with better catalytic performance for ethylene oligomerization. The effect of solvent, chromium source, ligand/Cr molar ratio, reaction temperature, Al/Cr molar ratio and reaction pressure on the catalytic activity and product selectivity were studied. The results showed that with increase of ligand/Cr molar ratio, reaction temperature and Al/Cr molar ratio, the catalytic activity increased at first and then decreased. However, the catalytic activity continuously increased with increase of reaction pressure. Under the optimized conditions, the catalytic system of hyperbranched PNP/Cr(III)/MAO led to catalytic activity of 2.68 × 10⁵ g/(mol Cr·h) and 37.71% selectivity for C₆ and C₈.     

丙烯酸酯三元共聚物负载硫铂络合物的合成及催化性能

丁二醇二丙烯酸酯、丙烯酸甲酯、丙烯酸β-氯乙酯或丙烯酸ω-氯己酯进行三元共聚,合成了两类4种带ω-氯侧基的交联型聚丙烯酸酯.它们以乙硫醇硫醚化,再与氯亚铂酸钾反应,得到4种交联型聚丙烯酸酯负载的硫铂络合物.这些络合物对癸烯-1、十二烯-1、苯基烯丙醚、苯乙烯与三乙氧基硅烷的硅氢加成反应具有良好的催化活性.讨论了温度、催化剂用量对催化性能的影响及催化剂的重复使用情况.     

硫化亚铜/四针状氧化锌晶须纳米复合材料的制备及其光催化性能(英文)

在聚乙烯吡咯烷酮的辅助下,采用多元醇法制备了不同铜/锌摩尔比的硫化亚铜/四针状氧化锌晶须纳米复合材料,并利用X射线衍射、场发射扫描电镜、X射线光电子能谱和紫外-可见漫反射光谱对样品进行了表征.结果表明,在紫外光照射下,样品对甲基橙的光降解效率优于纯ZnO晶须.在铜/锌摩尔比低于4%时,样品的光催化性能随着铜/锌摩尔比增加而增加,但随着铜/锌摩尔比的继续增加,样品的光催化性能下降.此外,还采用周期实验来评价催化剂的稳定性.结果表明,该催化剂具有优异的光催化稳定性.     

氯化稀土乙二醇二甲醚配合物催化丁二烯聚合

以Nd2O3、(CH3)3SiCl和乙二醇二甲醚(DME)为原料,合成了NdCl3·2DME配合物,并将其用于催化丁二烯聚合。 考察了助催化剂种类与用量、陈化温度和聚合时间对聚合的影响。 结果表明,以烷基铝与MAO共同作为助催[JP2]化剂时具有高聚合活性,而单独以烷基铝或甲基铝氧烷(MAO)为助催化剂时聚合活性很低。 当n(Nd)∶n(AlR3)∶n(MAO)=1∶30∶45时,催化活性最高。 陈化温度对聚合活性、聚合物结构及相对分子质量均有较大的影响。 陈化温度过低或者过高,聚合活性、聚丁二烯cis-1,4含量和相对分子质量均降低;陈化温度为50 ℃时,具有最高聚合活性和最高cis-1,4含量。 NdCl3·2DME催化体系所得聚丁二烯的cis-1,4含量高达98.7%（IR）,而1,4-结构总含量高达99.6%（1H NMR）。