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1.
利用溶胶凝胶法制备出一种三角形Au@TiO2核壳材料。经过水热晶化,该材料膨胀至300 nm,壳层TiO2晶化为介孔锐钛矿相,但核心三角形Au颗粒的形貌保持不变。采用粉末X射线衍射(PXRD)、ζ电位、高分辨透射电子显微镜(HRTEM)、热重分析(TGA)、光致发光(PL)光谱、光电流(i-t)以及光催化降解技术,对样品的结构和性能进行了系统、详细的检测与分析。经过晶化处理的Au@TiO2在可见光波段的光降解亚甲蓝性能比未晶化时有了显著的提升,1 mg·mL-1 Au@c-TiO2可以在可见光照射1 h后实现对60 mg·L-1亚甲蓝全降解。电子顺磁共振(EPR)测试表明·O2-和·OH两种自由基对光降解起到了很大作用。通过综合分析实验结果和时域有限差分(FDTD)分析,探究了催化反应的机理。  相似文献   

2.
以结晶氯化铝(AlCl3·6H2O)作为铝源,十二烷基苯磺酸钠(SDBS)为模板剂,采用水热法在硅藻土盘上制备了束状纳米结构γ-AlOOH/Al2O3复合吸附剂。采用XRD、SEM、TEM、TG/DSC、N2吸脱附等对样品进行了表征。研究了样品对133Cs+及Pb2+的吸附能力。研究表明,样品γ-AlOOH/硅藻土、γ-Al2O3/硅藻土对Cs+及Pb2+均具有良好的吸附性能,两者对Cs+的去除率分别为98.9%和99.6%;对Pb2+的最大吸附量分别为357.1、416.7mg·g-1。两种样品对Pb2+的吸附均符合Langmuir吸附模型。  相似文献   

3.
以松香基季铵盐(脱氢枞基三甲基溴化铵,标记为DTAB)为模板剂、正硅酸乙酯为硅源、氨水为碱性介质成功合成出具有纳米片状形貌的六方有序超微孔二氧化硅材料。采用X射线衍射、N2吸附-脱附、透射电镜、扫描电镜等手段对样品进行表征,结果表明,体系中模板剂添加量、硅源添加量、碱性介质添加量、晶化温度、搅拌时间对前驱体的有序度有着较大的影响。当物质的量之比为nSio2:nDTAB:nNH3·H2O:nH2O=1.0:0.1:11.3:924.0,晶化温度为373K,搅拌时间为24h,所得样品有序度最高。经煅烧后样品具有较大的比表面积(1024 m2·g-1)和孔容(0.56 cm3·g-1),以及狭窄的孔径分布(集中于1.80 nm)。  相似文献   

4.
对NaY分子筛(nSi/nAl=2.65)进行了草酸脱铝处理并作为载体采用液相离子交换法制备CuY催化剂,应用于常压甲醇氧化羰基化合成碳酸二甲酯(DMC)反应。NaY分子筛及其CuY催化剂通过N2低温吸附-脱附、透射电子显微镜、X射线衍射、29Si固体核磁共振、NH3吸附程序升温脱附、吡啶吸附红外光谱、H2程序升温还原、原子吸收等方法进行表征。研究结果表明,酸处理NaY分子筛后,骨架铝被脱除,导致骨架nSi/nAl比增加、相对结晶度降低并产生介孔,有利于产物分子的扩散,从而影响催化活性。采用4 h、2 mol·L-1草酸处理NaY分子筛作为载体制备的CuY催化剂显示出较高的催化性能,DMC时空收率和甲醇转化率分别从103.6 mg·g-1·h-1和6.3%增加到184.9 mg·g-1·h-1和10.2%。产生的介孔能够促进催化剂中铜活性位的可接近性及反应物分子和产物分子的扩散。  相似文献   

5.
对NaY分子筛(nSi/nAl=2.65)进行了草酸脱铝处理并作为载体采用液相离子交换法制备CuY催化剂, 应用于常压甲醇氧化羰基化合成碳酸二甲酯(DMC)反应。NaY分子筛及其CuY催化剂通过N2低温吸附-脱附、透射电子显微镜、X射线衍射、29Si固体核磁共振、NH3吸附程序升温脱附、吡啶吸附红外光谱、H2程序升温还原、原子吸收等方法进行表征。研究结果表明, 酸处理NaY分子筛后, 骨架铝被脱除, 导致骨架nSi/nAl比增加、相对结晶度降低并产生介孔, 有利于产物分子的扩散, 从而影响催化活性。采用4 h、2 mol·L-1草酸处理NaY分子筛作为载体制备的CuY催化剂显示出较高的催化性能, DMC时空收率和甲醇转化率分别从103.6 mg·g-1·h-1和6.3%增加到184.9 mg·g-1·h-1和10.2%。产生的介孔能够促进催化剂中铜活性位的可接近性及反应物分子和产物分子的扩散。  相似文献   

6.
The two title coordination compounds, (NH4)3[TbIII(ttha)]·5H2O (ttha = triethylenetetramine-N,N,N′,N″,N‴,N‴-hexaacetic acid) and (NH4)4[Tb 2 III (ttha)]·9H2O (dtpa = diethylenetriamine-N,N,N′,N″,N″-pentaacetic acid), have been prepared and characterized by FT-IR, elemental analyses, TG-DTA and single crystal X-ray diffraction techniques. The (NH4)3[TbIII(ttha)]·5H2O compound is monoclinic, P21/c; a = 10.398(1) Å, b = 12.791(1) Å, c = 23.199(2) Å; β = 90.914(2)°; V = 3084.9(5) Å3; Z = 4; D calc = 1.704 g/cm3; μ(MoK α ) = 2.376 mm; R = 0.023 and wR 2 = 0.049 for 5429 observed reflections with I ≥ 2σ(I). The [TbIII(ttha)]3− complex anion in the crystal has a nine-coordinate mononuclear molecular structure with pseudo-monocapped square-antiprismatic configuration. The (NH4)4[Tb 2 III (dtpa)2]·9H2O compound is triclinic, P-1; a = 9.739(1) Å, b = 10.010(1) Å, c = 12.968(2) Å; α= 85.890(2)°, β = 77.338(2)°, γ = 77.587(2)°; V = 1204.2(2) Å3; Z = 1; D calc = 1.832 g/cm3; μ(MoK α ) = 3.015 mm; R = 0.024 and wR 2 = 0.060 for 4750 observed reflections with I ≥ 2σ(I). The [Tb 2 III (dtpa)2]4− complex anion has a binuclear structure in the crystal; the two TbIII centers are equivalent and have a nine-coordinate environment with the same pseudo-tricapped trigonal-prismatic configuration. The thermal analysis revealed that the coordination cores of the (NH4)3[TbIII(ttha)]·5H2O and (NH4)4[Tb 2 III (dtpa)2]·9H2O compounds are stable up to 221°C and 252°C, respectively. Original Russian Text Copyright ? 2008 by J. Wang, X. Zh. Liu, X. F. Wang, G. R. Gao, Zh. Q. Xing, X. D. Zhang, and R. Xu The text was submitted by the authors in English. Zhurnal Strukturnoi Khimii, Vol. 49, No. 1, pp. 81–89, January–February, 2008.  相似文献   

7.
The chemiluminescence (CL) system K2MnO4-luminol is shown to be useful for the determination of lead(II). The method is based on the catalytic effect of Pb(II) on the CL reaction. The linear range was 3 × 10−3–9 × 10−1 mg L−1 (r = 0.9971) and the relative standard deviation (R.S.D.) for 5 × 10−2 mg L−1 Pb(II) measurement was 0.7% (n = 11). The detection limit was 3 × 10−4 mg L−1 (3σ) Pb(II). Based on this, an in vivo, on-line, real-time analytical system for monitoring the metabolism of free lead(II) in rabbit blood was developed. A microdialysis probe, implanted in the vein of a rabbit, was perfused with perfusate at a flow rate of 5 μL min−1. The concentration of free lead(II) in the dialysate was determined on-line with a flow-injection CL system. This system included microdialysis sampling, on-line separation and chemiluminescence detection. The concentration-time curve of lead(II) was in accordance with the one-compartmental open model, T1/2 (elimination half-life), Tmax (peak time) and Cmax (peak concentration) were 37.77 min, 85.20 min and 0.137 mg L−1, respectively.  相似文献   

8.
以5-(三氟甲基)吡啶-2-羧酸(Htpc)与DyCl3·6H2O、TmCl3·3H2O构筑了2种异质同晶的单核配合物[M(tpc)3(H2O)3]·H2O,其中 M=Dy (1)、Tm (2)。配合物 12 均为单斜晶系,P21/c 空间群,中心金属离子为八配位且形成了轻微扭曲的十二面体构型。温度梯度下的荧光和紫外测试表明,2 种配合物均能与牛血清白蛋白(BSA)发生静态猝灭作用,猝灭常数(Ksv)为 105~106 L·mol-1。配合物与BSA结合过程的ΔH和ΔS均为正值,说明疏水作用在其中扮演重要的角色。25℃时,2种配合物与BSA结合常数约为104 L·mol-1,表明二者与BSA的具有中等强度的结合力。  相似文献   

9.
以5-(三氟甲基)吡啶-2-羧酸(Htpc)与DyCl3·6H2O、TmCl3·3H2O构筑了2种异质同晶的单核配合物[M(tpc)3(H2O)3]·H2O,其中M=Dy(1)、Tm(2)。配合物12均为单斜晶系,P21/c空间群,中心金属离子为八配位且形成了轻微扭曲的十二面体构型。温度梯度下的荧光和紫外测试表明,2种配合物均能与牛血清白蛋白(BSA)发生静态猝灭作用,猝灭常数(Ksv)为105~106 L·mol-1。配合物与BSA结合过程的ΔH和ΔS均为正值,说明疏水作用在其中扮演重要的角色。25℃时,2种配合物与BSA结合常数约为104 L·mol-1,表明二者与BSA的具有中等强度的结合力。  相似文献   

10.
A binuclear copper(II) complex with two symmetric end-on azido bridges: [Cu2(tacn)2(μ-N3)2](ClO4)2 · CH3OH (1), where tacn = 1,4,7-triazacyclononane, has been synthesized and structurally as well as magnetically characterized. Compound (1) has the discrete binuclear structure, bridged by two end-on N3 anions. The macrocyclic ligand tacn functions as a terminal ligand. The magnetic data of compound (1) were analyzed by means of Ĥ = −2JŜ1Ŝ2 − DŜz, leading to J = 2.49 cm−1, g = 2.08, D = ±0.97 cm−1, zJ′ = −0.47 cm−1. The ferromagnetic interaction is discussed on the basis of the structural features and is compared with the model structure of Ruiz.  相似文献   

11.
娄太平  张乐  郭军兴 《化学学报》2010,68(6):466-470
研究了在不同温度下的NaNO3和AgNO3水溶液中Li1.3Ti1.7Al0.3(PO4)3和Na1.3Ti1.7Al0.3(PO4)3离子交换行为.实验表明Li1.3Ti1.7Al0.3(PO4)3和Na1.3Ti1.7Al0.3(PO4)3均显示出了高选择性与Na+和Ag+进行离子交换的特征,且对Ag+的选择性高于Na+.升高温度可显著提高Ag/Li和Ag/Na的交换反应速度.  相似文献   

12.
Single crystals of K3RESi2O7 (RE=Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) were grown from a potassium fluoride flux. Two different structure types were found for this series. Silicates containing the larger rare earths, RE=Gd, Tb, Dy, Ho, Er, Tm, Yb crystallize in a structure K3RESi2O7 that contains the rare-earth cation in both a slightly distorted octahedral and an ideal trigonal prismatic coordination environment, while in K3LuSi2O7, containing the smallest of the rare earths, lutetium is found solely in an octahedral coordination environment. The structure of K3LuSi2O7 crystallizes in space group P63/mmc with a=5.71160(10) Å and c=13.8883(6) Å. The structures containing the remaining rare earths crystallize in the space group P63/mcm with the lattice parameters of a=9.9359(2) Å, c=14.4295(4) Å, (K3GdSi2O7); a=9.88730(10) Å, c=14.3856(3) Å, (K3TbSi2O7); a=9.8673(2) Å, c=14.3572(4) Å, (K3DySi2O7); a=9.8408(3) Å, c=14.3206(6) Å, (K3HoSi2O7); a=9.82120(10) Å, c=14.2986(2) Å, (K3ErSi2O7); a=9.80200(10) Å, c=14.2863(4) Å, (K3TmSi2O7); a=9.78190(10) Å, c=14.2401(3) Å, (K3YbSi2O7). The optical properties of the silicates were investigated and K3TbSi2O7 was found to fluoresce in the visible.  相似文献   

13.
The near infrared spectra of aqueous solutions of the ethylsulfates of La, Nd, Gd, Tb, Er, Yb, Lu, Y, and Na have been determined from about 0.2 mol-dm–3 to nearly saturation. The extinction coefficients of water have been calculated taking into account the absorption of ethylslfate anions determined in separate experiments. Their values appeared to be nearly the same as that of pure water. The relative contents of free OH groups in 0.5 and 0.7M solutions have been estimated from the absorbances at 1160 nm. They were lower in solutions of the heavy rare-earth ethylsulfates (Tb, Er, Yb, Lu) than in equimolar solutions of the lighter ones (La, Nd), confirming our previous view that secondary hydration of the heavy trivalent rare-earth cations is distinctly stronger than that of the lighter ones. A comparison of the spectra of these aqueous ethylsulfates with those of perchlorates shows that the structure-breaking ability of the C2H5SO 4 ion is much smaller than that of perchlorate anion.  相似文献   

14.
The room temperature structures of the five layer Aurivillius phases A2Bi4Ti5O18 (A=Ca, Sr, Ba and Pb) have been refined from powder neutron diffraction data using the Rietveld method. The structures consist of [Bi2O2]2+ layers interleaved with perovskite-like [A2Bi2Ti5O16]2− blocks. The structures were refined in the orthorhombic space group B2eb (SG. No. 41), Z=4, and the unit cell parameters of the oxides are a=5.4251(2), b=5.4034(1), c=48.486(1); a=5.4650(2), b=5.4625(3), c=48.852(1); a=5.4988(3), b=5.4980(4), c=50.352(1); a=5.4701(2), b=5.4577(2), c=49.643(1) for A=Ca, Sr, Ba and Pb, respectively. The structural features of the compounds were found similar to n=2-4 layers bismuth oxides. The strain caused by mismatch of cell parameter requirements for the [Bi2O2]2+ layers and perovskite-like [A2Bi2Ti5O16]2− blocks were relieved by tilting of the TiO6 octahedra. Variable temperature synchrotron X-ray studies for Ca and Pb compounds showed that the orthorhombic structure persisted up to 675 and 475 K, respectively. Raman spectra of the compounds are also presented.  相似文献   

15.
针对银精矿样品复杂,难消解的特点,研究了不同酸溶法和碱熔法对样品的消解情况,建立了硝酸,盐酸,氢氟酸,高氯酸消解银精矿的方法。根据元素灵敏度和抗干扰性,选定各元素的测定波长。通过酸溶样和碱熔样测定结果比对,验证了方法准确性。建立了四酸消解-电感耦合等离子体光谱法测定银精矿中铜、铅、锌、砷、镉、钙、镁、锰含量的方法,元素的线性相关系数均在0.9999以上。通过共存元素干扰实验,确定了银精矿中高含量元素(铜、铅、锌、铁、锑、铋等)对测定元素结果没有影响。方法检出限:Cu 0.0063 mg/L, Pb 0.0159 mg/L ,Zn 0.0090 mg/L,As 0.0192 mg/L, Cd 0.0093 mg/L ,Ca 0.0084 mg/L, Mg 0.0075 mg/L, Mn 0.0081 mg/L。测定下限:Cu 0.0105mg/L,Pb 0.0265 mg/L, Zn 0.0150 mg/L, As 0.0320 mg/L, Cd 0.0155 mg/L, Ca 0.0140 mg/L, Mg 0.0125 mg/L,Mn 0.0135 mg/L。3个样品的相对标准偏差在0.87%~3.56%之间,加标回收率在95.00%~103.56%之间。方法流程短,操作简单,快速,灵敏度和再现性高,结果准确可靠,可以满足银精矿中铜、铅、锌、砷、镉、钙、镁、锰含量的测定。  相似文献   

16.
The crystal structures of compounds with nominal compositions Bi6FeP2O15+x (I), Bi6NiP2O15+x (II) and Bi6ZnP2O15+x (III) were determined from single-crystal X-ray diffraction data. They are monoclinic, space group I2, Z=2. The lattice parameters for (I) are a=11.2644(7), b=5.4380(3), c=11.1440(5) Å, β=96.154(4)°; for (II) a=11.259(7), b=5.461(4), c=11.109(7) Å, β=96.65(1)°; for (III) a=19.7271(5), b=5.4376(2), c=16.9730(6) Å, β=131.932(1)°. Least squares refinements on F2 converged for (I) to R1=0.0554, wR2=0.1408; for (II) R1=0.0647, wR2=0.1697; for (III) R1=0.0385, wR2=0.1023. The crystals are complexly twinned by 2-fold rotation about , by inversion and by mirror reflection. The structures consist of edge-sharing articulations of OBi4 tetrahedra forming layers in the a-c plane that then continue by edge-sharing parallel to the b-axis. The three-dimensional networks are bridged by Fe and Ni octahedra in (I) and (II) and by Zn trigonal bipyramids in (III) as well as by oxygen atoms of the PO4 moieties. Bi also randomly occupies the octahedral sites. Oxygen vacancies exist in the structures of the three compounds due to required charge balances and they occur in the octahedral coordination polyhedron of the transition metal. In compound (III), no positional disorder in atomic sites is present. The Bi-O coordination polyhedra are trigonal prisms with one, two or three faces capped. Magnetic susceptibility data for compound (I) were obtained between 4.2 and 350 K. Between 4.2 and 250 K it is paramagnetic, μeff=6.1 μB; a magnetic transition occurs above 250 K.  相似文献   

17.
Tao Lin  Wei Li  Maochu Gong  Yao Yu  Bo Du  Yaoqiang Chen   《Acta Physico》2007,23(12):1851-1856
TiO2,ZrO2-TiO2,andZrO2-TiO2-CeO2 were prepared by co-precipitation method and characterized by X-ray diffraction (XRD), specific surface area measurements (BET), temperature programmed desorption (NH3-TPD), oxygen storage capacity (OSC), and temperature programmed reduction (H2-TPR). The results showed that ZrO2-TiO2-CeO2 exhibited large number of surface strong acid, possessed some oxygen storage capacity, and strong redox property. The three materials were used as supports and the monolith catalysts were prepared with 1% (w) V2O5 and 9% (w)WO3 for selective catalytic reduction (SCR) of NO with ammonia in the presence of excessive O2, and the results of catalytic activity showed that the catalyst used ZrO2-TiO2-CeO2 as support yielded nearly 100% NO conversion at 275 °C at a gas hourly space velocity (GHSV) of 10000 h−1, and it had the best catalytic activity and showed great potential for practical application.  相似文献   

18.
The phase relations in the system In2O3–TiO2–MgO at 1100 and 1350°C are determined by a classical quenching method. In this system, there are four pseudobinary compounds, In2TiO5, MgTi2O5 (pseudobrookite type), MgTiO3 (ilmenite type), and Mg2TiO4 (spinel type) at 1100°C. At 1350°C, in addition to these compounds there exist a spinel-type solid solution Mg2−xIn2xTi1−xO4 (0≤x≤1) and a compound In6Ti6MgO22 with lattice constants a=5.9236(7) Å, b=3.3862(4) Å, c=6.3609(7) Å, β=108.15(1)°, and q=0.369, which is isostructural with the monoclinic In3Ti2FeO10 in the system In2O3–TiO2–MgO. The relation between the lattice constants of the spinel phase and the composition nearly satisfies Vegard's law. In6Ti6MgO22 extends a solid solution range to In20Ti17Mg3O67 with lattice constants of a=5.9230(5) Å, b=3.3823(3) Å, c=6.3698(6) Å, β=108.10(5)°, and q=0.360. The distributions of constituent cations in the solid solutions are discussed in terms of their ionic radius and site preference effect.  相似文献   

19.
Microstructures of three Bi-W-Nb-O phases have been examined by using high-resolution transmission electron microscopy. Bi17W2Nb3O39 and Bi17WNb3O36 have incommensurate superstructures derived from the defect fluorite-type δ-Bi2O3 and can be regarded as intermediate phases between the type II solid solutions in the Bi-Nb-O and Bi-W-O systems. Bi8W2Nb2O23 has a Bi2WO6-like subunit cell with a stepped superstructure. Formation mechanisms of various superstructures are discussed.  相似文献   

20.
The crystal structures of Bi2.5Na0.5Ta2O9 and Bi2.5Nam-1.5NbmO3m+3 (m=3,4) have been investigated by the Rietveld analysis of their neutron powder diffraction patterns (λ=1.470 Å). These compounds belong to the Aurivillius phase family and are built up by (Bi2O2)2+ fluorite layers and (Am-1BmO3m+1)2- (m=2-4) pseudo-perovskite slabs. Bi2.5Na0.5Ta2O9 (m=2) and Bi2.5Na2.5Nb4O15 (m=4) crystallize in the orthorhombic space group A21am, Z=4, with lattice constants of a=5.4763(4), b=5.4478(4), c=24.9710 (15) and a=5.5095(5), b=5.4783(5), c=40.553(3) Å, respectively. Bi2.5Na1.5Nb3O12 (m=3) has been refined in the orthorhombic space group B2cb, Z=4, with the unit-cell parameters a=5.5024(7), b=5.4622(7), and c=32.735(4) Å. In comparison with its isostructural Nb analogue, the structure of Bi2.5Na0.5Ta2O9 is less distorted and bond valence sum calculations indicate that the Ta-O bonds are somewhat stronger than the Nb-O bonds. The cell parameters a and b increase with increasing m for the compounds Bi2.5Nam-1.5NbmO3m+3 (m=2-4), causing a greater strain in the structure. Electron microscopy studies verify that the intergrowth of mixed perovskite layers, caused by stacking faults, also increases with increasing m.  相似文献   

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