可磁分离的"核-壳"结构Fe3O4@SiO2/Bi2WO6/Ag2O催化材料的制备及光催化性能研究

采用沉淀-沉积法制备了磁性Fe3O4@SiO2/Bi2 WO6/Ag2O催化材料,利用XRD、SEM和UV-Vis-DRS光谱对其组成、形貌和光吸收特性进行表征.以氙灯模拟可见光,以罗丹明B为模拟污染物对所得催化剂进行性能评价,考察了不同Ag2O复合量对Bi2WO6光催化剂反应活性的影响.结果表明,Fe3O4@SiO2/Bi2WO6/Ag2O的光催化活性明显优于纯Bi2 WO6,当Ag2 O的复合量为0.6;时,催化剂的活性最好.催化剂的活性增强增强机理分析表明,Ag2O的复合有效地降低了Bi2WO6的光生电子-空穴复合率,增加了Bi2WO6的可见光吸收范围.此外,该催化材料可进行磁分离,易于回收重复利用.     

BiOI/BiVO4异质结光催化剂的合成及其催化活性的研究

采用溶胶-凝胶法合成具有异质结结构BiOI/BiVO4,以罗丹明B为模型污染物,考察了BiOI/BiVO4的光催化活性,并采用XRD、SEM、FT-IR等进行了表征.结果表明,BiOI/BiVO4具有典型的异质结结构,具有抑制电子-空穴再复合、有效促进光生载流子分离的特点,BiOI的引入没有破坏BiVO4颗粒的晶体结构,仍为单斜相主体物相结构,而是增强了催化剂表面的活性位点,提高光电子的迁移速率.相比于单体钒酸铋,复合后的材料光谱响应范围更宽,同时,复合催化剂比单体钒酸铋的催化活性和稳定性更好,在BiOI的摩尔分数为20;时,复合光催化材料的催化活性最佳,实验条件下罗丹明B降解率为95.7;.     

CdS/沸石分子筛复合光催化剂的制备及光催化性能

以煤矸石为原料,经Na2CO3碱熔活化和水热合成获得了沸石分子筛;利用Cd2+对沸石分子筛进行离子交换并通过沉淀过程制得了CdS/沸石分子筛复合粉体.采用X射线粉末衍射(XRD)和扫描电子显微镜(SEM)对所得样品进行表征,并以模拟太阳光为光源,罗丹明B (RhB)为目标降解物,对其光催化活性进行了研究.结果显示:沸石分子筛上负载的CdS的晶相为立方相,制得的CdS/沸石分子筛复合粉体具有较好的光催化活性,且三次循环利用后仍具有较好的催化活性,在模拟太阳光辐照下,CdS/zeolite(0.5 M)复合粉体重复利用3次后,处理260 min对RhB的降解率仍可达91.3;.所得粉体对RhB的光催化过程符合一级动力学方程式,光催化过程中,RhB 紫外可见光谱的蓝移现象揭示所得CdS/沸石分子筛可通过脱乙基-共轭显色基团断裂途径降解RhB.     

GO/Tb4 O7复合材料的光催化性能研究

以氧化石墨烯(GO)和氧化铽(Tb4 O7)为原材料,采用水热法制备了GO/Tb4 O7复合粉体.通过SEM、XRD和分光光度计等手段对复合材料粉体进行了分析.用罗丹明B溶液作为模拟污染物,在光催化反应仪中采用紫外光照射不同时间后,利用分光光度计测试其光催化性能.实验结果表明:复合材料粉体中,氧化铽颗粒基本可以均匀的分布在GO表面;随着GO含量(6;,8;,10;)的增加,复合材料粉体和罗丹明B的反应速率逐渐加快;在60 min时三种复合材料粉体的降解率分别为98.40;、98.64;、98.94;.     

Bi4Ti3O12/BiOBr复合材料的溶剂热合成及可见光催化性能

采用一步溶剂热法合成了Bi4Ti3O12/BiOBr复合光催化剂,采用X-射线衍射仪(XRD)、扫描电子显微镜(SEM)、比表面积及孔径测定仪(BET)以及紫外可见漫反射光谱仪(DRS)等对样品的组成、形貌及可见光催化性能等进行了表征,讨论了合成条件对样品光催化活性的影响,探究了光催化反应过程中的活性物种及反应机理.研究结果表明,Bi、Ti、Br的投料比为10∶7∶5、乙二醇为溶剂、聚乙烯吡咯烷酮为表面活性剂且加入量为0.2g时,合成样品具有较高的光催化活性和较好的循环稳定性.在7 W LED灯照射140 min后,光催化剂对罗丹明B(RhB)的降解率达到85.1;.·O2-与h+在降解过程中起主要作用.     

α-Fe2O3/TiO2光催化剂的制备及可见光催化降解罗丹明B的研究

采用浸渍法制备不同掺杂量的负载型光催化剂 α-Fe2O3/TiO2,通过XRD、SEM-EDX、XPS和N2-sorption等手段对其进行表征,并研究其在可见光照射下对罗丹明B的降解性能.考察了不同掺杂量的复合纳米粒子、不同浓度的H2O2溶液、不同pH等条件对可见光降解罗丹明B的影响.结果表明,复合α-Fe2O3/TiO2催化剂的光催化活性均高于单一的α-Fe2O3或TiO2,其中α-Fe2O3掺杂量为6.0wt;的α-Fe2O3/TiO2的光催化活性和光降解稳定性最好.     

低温水热法制备高催化效率钒酸铋可见光催化剂

采用低温水热合成法,通过控制反应体系pH值实现了对晶体形貌的调控,制备了高催化效率的单斜相钒酸铋催化剂.对样品进行了X射线衍射、紫外可见漫反射吸收光谱、扫描电镜和比表面积分析,并以罗丹明B的降解考察了样品的光催化活性.结果表明,反应体系pH值影响钒酸铋的形貌和光催化性能,pH值为7条件下制备得到的BiVO4样品对罗丹明B的光催化降解率最大,光催化反应lh对罗丹明B的降解率为93.56;.H2O2作为电子捕获剂,与电子反应形成羟基自由基,抑制电子和空穴对的复合,H2O2协同催化显著提高了光催化效率.     

微波合成Bi2S3/g-C3N4复合光催化剂及其光催化性能研究

采用微波合成法制备了Bi2 S3/g-C3 N4复合光催化剂,利用X射线衍射(XRD)、傅里叶红外光谱(FT-IR)、X射线光电子能谱(XPS)、紫外可见-漫反射吸收光谱(Uv-vis)、物理吸附仪(BET)等对其进行了表征,以罗丹明B(RhB)为目标化合物对其光催化性能进行了评价.结果表明,与纯Bi2 S3和g-C3 N4相比,复合样品的禁带宽度变小,比表面积增大,光生载流子的复合效率降低,显著提高了其光催化降解RhB的效率.复合样品5-CNBS对RhB的降解率达99;以上,分别是纯g-C3 N4和Bi2 S3单体对RhB降解效率的1.59倍和4.95倍.     

CdS/煤矸石复合粉的声化学法制备及光催化性能

采用EDTA对煤矸石粉进行了表面改性,然后以表面改性煤矸石粉、乙酸镉和硫代乙酰胺为原料,采用超声化学法制备了CdS/煤矸石复合粉体.采用X射线粉末衍射(XRD)、高分辨透射电子显微镜(HRTEM)、扫描电子显微镜(SEM)以及所带能谱仪(EDS)对所制得的样品进行了表征,并以紫外光为光源,甲基橙为目标降解物,对其光催化活性进行了研究.结果表明:煤矸石表面有许多直径100 nm左右絮状球形立方相CdS小颗粒包覆着;CdS/煤矸石复合粉体表现出较高的光催化降解能力,在60W紫外灯辐照下,CdS/煤矸石的复合粉体重复利用3次后,处理3h对甲基橙的降解率仍可达92.8;.     

石墨烯/Fe3O4/ZnO磁性纳米催化材料的制备及其性能研究

以石墨烯为助催化剂,借助水热法合成石墨烯/Fe3O4/ZnO磁性纳米复合光催化材料对ZnO改性.光催化降解测试显示复合材料对对硝基苯酚和罗丹明B降解率可分别达到95.7;和94.2;,重复试验3次后,降解率仍超过90;.对复合材料在光催化体系中磁性回收利用进行了研究,其饱和磁化强度为23.05 emu·g-1,并讨论了其光催化反应机理.     

Triethyl ammonium salt of O,O′-bis(p-tolyl)dithiophosphate, [Et3NH]+[(4-MeC6H4O)2PS2]−

Triethyl ammonium Salt of O,O′-bis(p-tolyl)dithiophosphate and O,O′-bis(m-tolyl)dithiophosphate have been obtained by reaction of p- and m-cresol, respectively with P₂S₅ in toluene and have been characterized by elemental analysis, IR, ¹H and ³¹P NMR spectroscopy. The molecular structure of O,O′-bis(p-tolyl)dithiophosphate has been determined. Crystal data: [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻: Monoclinic, P2₁/c, a=15.2441(9) ?, b=10.415(2) ?, c=3.9726(9) ?, β=91.709(7)°, V=2217.5(1) ?⁻³, Z=4.Supplementary materials Additional material available from the Cambridge Crystallographic Data Centre (CCDC no. 600927 for [Et₃NH]⁺[(4-MeC₆H₄O)₂PS₂]⁻ comprises the final atomic coordinates for all atoms, thermal parameters, and a complete listing of bond distances and angles. Copies of this information may be obtained free of charge on application to The Director, 12 Union Road, Cambridge CB2 2EZ, UK (fax: +44-1223-336033; email: deposit@ccdc.cam.ac.uk or www:http://www.ccdc.cam.ac.uk).     

First-principles coexistence simulations of supercooled liquid silicon

We perform first-principles coexistence simulations of the low-density and the high-density phases of supercooled liquid silicon and find a negative slope for the coexisting line in the temperature-pressure plane. Electron density maps and electron-localization function plots of the two phases of silicon show marked differences. The calculated differences suggest more localized electrons in the low-density liquid compared to the high-density liquid, coming from an increased population of covalent bonds, which further explain the calculated negative slope in the two phase coexistence regime. This is consistent with the presence of a pseudo-gap in low-density liquid silicon, absent in the high-density liquid which shows a metallic behavior.     

Crystal structures of thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane

Structures of both thecis andtrans isomers of dithiahexahydro[3.3]metacyclophane, ?C₆H₄?CH₂SCH₂?C₆H₁₀?CH₂SCH₂?, have been determined, wherecis andtrans refer to the attachments to the cyclohexane ring. Thecis form crystallizes in the monoclinic space groupP2₁/c witha=8.4299(11)Å,b=21.772(2)Å,c=8.9724(13)Å, β=116.574(11)^o, andZ=4. Thetrans isomer packs into the monoclinic space groupP2₁ witha=8.159(16)Å,b=10.185(5)Å,c=9.558(2)Å, β=112.435(18)^o, andZ=2. The cyclohexane ring of thecis isomer is in the chair conformation, while the cyclohexane of thetrans isomer is found in a twisted boat conformation.     

CTAB与SDBS对碳酸锶粒子生长形态调控及机理研究

以表面活性剂CTAB和SDBS为化学添加剂,采用化学共沉淀法对碳酸锶晶体的生长形态进行调控,成功地制备出了实心的树枝状和花瓣为空心的花状碳酸锶粉体,并用X射线衍射(XRD)、扫描电子显微镜(SEM)和傅里叶变换红外光谱(FT-IR)等分析手段对样品进行了表征;最后重点对化学添加剂可能产生的影响机理进行了初步的探讨.结果表明,CTAB和SDBS在晶体生长的过程中能起到显著的影响作用,两者对粒子分散性能的作用效果相反,而且后者对晶体(013)和(213)晶面表面能降低的贡献明显大于前者.     

Crystal structure of Zn4Na(OH)6SO4Cl·6H2O

The structure of Zn₄Na(OH)₆SO₄Cl·6H₂O, a secondary mineral from Hettstedt, Germany, was determined by single-crystal X-ray diffraction. The crystals are hexagonal,a=8.413(8),c=13.095(24) Å, space group $P\bar 3$ , Z=2. The structure was refined to R=0.0554 and R_w=0.0903 for 970 reflections with I≥3σ(I). The structure can be described as zinc hydroxide layers perpendicular toc, from which sulfates and chlorides extend. The layers are held together by a system of hydrogen bonds involving hexaaquo Na⁺ ions which occupy the interlayer space.     

Synthesis and Crystal Structure of 5-[2-(6-bromonaphthalenyloxymethyl)]-3-(4-morpholinomethyl)-1,3,4-oxadiazole-2(3<Emphasis Type="Italic">H</Emphasis>)-thione

Abstract  The title compound, C₁₈H₁₈BrN₃O₃S, a derivative of 1,3,4-oxadiazole, crystallizes in the triclinic space group P-1 with unit cell parameters a = 6.8731(3), b = 8.9994(4), c = 15.7099(6) ?, α = 92.779(3)°, β = 130.575(3)°, γ = 107.868(4)°, Z = 2. The dihedral angle between the mean planes of the planar naphthyl and morpholine (chair) rings with the planar oxadiazol ring is 50.1(8) and 76.8(6)°, respectively. The planar naphthyl ring is twisted 52.2(5)° with the mean plane of the morpholine ring. A group of four intermolecular close contacts are observed between a bromine atom and hydrogen atoms from the closely packed naphthyl, morpholine and oxy–methyl groups in the unit cell. These molecular interactions in concert with an additional series of π–π stacking interactions that occur between the center of gravity of the two 6-membered rings of the naphthalene group influence the twist angles of each of these three groups. A MOPAC AM1 calculation of the conformation energy of the crystal structure [226.0128(9) kcal] compared to that of the minimum energy structure after geometry optimization [29.9744(1) kcal] reveals a significantly reduced value. The twist angles of the three groups above also change after the AM1 calculation giving support to the influence of both intermolecular C–H···Br short-range interactions and Cg π–π stacking interactions on these angles which therefore play a role in stabilizing crystal packing. Graphical Abstract  Crystal structure of 5-{[(6-bromonaphthalen-2-yl)oxy]methyl}-3-(morpholin-4-ylmethyl)-1,3,4-oxadiazole-2(3H)-thione, C₁₈H₁₈BrN₃O₃S, is reported and its geometric and packing parameters described and compared to a MOPAC computational calculation. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Crystal structure of irisolidone from the flowers of Pueraia lobata

Irisolidone (5,7-dihydroxy-6,4′-dimethoxyisoflavone) was isolated from the flowers of Pueraia lobata and its crystal structure was examined by X-ray single crystal diffraction. The crystal structure of irisolidone is monoclinic, space group P2₁/c with a = 15.491(9) ?, b = 7.895(4) ?, c = 13.321(7) ?, β = 110.546(9)° and Z = 4. Hydrogen bonding and aromatic π–π stacking assemble the title compound into a three-dimensional networking structure.     

Synthesis of spinacine and spinacine derivatives: crystal and molecular structures of Nπ-hydroxymethyl spinacine and Nα-methyl spinaceamine

The natural amino acid L-Spinacine (4,5,6,7-tetrahydro-1H-imidazo[4,5-c]pyridine-6-carboxylic acid) has been synthesized following a new pathway which gives a chemically and optically pure product with an excellent yield. The crystal structures of a synthetic intermediate, N^π-hydroxymethyl-spinacine, and a spinacine derivative, N^α-methyl-spinaceamine, have been investigated through X-ray diffraction: Spi(πMeOH)·H₂O, monoclinicP2 _i,a=8.571(1),b=6.682(1),c=8.588(1) Å, and β=94.67(1)^o. Spm(αMe)·2HCl·H₂O, triclinicP l,a=7.492(4),b=10.799(3),c=7.040(2) Å, α=91.88(2), β=98.36(3) and γ=73.34(3)^o. Spi(πMeOH) crystallizes with a water molecule and displays a zwitterionic character. The carboxylate group is in equatorial position and forms a short electrostatic interaction of 2.618(2) Å between one of its oxygens and the protonated nitrogen of the tetrahydropyridine ring. The crystal packing is assured by strong O?H???O, O?H???N, N?H???N intermolecular hydrogen bonds and C?H???O close contacts. The biprotonated compounds Spm(αMe) crystallizes with two Cl^? anions and a water molecule. The positive charge on the imidazole ring is delocalized on the conjugated moiety N=C?N. The crystal is built up by clusters formed by two biprotonated Spm(αMe) molecules, four Cl^? anions and two water molecules linked together by hydrogen bonds.