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1.
SiO负载磷钨钒杂多酸杂化材料的制备及其氧化脱硫性能的研究 《燃料化学学报》2016,44(9):1099-1104
利用磷酸氢二钠、偏钒酸纳和钨酸钠为原料,合成了具有Keggin结构的磷钨钒杂多化合物(H5PW10V2O40),并与1-丁基-3-甲基咪唑溴(BmimBr)离子液体反应生成一种杂多酸杂化材料([Bmim]5PW10V2O40)。利用红外光谱(FT-IR)、X射线衍射光谱(XRD)和紫外可见光谱(UV-vis)对所合成的杂多酸杂化材料进行表征。结果表明,[Bmim]5PW10V2O40具有咪唑阳离子基团和Keggin型杂多阴离子基团的结构特征,并且两种基团之间存在相互作用。以SiO_2为载体制备负载型的杂多酸杂化材料催化剂[Bmim]5PW10V2O40/SiO_2,以H2O_2作为氧化剂,考察该催化剂对模拟油中DBT的氧化性能,并优化氧化反应条件,在反应温度40℃,O/S物质的量比为3.0的条件下,反应50min,模拟油品中的DBT的转化率可以达到100%。催化剂可以通过离心法分离,经过干燥之后,可以循环使用至少七次,而对DBT的氧化活性没有降低。 相似文献
2.
Xiao-Bing Cui Ji-Qing Xu Lan Ding Hong Ding Ling Ye Guo-Yu Yang 《Journal of Molecular Structure》2003,660(1-3):131-137
The compound [Zn(H2O)4]2[H2As6V15O42(H2O)]·2H2O (1) has been synthesized and characterized by elemental analysis, IR, ESR, magnetic measurement, third-order nonlinear property study and single crystal X-ray diffraction analysis. The compound 1 crystallizes in trigonal space group R3, a=b=12.0601(17) Å, c=33.970(7) Å, γ=120°, V=4278.8(12) Å3, Z=3 and R1(wR2)=0.0512 (0.1171). The crystal structure is constructed from [H2As6V15O42(H2O)]4− anions and [Zn(H2O)4]2+ cations linked through hydrogen bonds into a network. The [H2As6V15O42(H2O)]6− cluster consists of 15 VO5 square pyramids linked by three As2O5 handle-like units. 相似文献
3.
以NH4VO3, H3PMo12O40·xH2O, Cu(NO3)2和哌嗪为主要原料,采用水热方法,合成了一个新的钼钒二聚体簇合物--(H2NC4H8NH2)6[MoVI16VV12P2O84]·5H2O(1),其结构和性能经UV-Vis, IR, X-射线衍射、光电子能谱及热重分析表征。1属单斜晶系,P2(1)/c空间群, 晶胞参数a=20.450(4) , b=24.989(5) , c=20.450(4) , β=93.89 °, V=10 427(4) 3, Fw=4 159.18, Dc=2.650 g·cm-3, μ=3.018 mm-1, F(000)=7 952, Gof=1.029。晶体结构解析表明:1由两个单元Keggin型簇核[PMo8V6O42]7-聚合而成一个二聚体簇[P2Mol6V12O84]14-,该二聚体簇核和有机配体哌嗪之间通过复杂的氢键相互作用,展示三维超分子网络结构。 相似文献
4.
ZHOU Yun-shan HASSAN ul Sadaf LI Xian-qi ZHANG Li-juan AHMAD Waqar SHI Zong-hai 《高等学校化学研究》2013,29(4):621-626
Structural comparison of a new compound[(bpp)3H6]Fe2IIIFe2IIMo24V(H2PO4)8(HPO4)4(PO4)4O48(OH)12· (H2O)4·2H2O(1)[bpp=1,3-di(4-pyridyl)propane] with our previously reported two compounds[(bpy)3FeII]3· Fe2IIIFe2IIMo24V(H2PO4)8(HPO4)4(PO4)4O48(OH)12(H2O)4·12H2O(2) and[(bpy)3FeII]2FeIIFeIIIMo12V(H2PO4)2(H2-xPO4)·(H1+xPO4)(HPO4)2(PO4)2O24(OH)6(H2O)2·9H2O(x=0―1)(3)(bpy=2,2'-bipyridine), which all exhibit one-dimensional mixed-valence iron molybdophosphate anionic chains constructed by alternating connection of FeIII ions and magic[FeII(Mo6P4O31)2] units, reveals that the non-hydrogen atomic ratios of Mo:Fe:P:O within the polymeric anionic chains are the same for all the three compounds, while the polymeric anionic chains of the different compounds bear different numbers of negative charges. And therefore there exist different numbers of counter cations per {Fe2III[Fe2II(P16Mo24VO124)]} unit found in the titled compounds. It discloses that not only are the spatial assembling of counter cations and polymeric inorganic chains of three compounds quite different, but also the O―FeIII―O bond angles and FeIII―O bond lengths of the three different inorganic chains exhibit small differences. What is more important is that such small changes in bond length and bond angle in the assemblage of FeIII―O bonds lead to the considerable fluctuations of inorganic chains in their structural conformation within the three compounds, reflecting an interesting phenomenon of “flexibility" in the pure inorganic one dimensional mixed-valence iron molybdophosphate chains. 相似文献
5.
Based on a new biscarboxyl-functionalized Schiff base ligand 1,2-cyclohexanediamino-N,N'-bis[3-methoxyl-5-(p-carboxyl-phenylazo)] salicylidene(H4L), four polymers,[(CH3)2NH2]2·[Mn3(L)2(H2O)4]·2DMF(CP1),[Fe2(L)(H2O)(DMF)](CP2),[(CH3)2NH2]·[Cu(HL)]·H2O(CP3) and[Ni2(L)(teta)]·2DMF·H2O(CP4), have been synthesized(teta=5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane). In CP1, both of the internal[N2O2] pocket and the external carboxylate groups of L4- anion are ligated by Mn2+ ions, and the structure displays a layer. In CP2, the Fe2+ cations are linked by L4- anions to form a binuclear double chain. CP3 displays a[Cu2(HL)2] dimer. In CP4, the Ni2+ ions are connected by L4- anions to form a chain. The structures are further linked by hydrogen bonds to form 2D or 3D supramolecular architectures, respectively. CP1 exhibits adsorption ability to three organic dyes. 相似文献
6.
Structural tuning of coordination polymers by 4-connecting metal node and secondary building process
Due to variation in ligand's conformation, metal node's connecting geometry, and secondary building process by anions, bat-like, dumbell-like, diamondoid, or pillar-layer topologies are achieved. 相似文献
7.
ZHOU Yunshan QU Ningning WANG Xuan ZHANG Lijuan SHI Zonghai HASSAN ul Sadaf 《高等学校化学研究》2014,30(5):715-719
Abstract By reacting the unique Keplerate type molybdenum-oxide based polyoxometalate (NH4)42·[MoI320372·(CH3COO)30(H2O)y2]·ca.300H2·ca. 10CH3COONH4(1) with tetramethylammonium bromide, a new derivative (NH4)26[TMA]16{MoI32O372(H2O)72(CH3COO)30}·ca.7NH4CH3COO·ca.189H2O(2, TMA=tetramethylammonium) was prepared. Compound 2 was characterized by Fourier transform infrared spectroscopy(FTIR), UV-Vis, elemental and thermogravimetric analyses. By the well-established Z-scan technique, investigations on the nonlinear opti- cal(NLO) properties of the series of compounds derived from the Keplerate type molybdenum-oxide-based poly- oxometalate, namely, the newly prepared compound 2, the three previously reported compounds, included compound 1, (NH4hs(TBA)24{Mo132O372(H2O)72(CH3COO)30}·ca.7NH4CH3COO·ca. 173H2O(3, TBA=tetrabutylammonium) and (DODA)40(NH4)2[(H2O)nMo132O372(CH3COO)3o(H20)72](4, DODA=dimethyldioctadecylammonium), reveal that the third-order nonlinearity[x(3)] values of compounds 1, 2 and 3 in the DMF/H2O solution and compound 4 in chloro- form are almost the same, which indicates that the counter cations with different length of alkyl chains show ignora- ble impacts on the NLO susceptibility. In other words, the remarkable third-order nonlinearities[x(3)≈10 19 m2/V2] mainly come from the [MoI32O372(CH3COO)30(H2O)72]42 anions. This fact reveals that the applications of the NLO active polyoxometalates in various environments(such as hydrophilic, hydrophobic, polar, apolar, etc.) can be achieved by simply varying cations to meet the demands in the design of diverse devices. Keywords Keplerate type polyoxometalate; Nonlinear optical property; Z-Scan technique; Self-defocusing; Reverse saturable absorption 相似文献
8.
在水热和弱酸性反应条件下,螯合型表面活性剂前驱体乙二胺三乙酸分别与氯化锌、氯化钴反应,形成水合乙二胺三乙酸金属配合物[M(H2O)6][M(ED3A)(H2O)]2·2H2O[M=Zn(1),Co(2);H3ED3A=乙二胺三乙酸,C8H14N2O6]。 产物经元素分析、红外、热重、液体核磁共振和X射线单晶衍射结构表征。 乙二胺三乙酸和锌(Ⅱ)、钴(Ⅱ)五配位,并与水一起形成典型的[MN2O4]或[MO6]八面体结构。 13C核磁共振实验结果表明,溶液中乙二胺三乙酸与锌形成配合物在弱酸性条件下(pH值3~7)稳定存在,在酸性溶液中完全解离,乙二胺三乙酸进一步经分子内成环反应生成3-酮哌嗪二乙酸(H2kpda=C8H12N2O5)。 相似文献
9.
通过水热方法合成了2个由多铌酸盐和过渡金属配合物形成的有机-无机杂化配合物[Cu(TETA)]4[VNb12(VO)4O40][OH]·10H2O(1)和[Cu(TETA)]4[VNb12(VO)6O40][OH]5·5H2O(2)(TETA=三亚乙基四胺). 化合物1和2的多阴离子分别是由4个{VO5}帽和6个{VO5}帽加盖在Keggin型多铌酸盐的方形缺口上形成的, 它们通过多酸阴离子中Nb-Ot (Ot =端氧)与[Cu(TETA)]2+配合物的金属中心配位构筑形成三维结构. 价键计算结果表明, Keggin中心的钒为+5价, 帽位的钒为+4价, X射线光电子能谱分析(XPS)结果也证实了这一结论. 通过单晶X射线衍射分析、红外光谱(IR)、粉末X射线衍射(PXRD)、热重(TG)分析和元素分析对这2个化合物的结构和性质进行了表征. 相似文献
10.
Optimised hydrothermal synthesis of multi-dimensional hybrid coordination polymers containing flexible organic ligands 总被引:2,自引:0,他引:2
Filipe A. Almeida Paz Joo Rocha Jacek Klinowski Tito Trindade Fa-Nian Shi Luís Mafra 《Progress in Solid State Chemistry》2005,33(2-4):113-125
In this paper, we summarise our recent research interest in the hydrothermal synthesis and structural characterisation of multi-dimensional coordination polymers. The use of N-(phosphonomethyl)iminodiacetic acid (also referred to as H4pmida) in the literature as a versatile chelating organic ligand is briefly reviewed. This molecule plays an important role in the formation of centrosymmetric dimeric [V2O2(pmida)2]4− anionic units, which were first used by us as building blocks to construct novel coordination polymers. Starting with [V2O2(pmida)2]4− in solution, we have isolated [M2V2O2(pmida)2(H2O)10] species (where M2+ = Mn2+, Co2+ or Cd2+) via the hydrothermal synthetic approach, which were then employed for the construction of [CdVO(pmida)(4,4′-bpy)(H2O)2]·(4,4′-bpy)0.5·(H2O), [CoVO(pmida)(4,4′-bpy)(H2O)2]·(4,4′-bpy)0.5, [Co(H2O)6][CoV2O2(pmida)2(pyr)(H2O)2]·2(H2O) and [Cd2V2O2(pmida)2(pyr)2(H2O)4]·4(H2O) by the inclusion of bridging organic ligands in the reactive mixtures, such as pyrazine (pyr) and 4,4′-bipyridine (4,4′-bpy). These materials can contain channel systems, and exhibit magnetic behaviour, not only due to the V4+ centres but also to the transition metal centres which establish the links between neighbouring dimeric [V2O2(pmida)2]4− anionic units. A closely related anionic moiety, [Ge2(pmida)2(OH)2]2−, was engineered to allow the study of such crystalline hybrid materials using one- and two-dimensional high-resolution solid-state NMR. 相似文献
11.
Two new compounds,[ErAg(INA)2(C2O4)]·2H2O(1)(HINA=nicotinic acid) and [Tb0.8Y0.2Ag2(IN)4·(H2O)5]·NO3·2H2O(2)(HIN=isonicotinic acid),based on the {Ln2} building units,have been hydrothermally synthesized and characterized by single-crystal X-ray diffraction,infrared spectroscopy,thermal analysis and powder X-ray diffraction(PXRD).Single-crystal X-ray diffraction data reveal that both compounds crystallized in the low-symmetry triclinic space group P1-.Compound 1 is a 3D heterometallic coordination framework based on {Er2}clusters,oxalate ligands and bridging [Ag(INA)] linkers,while compound 2 consists of 0D [Tb0.8·Y0.2Ag2(IN)4(H2O)5]2 subunits that give a 3D supramolecular structure through hydrogen bond interaction.The photoluminescent properties of both compounds(1 and 2) were studied. 相似文献
12.
多金属氧酸盐 (也称金属 -氧簇 )由于在催化、材料及医药等领域的应用日益广泛而备受关注 .近年来 ,一些新颖的非经典结构的化合物不断被合成出来 .如带二帽的 Keggin结构化合物 [V15O4 2 ]9- [1] ,[PV14 O4 2 ]9- [2 ] ,[As V14 O4 2 ]9- [3 ] ,[{ Mo8V7O4 2 } 2 ]14 - [4 ] , 相似文献
13.
Three novel scandium-containing heteropolytungstates[Sc3(H2O)3NO3(PW9O34)2]10-(1a),[Sc8(H2O)2(GeW9O34)2(GeW6O26)2]12-(2a) and[Sc11(W6O10)2(OH)2(H2O)16(BiW9O33)6]27-(3a) were synthesized by reactions of ScIII ions with trilacunary Keggin precursors,[A-α-XW9O34]n-(X=P, Ge, n=9, 10) or[B-α-BiW9O33]9-, in NaOAc/HOAc buffer solution under conventional synthetic condition, respectively. All the three compounds were characterized by means of single-crystal X-ray diffraction(XRD), Fourier transform-infrared(FTIR) spectroscopy ultraviolet-visible(UV-Vis) spectroscopy, elemental analysis, and thermogravimetric analysis. The aqueous solution stability of the sandwich polyanion[Sc3(H2O)3NO3(PW9O34)2]10- was also verified by electrospray ionization mass spectrometry(ESI-MS) due to its good solubility in water. 相似文献
14.
制得硝酸钪与两种冠醚的固态络合物,确定其组成为Sc(NO3)3·C16H20O7·H2O及Sc(NO3)3·C14H16O6·H2O。研究了冠醚本身及其钪的相应络合物的合成及有关性质。 相似文献
15.
Yanjuan Qi Yonghui Wang Hongmei Li Minhua Cao Changwen Hu Enbo Wang Ninghai Hu Hengqing Jia 《Journal of Molecular Structure》2003,650(1-3):123-129
The hydrothermal reactions of vanadium oxide starting materials with divalent transition metal cations in the presence of nitrogen donor chelating ligands yield the bimetallic cluster complexes with the formulae [{Cd(phen2)2V4O12]·5H2O (1) and [Ni(phen)3]2[V4O12]·17.5H2O (2). Crystal data: C48H52Cd2N8O22V4 (1), triclinic.
a=10.3366(10), b=11.320(3), c=13.268(3) Å, =103.888(17)°, β=92.256(15)°, γ=107.444(14)°, Z=1; C72H131N12Ni2O29.5V4 (2), triclinic.
a=12.305(3), b=13.172(6), c=15.133(4), =79.05(3)°, β=76.09(2)°, γ=74.66(3)°, Z=1. Data were collected on a Siemens P4 four-circle diffractometer at 293 K in the range 1.59° <θ<26.02° and 2.01°<θ<25.01° using the ω-scan technique, respectively. The structure of 1 consists of a [V4O12]4− cluster covalently attached to two {Cd(phen)2}2+ fragments, in which the [V4O12]4− cluster adopts a chair-like configuration. In the structure of 2, the [V4O12]4− cluster is isolated. And the complex formed a layer structure via hydrogen bonds between the [V4O12]4− unit and crystallization water molecules. 相似文献
16.
室温固相反应制备Keggin结构杂多酸铵盐纳米粒子 总被引:19,自引:1,他引:18
纳米材料由于其量子尺寸效应及表面效应而在磁、光、电等方面显示出许多常规粒子所不具有的特性[1] .纳米材料成功应用的实例及潜在应用前景推动了各种纳米粉末的合成及合成方法的发展 [2~ 4 ] .利用低温固相反应制备纳米粒子尚不多见 ,但已有报道 [5,6] .多金属氧酸盐因其独特的结构而具有较高的催化活性、导电性、磁性、光电致变色性以及抗病毒活性 ,因而有着广阔的应用前景 ,这些方面的研究已越来越引起人们的兴趣 [7~ 10 ] .本文采用室温固相反应首次制备了多金属氧酸盐纳米粒子 (NH4 ) 3PMo12 O4 0 · 9H2 O(1 )和 (NH4 ) 3PW12… 相似文献
17.
[Zn(phen)3]·ZTO·6H2O(1) and[Cu(phen)3]·ZTO·6H2O(2) were synthesized by the reaction of Zn(NO3)2·6H2O/Cu(NO3)2·3H2O with 4,4-azo-1H-1,2,4-triazol-5-one(ZTO) and 1,10-phenanthroline(phen). The two compounds were characterized by elemental analysis and IR spectrum analysis, respectively. Compound 1 was also characterized by single crystal X-ray diffraction analysis. For compound 1, the coordination geometry around the Zn2+ is a distorted octahedron, with the bite angles of 76.7(3)°-77.6(4)° for all three phen ligands. Moreover, the thermal behaviors and thermal decomposition kinetics were studied and analyzed. Besides, thermal stability and safety parameters(TSADT, Tb) are 164.7 and 166.4℃ for compound 1, and 149.6 and 150.8℃ for compound 2, respectively. 相似文献
18.
新型杂多酸盐光催化降解亚甲基蓝染料废水 总被引:2,自引:0,他引:2
以水热自组装法合成的新型杂多酸盐[PMo8V6O42][Co(Phen)2][Him]2·2H3O·3H2O(1),通过红外光谱、拉曼光谱、紫外-可见光谱、光电子能谱和X粉末衍射等技术手段进行表征。 以此物质为催化剂光催化降解亚甲基蓝染料废水。 分别讨论催化剂投加量、亚甲基蓝废水初始浓度、废水溶液酸度(pH)对亚甲基蓝降解率的影响。 实验结果表明:催化剂投加量为50 mg/L、亚甲基蓝初始浓度为4 mg/L、模拟废水溶液的初始pH=1、降解时间220 min时,废水降解率可达到99.2%。 光催化动力学分析显示,以合成杂多酸盐为催化剂光催化降解亚甲基蓝废水降解过程满足一级动力学方程,该一级方程反应速率常数为0.0144 min-1,拟合常数为0.9918。 另外,此催化剂还表现出较好的重复使用性能,连续使用5 次后降解率仍为92.4%。 相似文献
19.
Two novel 3D supramolecular architectures with hexamolybdate and phosphotungstate anions were synthesized under ionothermal conditions. The structures were named as[CuI(L1)2]2L2[Mo6O19](1) and[CuI(L3)2]2.5· H0.5[PW12O40]·H2O(2)(L1=2,2'-bipyridine, L2=4,4'-bipyridine, L3=2,2'-biimidazole) and characterized via Fourier transform infrared spectroscopy(FTIR) and FT-Raman spectroscopy analyses. Single-crystal X-ray diffraction analysis revealed that the two compounds crystallized in the space group P and were constructed through hydrogen bonding. 相似文献
20.
YU Yang LIU Dan HU Wei-wei LI Jia PENG Yu ZHOU Qi YANG Fen LI Guang-hua SHI Zhan FENG Shou-hua 《高等学校化学研究》2012,28(2):186-190
Three metal molybdate hydrates,Fe(H2O)2(MoO4)2·H3O(FeMo),NaCo2(MoO4)2(H3O2)(CoMo)and Mn2(MoO4)3·2H3O(MnMo),were synthesized by the mixed-solvent-thermal methods and characterized by singlecrystal X-ray... 相似文献