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自从系列磷酸铝微孔晶体首次被报道以来, 空旷骨架磷酸盐化合物的合成取得了长足进展[1,2]. 其中, 空旷磷酸镓骨架化合物以其丰富的拓扑连接方式成为研究的热点之一[1,3,4]. 特别是向水热合成体系中引入氟离子, 导致了新颖微孔磷酸镓化合物的不断出现, 如磷酸镓-CLO[5], 磷酸镓MIL-31[6]等化合物. 目前, 合成实验表明, 乙烯胺类化合物(如二乙烯三胺)因其构象变化复杂, 可以诱导出多种新颖空旷骨架磷酸盐[7~9]. 由于氟离子可以同磷酸镓骨架中的镓原子配位, 进而改变骨架拓扑连接方式和电荷分布, 因此氟原子与二乙烯三胺协同作用可能获得新颖的无机骨架与导向剂的自组装模型. 相似文献
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自 Parise报道微孔磷酸镓化合物以来 ,又不断有新颖磷酸镓骨架的化合物见报 [1~ 3] .与磷酸铝化合物相比 ,磷酸镓化合物中的镓原子具有明显的五、六配位形成倾向 ,由镓氧多面体结构单元可生成相当数量的与沸石类 ( zeotype)结构不同的新型拓扑结构 [3~ 5] .已有人采用向体系中引入氟离子与非水溶剂热的典型合成方法丰富了磷酸镓族系的结构类型 ,如 :Ga PO- CLO[5]与 NTHU- 1 [6 ] .最近 ,我们报道了一种新颖的镓化合物 [Ga3( PO4 ) 3F2 ]( H3O) ( H3NCH2 CH2 ) 2 NH2 [7] ,其中氟参与了骨架的构建 .作为对比 ,本文考察了体系中… 相似文献
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过渡金属磷酸盐是空旷骨架磷酸盐体系中重要的组成部分[1~3]. 几种由碱金属或碱土金属作为平衡阳离子的磷酸钴的研究已被报道[4~5]. 采用有机胺结构导向剂合成的具有空旷磷酸钴骨架结构的化合物亦见报道[6~9]. 本文采用中温水热合成技术合成出新颖的具有螺旋孔道的磷酸钴Co2(HPO4)2*H2O, 这种化合物在沸石拓扑集合中尚未发现结构对应成员. 相似文献
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由于在电学、磁学、光学、吸附、离子交换和催化等领域具有潜在的应用价值,具有开放骨架结构的金属磷酸盐的合成一直受到人们的广泛关注。在这些磷酸盐微孔化合物中,磷酸锌晶体是拓扑结构最为丰富的一种犤1犦。自从Stucky等犤2犦报道具有SOD、Li-ABW、FAU等已知结构磷酸锌的合成以来,已经有近百种具有0-D犤3,4犦,1-D犤5,6犦,2-D犤7~9犦,3-D犤10~13犦结构的磷酸锌被成功地合成出来。其中令人瞩目的是具有螺旋孔道的手性磷酸锌犤14犦以及具有二十四元环孔道的两种微孔磷酸锌化合物犤15,16犦的合成。这些化合物大多是采用水热技术以有… 相似文献
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《高等学校化学学报》2015,(11)
在无有机模板剂的条件下,以Na+离子为结构导向剂,通过水热合成法制备了一种与利用1,3-丙二胺合成的Uio-14具有相同层结构的二维磷酸铝化合物Na4[Al4P4O18]·H2O(1),通过单晶X射线衍射确定了其拓扑结构.利用粉末X射线衍射、扫描电子显微镜、电感耦合等离子体(ICP)元素分析和热重分析等对其物理化学性质进行了表征.结果表明,化合物1属于单斜晶系,空间群为P21/c,晶胞参数a=1.00887(9)nm,b=0.86747(8)nm,c=0.97580(9)nm,V=0.77387(12)nm3,Z=2,其阴离子层由铝氧三角双锥(Al O5)和磷氧四面体(PO4)构成,层间通过Na+离子平衡电荷;与Uio-14相比,化合物1具有更高的热稳定性,在400℃空气条件下煅烧后结构仍然保持完好.对化合物1的质子电导性能测试结果表明,相比于传统的分子筛类材料,化合物1展现出优异的质子电导性能,在55℃下质子电导率可达到1.19×10-3S/cm. 相似文献
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以哌嗪为模板剂,在水-乙醇混合溶剂体系中溶剂热合成了两个具有三维开放骨架结构的稀土硫酸盐[Ln4(H2O)4(SO4)10](C4N2H12)4(H2O)4(Ln = Gd,化合物1和Eu,化合物2),并对其进行了结构表征、热重以及荧光光谱分析. 单晶结构解析表明,化合物1和2属于同构异质,均结晶于单斜晶系,P21/c空间群,化合物1,a = 19.691(3) ?,b = 19.249(3) ?,c = 13.186(2) ?,β = 92.33(0)o,V = 4993.5(1) ?3, Z =4. 化合物2,a = 19.7233(8) ?,b = 19.2791(8) ?,c = 13.2095(5) ?,β = 92.329(1)o,V = 5018.7(3) ?3, Z =4. 两个化合物在ab平面上由SO4,GdO8和GdO9多面体共边或共角交错连接形成含有八元环和十六元环的二维层状结构,该二维层沿c方向平行排列,相邻层通过SO4四面体相连形成具有孔道的三维开放骨架结构,其孔道之中包含平衡骨架负电荷的质子化哌嗪分子. 化合物2的固体荧光光谱分析显示其在397nm激发波长下,表现出典型的Eu3+发光性质. 相似文献
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以外消旋的2-甲基-1,5-戊二胺(MPMD)为结构导向剂,在水热条件下合成出新磷酸铝化合物[Al4P5O19(OH)][C6H18N2](AlPO-MPMD)和新磷酸镓化合物[Ga8P8O32F5.5][C6H18N2]2[H30+]1.5(GaPO-MPMD).采用单晶x射线衍射结构分析、粉末x射线衍射分析(XRD)、热重-差热分析(TGA-DTA.A)、固体核磁共振(MAs NMR)、旋光分析(Optical rotation)以及振动圆二色光谱分析(Vibrational circular dichroism,VCD)等技术对产物进行了表征.对产物的VCD实验光谱和理论模拟光谱对比分析及旋光分析表明,在水热合成过程中,具有S构象的手性结构导向剂分子比具有R构象的手性结构导向剂分子更多地进入无机化合物骨架中,显示了手性对映体分子在该水热条件下的原位手性拆分. 相似文献
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pH对两步法非离子模板合成MSU-X类硅基介孔结构的影响 总被引:1,自引:0,他引:1
采用两步法以非离子型表面活性剂Tween 20为模板剂合成硅基介孔材料, 研究了pH对介孔材料结构的影响. 结果表明, 没有氟离子存在且模板剂浓度较低(约为2%(w))的条件下, 在弱酸性环境中(pH=3.32-4.26)可以制备有序的MSU-X类硅基介孔材料, 本研究中的简单合成体系有助于查明MSU-X合成机理. 对所得介孔材料测试表明, 在同样的合成体系中, 随着体系pH的变化, 所得硅基介孔材料的形貌和孔壁结构都发生了变化. 相似文献
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利用水热法在150 ℃合成了新的化合物六氟钛酸十六烷基三甲基胺二水合物([(n-C16H33)N(CH3)32[TiF6]·2H2O), 并利用单晶X射线衍射技术解析了其结构, 同时利用傅立叶变换红外光谱、元素分析及热分析技术加以佐证. 该化合物由六氟钛酸根离子(TiF2-6)、水分子及十六烷基三甲基胺离子([(n-C16H33)N(CH3)3]+)组成, 属于单斜晶系, 其空间群为C2/c. 氢键在其构筑三维结构时起着重要的作用. 相似文献
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Synthesis and Structure of New Sodium Hydrogen Sulfates Na(H3O)(HSO4)2, Na2(HSO4)2(H2SO4), and Na(HSO4)(H2SO4)2 Three acidic sodium sulfates have been synthesized from the system sodium sulfate/sulfuric acid and have been crystallographically characterized. Na(H3O)(HSO4)2 ( A ) crystallizes in the space group P21/c with the unit cell parameters a = 6.974(2), b = 13.086(2), c = 8.080(3) Å, α = 105.90(4)°, V = 709.1 Å3, Z = 4. Na2(HSO4)2(H2SO4) ( B ) is orthorhombic (space group Pna21) with the unit cell parameters a = 9.970(2), b = 6.951(1), c = 13.949(3) Å, V = 966.7 Å3 and Z = 4. Na(HSO4)(H2SO4)2 ( C ) crystallizes in the triclinic space group P1 with the unit cell parameters a = 5.084(1), b = 8.746(1), c = 11.765(3) Å, α = 68.86(2)°, β = 88.44(2)°, γ = 88.97(2)°, V = 487.8 Å3 and Z = 2. All three compounds contain SO4 tetrahedra as HSO4? anions and additionally in B and C in form of H2SO4 molecules. The ratio H:SO4 determines the connectivity degree in the hydrogen bond system. In A , there are zigzag chains and dimers additionally connected via oxonium ions. Complex chains consisting of cyclic trimers (two HSO4? and one H2SO4) are present in B . In structure C , several parallel chains are connected to columns due to the greater content of H2SO4. Sodium cations show a distorted octahedral coordination by oxygen in all three structures, the NaO6 octahedra being “isolated” (connected via SO4 tetrahedra only) in A . Pairs of octahedra with common edge form Na2O10 dimeric units in C . Such double octahedra are connected via common corners forming zigzag chains in B . 相似文献
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Abderrahmen Guesmi Mohamed Faouzi Zid Ahmed Driss 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(5):511-512
In the title compound, disodium cobalt tetrakis(dihydrogenphosphate) tetrahydrate, the CoII ion lies on an inversion centre and is octahedrally surrounded by two water molecules and four H2PO4 groups to give a cobalt complex anion of the form [Co(H2PO4)4(OH2)]2?. The three‐dimensional framework results from hydrogen bonding between the anions. The relationship with the structures of Co(H2PO4)2·2H2O and K2CoP4O12·5H2O is discussed. 相似文献
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[Mn(H2O)4(C4N2H4)][C6H4(COO)2] – An One‐Dimensional Coordination Polymer with Chain‐like [Mn(H2O)4(C4N2H4)]n2n+ Polycations Orthorhombic single crystals of [Mn(H2O)4(C4N2H4)][C6H4(COO)2] have been prepared in aqueous solution at room temperature. Space group Imm2 (no. 44), a = 1039.00(6) pm, b = 954.46(13) pm, c = 737.86(5) pm, V = 0.73172(12) nm3, Z = 2. Mn2+ is coordinated in a octahedral manner by four water molecules and two nitrogen atoms stemming from the pyrazine molecules (Mn–O 215.02(11) pm; Mn–N 228.7(4), 230.7(4) pm). Mn2+ and pyrazine molecules form chain‐like polycations with [Mn(H2O)4(C4N2H4)]n2n+ composition. The positive charge of the polycationic chains is compensated for by phthalate anions, which are accomodated between the chains. The phthalate anions are linked by hydrogen bonds to the polycationic chains. Thermogravimetric analysis in air revealed that the loss of water of crystallisation and pyrazine occurs in two steps between 130 and 245 °C. The resulting sample was stable up to 360 °C. Further decomposition yielded Mn2O3. 相似文献
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Prof. Dr. Friedrich Asinger Alfons Saus E. Fichtner H. -J. Gräber W. Leuchtenberger 《Monatshefte für Chemie / Chemical Monthly》1975,106(6):1449-1460
2H-Imidazole-4(3H)-thiones (a), available from methyl alkyl and methyl aryl ketones with sulfur and ammonia, react via their corresponding N-sodium compounds or in presence of tert. amines with alkyl and aryl carboxylic acid chlorides to give the corresponding intensely coloured (orange to violett) cryst. 3-acyl-2H-imidazole-4(3H)-thiones4 a-q and6–26. With dicarboxylic acid dichlorides the colourless cryst. N,N′-diacyl-bis-3-imidazoline-5-thiones5 a-d and27–32 are obtained. With carbamic acid chlorides and chloroformic acid esters the corresponding urea (33–35) and urethane derivatives36, 37 are formed. In an analogous way 2H-imidazol-4(3H)-ones react with acid chlorides to 3-acyl-2-imidazol-4(3H)-ones (44–50), which can also be obtained by treating the corresponding 3-acyl-2H-imidazole-4(3H)-thione with KMnO4. 相似文献
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Masato Hashimoto Michiru Kubata Atsushi Yagasaki 《Acta Crystallographica. Section C, Structural Chemistry》2000,56(12):1411-1412
The title compound, triammonium cis‐diaqua‐cis‐dioxo‐trans‐disulfatovanadate 1.5‐hydrate, was obtained by oxidizing VIV to VV in a 2 M sulfuric acid solution of vanadyl sulfate and adding ammonium sulfate. Here, the V atom is sandwiched by two sulfate groups by corner‐sharing to form a discrete [VO2(SO4)2(OH2)2]3? anion. The water molecules occupy cis positions in the equatorial plane of the vanadium octahedron. 相似文献