一个新颖三维配位聚合物Pb(1，4-napdc)(DMF)的合成、结构及热稳定性研究

A novel 3D metal-organic coordination polymer Pb(1,4-napdc)(DMF) (1,4-napdc=naphthalene-1,4-dicarboxylate) was synthesized at room temperature using slow vapor diffusion method to grow single crystal that has been analyzed by X-ray diffraction. The crystal belongs to orthorhombic with space group P2₁2₁2₁. The unit cell parameters are as fellows: a=0.701 3(2) nm, b=1.407 6(3) nm, c=1.521 5(4) nm, V=1.501 8(6) nm³ and Z=4. In the crystal structure of Pb(1,4-napdc)(DMF), the square grids constructed with paddle-wheel units of Pb(Ⅱ) and 1,4-napdc links stack over each other to generate infinite 3D network, which has square apertures (1.158×1.158 nm²) along the crystallographic a-axis. The thermal stability of compound was investigated by differential scanning calorimetry and thermogravimetric analysis. CCDC: 293617.     

A Large Conformational Change of a Bridged β-Cyclodextrin Dimer in Aqueous Solution

A novel bridged β-CD dimer in which two β-cyclodextrins were linked by a naphthalene at positions 2 and 7 has been synthesized. 1H and 13CNMR measurements showed that a large change in the conformation of the dimer occurred in aqueous solution. The dimer interacted with methyl and ethyl orange to form stable inclusion complexes via "induced fit" mechanism.     

Synthesis and Crystal Structure of 1,4-Bis(2-hydroxymethylphenyl)-1,4-dioxabutane

1 INTRODUCTION Macrocyclic ligands and their metal complexes have received much attention due to their applications in ion transport, ion separation and as models in biomimic researches[1~7]. The synthetic methods of macrocyclic ligands and their metal complexes are mainly divided into three kinds[8]. The first one is synthesizing free ligand, then forming the metal complexes; the second is template synthesis; and the third is synthesizing the end-off or side-off precursor ligand, then c…     

球形SiO2-Al2O3的制备、结构和性能

将Na2SiO3·9H2O 溶液通过强酸性阳离子树脂进行离子交换得到酸性硅溶胶,再将硅溶胶与铝溶胶及六次甲基四胺混合后采用油柱成型法制备了球形SiO2-Al2O3复合氧化物. 通过XRD、BET 及TPD等手段对样品进行测试和表征, 结果表明, 600 ℃焙烧得到的SiO2-Al2O3中SiO2以无定型形式存在, 其比表面、孔容与表面酸性随SiO2含量的增加而提高, 孔径、堆密度随SiO2含量的提高而减小, 压碎强度基本保持不变.     

超声提取-超高效液相串联质谱分析沉积物中15种抗生素

在现有方法基础上对沉积物中磺胺类、喹诺酮类、大环内脂类和四环素类抗生素的提取、富集、净化以及仪器分析方法进行了优化。以EDTA-Mcllvaine缓冲溶液与乙腈(V:V,1:1)混合液作为提取液,利用超声波细胞破碎仪进行超声提取,串联强阴离子交换柱(SAX)和HLB固相萃取柱进行固相萃取(SPE),通过超高效液相/串联质谱(UPLC-MS/MS)测定沉积物中抗生素的含量。抗生素基质加标回收率在56.4%~110%,相对标准偏差为1.1%~24.3%,方法检出限0.0055~0.716 ng/g。本方法有效地提高了沉积物中抗生素的提取效率,并应用于实际样品的测定中。     

一种含有亚微米孔洞的新型微孔磷酸盐晶体材料的合成及其生长机理

采用水热法成功地合成了一种含有亚微米级孔洞的微孔磷酸盐晶体材料(记为HAP-TAP),其形貌特征是:六棱柱形的晶体表面分布着大量0.4～0.8μm的亚微米级孔洞,孔洞内长有片层状晶体.在样品晶化的过程中,通过控制合成时间,获得了纯六棱柱形晶体的大单晶(记为HAP).使用扫描电子显微镜(SEM)、粉末X射线衍射(XRD)、红外光谱和电子能谱(EDX)对HAP-TAP独特形貌的形成机理进行了研究和揭示.HAP的单晶XRD数据表明,HAP是一种具有二维空旷骨架结构的新型微孔磷酸铝晶体,其分子式为Al5(OH)2(PO4)7(C2N2H10)3.0.5H2O.EDX分析结果表明,生长于六棱柱形晶体孔洞内的片层状晶体为磷酸钛铝材料.     

N-环丙甲基-7α-[(R)-1-羟基-1-甲基-3-(2-噻吩)丙基]-6,14-内乙基桥四氢去甲基蒂巴因(噻诺啡)合成和晶体结构

N-环丙甲基-7α-[(R)-1-羟基-1-甲基-3-(2-噻吩)丙基]-6,14-内乙基桥四氢去甲基蒂巴因(噻诺啡)是阿片受体部分激动剂.噻诺啡经过一步法合成其结构通过单晶X射线衍射分析确证,其结构保持吗啡"T"型主体结构.     

锐钛矿型纳米TiO2介孔粉体表面织构的研究

以硫酸钛和尿素为原料,聚乙二醇-1000为空间构造剂,104℃下经尿素水解均匀沉淀法研制颗粒分散均匀、粒径可控的高热稳定性锐钛矿型纳米TiO2介孔粉体,并对其晶相、颗粒大小、比表面积、形貌和孔道结构进行了表征.结果表明,未经任何热处理的TiO2粉体即为锐钛型晶相,颗粒为均匀分散的类球型颗粒,且颗粒间形成直通型的介孔孔道,其孔径在10～30nm之间.控制焙烧温度可以达到控制颗粒大小及形貌的目的,经850℃焙烧5h的样品仍保持锐钛矿型晶相,未出现向金红石型晶相转变的迹象.     

CuZnAl水滑石衍生催化剂上甲醇水蒸气重整制氢Ⅲ.合成水滑石用金属盐的影响

采用共沉淀法,用不同金属盐为Cu源和Zn源合成了一系列CuZnAl水滑石,以此为前体经600℃焙烧后制得相应催化剂.用硝酸盐和醋酸盐合成的水滑石结晶度高,其衍生催化剂比表面积大、Cu的分散性好且易于还原;而用硫酸盐和盐酸盐合成的水滑石结晶度差,其衍生催化剂比表面积小、Cu的分散性差且不易还原.反应评价结果显示,用硝酸盐和醋酸盐制得的催化剂活性高、反应稳定性好;而用硫酸盐和盐酸盐制得的催化剂由于低的Cu表面积以及S和Cl的毒化作用而几乎无催化活性.在醋酸盐制备的催化剂上,产物干气中CO的浓度明显较低,在250℃和WHSV=3.28 h-1的条件下约为0.03%~0.04%,仅为硝酸盐所制催化剂上CO浓度的1/5;在210℃和WHSV=0.5 h-1的条件下,该催化剂上甲醇几乎完全转化,同时CO浓度降至约0.005%.N2O滴定、CO2程序升温脱附和程序升温还原结果显示,用醋酸盐和硝酸盐制备的催化剂具有极相近的Cu表面积和表面碱性,但前者CuO的还原峰温较后者低近70℃,归因于ZnO与CuO间的强相互作用,这是催化剂具有良好选择性的可能原因.     

6′,6″-二吡啶基-2,2′:4′,4″:2″,2′″-四联吡啶稀土配合物的合成、表征及荧光性质研究(英文)

0 IntroductionMetallosupramolecular oligomers and polymerscan result from the interaction of metal ions with ap-propriate multidentate ligands designed for multinucle-ar binding[1,2], and there are considerable interests in thedesign of species containing known numbers of metalions in defined spatial arrangements. The electronic andphotophysical properties of oligopyridine complexes oftransition-metal ions make their incorporation particu-larlyattractive and the possibilityofinter-metallic ele…