均匀沉淀法制备Co(OH)2及其超电容特性

以氯化钴为原料、氨水(28wt%)为沉淀剂采用均匀沉淀法成功地合成了Co(OH)₂。X-射线衍射(XRD)、扫描电镜(SEM)测试表明，表面活性剂Tween-80的加入使所制备的α-Co(OH)₂呈现出类似花朵的形貌;循环伏安、恒电流充放电、交流阻抗和循环寿命等电化学测试表明，该材料的电化学性能也得到一定的提高，其单电极比电容可达到370 F·g^-1。     

水淬渣-累托石颗粒吸附材料的制备及应用

研究了水淬渣-累托石颗粒吸附材料制备工艺条件、再生方法及其去除铜冶炼工业废水中重金属的条件.试验结果表明,累托石与水淬渣的比例为1∶1,另加入10%的添加剂(IS)和50%的水,焙烧温度为400℃时,制成的颗粒吸附材料体积密度为1.06kg/m3,显气孔率为62.29%,吸水率为58.82%,抗压强度为2.22Mpa,吸附效果好,散失率较低.在未调节铜冶炼工业废水pH值的条件下,颗粒吸附材料用量为0.05g/cm3,反应时间为40min,吸附温度为25℃(常温)时,Cu2 、Pb2 、Zn2 、Cd2 、Ni2 的去除率分别为98.2%、96.3%、78.6%、86.2%、64.2%,处理后的水符合国家污水综合排放标准(GB8978-1996)一级标准.颗粒吸附材料对Zn2 、Cu2 有很好的选择性.吸附饱和的颗粒吸附材料用1mol/L氯化钠溶液再生效果好.该颗粒吸附材料具有分离容易、可重复使用、处理效果好、应用前景广阔的优点.     

A convenient synthesis of 2-aryl substituted benzo[f] [1,2,4]triazolo[1,5-a]azepine derivatives

A convenient synthetic pathway to 2-aryl-5,6-dihydro-4H-benzo[f][1,2,4]triazolo[1,5-α]azepine derivatives 7 was developed. The synthesis was based on the cycloaddition of the 1,2,3,4-tetrahydronaphthalene a-acetoxy azo compounds 3 with Ar-CN in the presence of AlCl3 and the consecutive ring enlargement.     

配合物[Mn(phendione)(PDC)(H2O)2]·2H2O的合成与晶体结构

The title compound [Mn(phendione)(PDC)(H₂O)₂]·2H₂O (H₂PDC=pyridine-2，6-dicarboxylic acid) has been prepared in aqueous solution and characterized by single X-ray diffraction structure determination， elemental analysis， IR spectroscopy， and thermal analyses. The compound crystallizes in Monoclinic system， space group C2/c， a=1.017 51(11) nm， b=1.483 25(11) nm， c=1.461 21(13) nm， β=109.86(10)°， V=2.074 1(3) nm³， Z=4， F(000)=1 028， μ=0.701 mm^-1， D_c=1.609 g·cm^-3， R₁=0.028 9， wR₂=0.078 8 [I>2σ(I)]. Crystal structure reveals that complex consists of one-dimensional chain framework bridged by hydrogen bonds that formed by uncoordinated water and oxygen atom of carboxyl group in PDC^2-. Furthermore， the complexes form a three-dimensional super-molecular structure through hydrogen bonds. CCDC: 648570.     

SYNTHESIS, CHARACTERIZATION, METAL-UPTAKE BEHAVIOR OF BIS（BENZIMIDAZOLE） RESIN SUPPORTED ON EPOXIDE POLYMER

The new chelate resins, abbreviated as PNBMZs and PBBMZs based on epoxide polymer, were synthesized by polycondensation of N,N-diglycidyl-4-glycidyloxyaniline or 1,4-bis（2,3-epoxypropyl）benzene with the primary amine group of 1,3-bis（benzimidazol-2yl）propylamine （BBPAH）. The ion exchangers contain 2.71-3.23 mmol of the ligand contents per gram of the resin. Batch extraction capacities were determined for the metal chloride salts in buffer solutions in the pH range from -1 to 6.0. The chelate resins were very selective for Cu^2＋, Zn^2＋, Cd^2＋ in the presence of other divalent transition metal ions. The maximum uptake capacities of PNBMZ （synthetic molar ratio = 1：1.5） under non-competitive condition were found to be 0.94 mmol/g for Cu^2＋ at pH = 2, 1.3 mmol/g for Cd^2＋ at pH = 1 and 1.75 mmol/g for Zn^2＋ at pH = -1 respectively. While in the case of PBBMZ, it was 1.39 mmol/g for Cd〉 at pH = 1. The metal-uptake behaviors for both of them showed strong pH dependence, and their extraction capacities increase with decreasing pH. The uptake of Cu^2＋ by the resin PNBMZs at pH = 1 was found to be rather fast with t1/2 = 18 min. Metal-uptake experiments under competitive conditions also confirm that the chelate resins have a high selectivity for Cu^2＋, Zn^2＋, Cd^2＋ and the contrary pH dependence.     

氟掺杂锐钛矿型TiO2溶胶的制备、表征及催化性能

以四氯化钛为前驱物, 采用改性的沉淀-溶胶-水热晶化法制备了一种具有锐钛矿型结构的氟掺杂的二氧化钛(F-TiO₂)溶胶. 研究了氟掺杂、水热晶化的温度、时间及介质pH值对溶胶粒子的晶型和晶化度的影响. 采用XRD, TG-DTA, TEM, UV-Vis-DRS, FTIR, XPS技术及吸附、表面酸度测定手段对溶胶粒子的结构进行了表征. XRD分析结果表明: 氟的掺入可以降低水热晶化反应的温度或减少反应时间、提高粒子的晶化度, 溶胶粒子具有锐钛矿型结构; TEM分析显示: 粒子呈圆球型, 平均粒径大约为6.5 nm. XPS测定结果表明; 氟在溶胶粒子中以吸附态和结合态两种形式存在; 吸附、表面酸度及光催化活性测定表明: 与P25型TiO₂及纯TiO₂溶胶粒子相比, F-TiO₂溶胶粒子具有更大的吸附能力、更强的表面酸度及更高的光催化活性. 还从光生载流子分离效率等方面探讨了掺杂对催化剂活性影响的机理.     

苯炔与硝酮[3+2]环加成制备二取代苯并异噁唑烷

采用[3 2]1,3-偶极环加成反应,苯炔前体邻-三甲硅基苯酚三氟甲磺酸酯在氟化铯的作用下与硝酮反应合成了9个2,3-二取代苯并[d]异噁唑烷,收率87%～97%。其结构经1H NMR,13C NMR和高分辨率MS确证。     

2,2′-对苯二甲硫基二乙酸配合物的合成及表征

本文报道了配体 2 ,2′-对苯二甲硫基二乙酸和过渡金属铜 ( )、钴 ( )、镍 ( )配合物的合成。经元素分析、X射线衍射分析、红外光谱、差热 -热重分析等推算了它们的组成并指认了谱带的归属。对铜 ( )配合物进行了电子顺磁共振谱研究。     

探究Cu/ZnO相互作用对CO2加氢制甲醇反应性能的影响

Using renewable green hydrogen and carbon dioxide (CO₂) to produce methanol is one of the fundamental ways to reduce CO₂ emissions in the future, and research and development related to catalysts for efficient and stable methanol synthesis is one of the key factors in determining the entire synthesis process. Metal nanoparticles stabilized on a support are frequently employed to catalyze the methanol synthesis reaction. Metal-support interactions (MSIs) in these supported catalysts can play a significant role in catalysis. Tuning the MSI is an effective strategy to modulate the activity, selectivity, and stability of heterogeneous catalysts. Numerous studies have been conducted on this topic; however, a systematic understanding of the role of various strengths of MSI is lacking. Herein, three Cu/ZnO-SiO₂ catalysts with different strengths of MSI, namely, normal precipitation Cu/ZnO-SiO₂ (Nor-CZS), co-precipitation Cu/ZnO-SiO₂ (Co-CZS), and reverse precipitation Cu/ZnO-SiO₂ (Re-CZS), were successfully prepared to determine the role of such interactions in the hydrogenation of CO₂ to methanol. The results of temperature-programmed reduction (H₂-TPR) and X-ray photoelectron spectroscopy (XPS) characterization illustrated that the MSI of the catalysts was considerably affected by the precipitation sequence. Fourier transform infrared reflection spectroscopy (FT-IR) results indicated that the Cu species existed as CuO in all cases and that copper phyllosilicate was absent (except for strong Cu-SiO₂ interaction). Transmission electron microscopy (TEM), X-ray diffraction (XRD), and N₂O chemical titration results revealed that strong interactions between the Cu and Zn species would promote the dispersion of Cu species, thereby leading to a higher CO₂ conversion rate and improved catalytic stability. As expected, the Re-CZS catalyst exhibited the highest activity with 12.4% CO₂ conversion, followed by the Co-CZS catalyst (12.1%), and the Nor-CZS catalyst (9.8%). After the same reaction time, the normalized CO₂ conversion of the three catalysts decreased in the following order: Re-CZS (75%) > Co-CZS (70%) > Nor-CZS (65%). Notably, the methanol selectivity of the Re-CZS catalyst was found to level off after a prolonged period, in contrast to that of Co-CZS and Nor-CZS. Investigation of the structural evolution of the catalyst with time on stream revealed that the high methanol selectivity of the catalyst was caused by the reconstruction of the catalyst, which was induced by the strong MSI between the Cu and Zn species, and the migration of ZnO onto Cu species, which caused an enlargement of the Cu/ZnO interface. This work offers an alternative strategy for the rational and optimized design of efficient catalysts.     

EVA-g-VC的结构和动态粘弹性

本文研究了聚乙烯-醋酸乙烯酯(EVA,VAc:14％)与氯乙烯(VC)接枝共聚物(EVA-g-VC)的相结构和分子结构。接枝物EVA-g-VC由游离EVA、均聚PVC和EVA-VC接枝高分子三者组成,EVA呈连续相,PVC呈分散微粒。EVA-g-VC中EVA的含量越高,PVC粒子体积越小。实验结果表明,接枝物中“凝胶”的EVA玻璃化温度,随投料比(VC/EVA)的减小而升高;另外随VC/EVA减小,凝胶中PVC的含量和PVC的分子量也减小。这些结果说明,VC/EVA较小时得到的接枝物中,EVA上VC接枝点的数目较多,而PVC接枝链的长度较短。EVA-VC是不相容两相——EVA和PVC的“粘着剂”,其作用表现在:VC/EVA越小,接枝物中EVA和PVC的玻璃化温度越靠近。