高性能T型沸石膜的合成及水热/耐酸性能

考察了晶种尺寸形貌及晶化温度对T型沸石膜的形成演化过程以及分离性能的影响,调查表明采用小尺寸的晶种可制备出致密的沸石膜,且膜的生长速率受晶化温度影响,低温下合成同性能的膜需更长的晶化时间。当晶种尺寸分别为0.4和0.6μm时,423 K晶化4 h可制得高性能的T型沸石膜,348 K分离90%(w/w)异丙醇/水混合物体系,其通量分别高达6.21和5.98 kg·m~(-2)·h~(-1),分离因子均10 000。实验发现,膜的形成过程受外延生长机理控制,与晶种形貌尺寸和晶化温度无关,且所制得的高性能T型沸石膜具有很好的水热稳定性及耐酸性。     

刚性配体3-噻吩-5-三氟甲基-2,3-二氢-1-H吡唑合成的2个Keggin型超分子化合物

选用新颖的有机配体3-噻吩-5-三氟甲基-2,3-二氢-1-H吡唑（L）,在水热条件下成功得到2个新的基于Keggin多酸的超分子化合物,{[Ag（L）_2]_3[PMo_（12）O_（40）]}·3H_2O（1）和{[Ag（L）_2]_3[HSiMo_（12）O_（40）]}·3H_2O（2）.通过红外光谱、元素分析和单晶X-射线对化合物1和2的结构进行了表征.化合物1和2同构,包含1个孤立的Keggin多阴离子和3个金属-有机亚单元[Ag（L）2]＋.其中多酸阴离子和[Ag（L）2]＋片段通过氢键作用力交替连接形成1个一维超分子链.相邻一维链进一步通过氢键连接成二维超分子层状结构.光催化和电化学性质表明,化合物1和2具有相同的电化学性能.     

高性能多级花状Co3O4基无酶葡萄糖电化学传感器

以硝酸钴、碳酸钠、尿素为原料,泡沫镍为基体,采用水热和煅烧相结合的二步法制备了一种多级花状Co_3O_4/Ni异质结构的无酶葡萄糖传感器。通过X射线衍射与扫描电镜对Co_3O_4/Ni电极的成分及形貌进行了表征,并采用循环伏安法在1mol/L KOH溶液中测试了Co_3O_4/Ni异质结构葡萄糖传感器电极的电化学性能。结果表明,通过二步法在泡沫镍表面制备的Co_3O_4呈现多级花状纳米纤维结构。将制备的Co_3O_4/Ni异质结构作为电极构建的无酶葡萄糖传感器表现出响应时间快(低于5s)、检测灵敏度高(7.4m A·(mmol/L)~(-1)·cm~(-2))、检出限低(1.17μmol/L,S/N=3)和线性检测范围宽(0~5 mmol/L)的特点。进一步的抗干扰性检测表明所制备的传感器在+0.44V vs.SCE对葡萄糖表现出良好的选择性。本文所制备的多级花状Co_3O_4基电极在无酶葡萄糖传感器的发展中有着很大的应用潜力。     

Cu/SAPO-34催化剂的NH_3-SCO活性及抗水热性能研究

采用浸渍法制备了一系列不同铜含量的Cu/SAPO-34催化剂,考察了该系列催化剂上NH_3选择性催化氧化反应性能(NH_3-SCO)。实验结果表明,10%-Cu/SAPO-34催化剂在300℃温度下具有100%的NH_3去除率,且其氮气选择性大于90%。与此同时,通过XRD、BET、UV-vis、H_2-TPR和XPS等表征分析结果表明,高度分散的CuO是Cu/SAPO-34催化剂的主要活性组分。对10%-Cu/SAPO-34催化剂进行水热处理后,催化剂低温活性明显提高,催化剂的N_2选择性在325℃急剧下降。这是由于水热处理导致一定数量的铜物种发生迁移并且形成了更稳定的铜物种引起。SAPO-34的骨架结构遭到一定程度的破坏。     

Green synthesis of hydrotalcite from untreated magnesium oxide and aluminum hydroxide

The influence of reaction temperature and time on the hydrothermal dissolution-precipitation synthesis of hydrotalcite was investigated. Untreated MgO, Al(OH)₃ and NaHCO₃ were used. An industrially beneficial, economically favourable, environmentally friendly, zero effluent synthesis procedure was devised based on green chemistry principles, in which the salt-rich effluent typically produced was eliminated by regenerating the sodium bicarbonate in a full recycle process. It was found that the formation of hydromagnesite dominates at low temperatures independent of reaction time. With an increase in reaction time and temperature, hydromagnesite decomposes to form magnesite. At low temperatures, the formation of hydrotalcite is limited by the solubility of the Al(OH)₃. To achieve a hydrotalcite yield of 96%, a reaction temperature of 160°C for 5?h is required. A yield higher than 99% was achieved at 180°C and 5?h reaction time, producing an layered double hydroxide with high crystallinity and homogeneity.     

水热污泥与煤在混燃过程中的协同效应特性研究

以城市污泥衍生的水热污泥(SS-derived hydrochar)为对象,结合傅里叶红外光谱分析(FT-IR)、X射线荧光光谱分析(XRF)和X射线衍射分析(XRD)等对比研究了水热污泥与三种不同品阶煤(褐煤、烟煤和无烟煤)在有机/无机结构与燃料特性上的异同;同时,通过热重(TG)与偏差分析(Deviation)考察水热污泥与各阶煤在不同混合比例条件下的协同燃烧行为及其作用机制。结果表明,污泥经过水热处理后其有机结构和燃烧行为均提升至与煤相似的水平,该过程不仅改善污泥的燃烧特性,并增强其与煤之间的协同燃烧效应。水热污泥中适量的轻质组分与(碱)碱土金属能在混合燃烧过程中加速煤的失重速率,其对三种煤的促进作用可达4.4%-16.1%(褐煤)、1.9%-9.4%(烟煤)和4.8%-12.1%(无烟煤)。总体而言,水热污泥与褐煤混合而成的燃料在燃料性能上具有较大的优势,并且其混合比例以30%(水热污泥):70%(褐煤)与50%(水热污泥):50%(褐煤)为宜。     

Hydrothermal Synthesis and Structure of a Novel Molybdenum Phosphate: Na_4(H_3O) [Na(HPO_4)_2(PO_4)_4Mo_(18)O_(49)]·16H_2O

1 INTRODUCTION The design synthesis of metal oxide heterpoly compounds have been the subject due to their diverse structures and potential applications in catalysis, sorption, electrical conductivity, ion exchange and anti-virus[1]. Molybdenum phosphates with microporous framework serve as a new kind of inorganic microporous materials. In the course of our investigation on the synthesis of Molybdenum phosphates, we have hydrothermally synthesized an organically templated solid material[…     

空心微球表面定向生长TiO2纳米棒及其光催化性能研究

通过表面溶胶-凝胶处理和水热反应成功制备出包覆有二氧化钛纳米棒的复合空心微球. 用扫描电子显微镜(SEM)和X射线衍射仪(XRD)等表征了所得产品, 探索了水热反应时间、煅烧时间对产物形貌和结构的调控作用, 并对产物光催化降解亚甲基蓝进行了研究. 结果表明, 所制备的表面包覆有二氧化钛纳米棒的复合空心微球在紫外光照射下可将亚甲基蓝完全降解. 该材料质轻, 可浮于水面, 有望成为一种新型光催化剂, 应用于治理水体表面的大面积污染.     

Hydrothermal Synthesis, Crystal Structure and Thermal Stability of [Ni(phen)3]·(C8H12O4)·(H2O)14

One novel complex [Ni(phen)3]·(C8H12O4)·(H2O)14 with hexane dicarboxylic acid and 1,10-phenanthroline has been hydrothermally synthesized and characterized. Crystal data: monoclinic, space group C2/c, a = 2.3475(5), b = 1.2208(2), c = 1.9499(4) nm, β = 114.682(3)o, V = 5.0778(16) nm3, Dc = 1.339 g/cm3, Z = 4, μ(MoKα) = 0.458 mm-1, F(000) = 2168, GOOF = 1.014, R = 0.0401 and wR = 0.0961. The nickel(Ⅱ) center in the title complex is coordinated with six nitrogen atoms of three 1,10-phenanthroline molecules, giving a distorted octahedral coordination geometry. However, the nickel(Ⅱ) ion does not coordinate to the hexane dicarboxylic acid. The complex molecules form a 3D structure through hydrogen bonds. TG analysis shows that the title complex is stable below 240.0 ℃.