Synthesis and characterization of mesoporous Mn-MCM-41 materials

MCM-41 has been synthesized at two different pH using cetyl-trimethylammonium bromide (CTAB) surfactant as template and adding the silica precursor to aqueous solutions containing CTAB. The obtained solids were calcined at 600 °C for 4 h. Mn-MCM-41 powders with different Mn/Si molar ratios were prepared using the incipient wetness method, followed by calcination at 550 °C for 5 h. At the end of the impregnation process the powders colour changed from white to brown whose intensity depends on manganese quantity. The materials characterization was performed by X-ray diffraction, N₂ adsorption, ²⁹Si Cross Polarization-Magic Angle Spinning NMR, and X-ray Photoelectron Spectroscopy. The effects of the manganese quantity and of the structural characteristic of the MCM-41 support were studied. The catalytic activity of the prepared systems was evaluated in a complete n-hexane oxidation.     

Separation of precious metals using selective mesoporous adsorbents

The mesoporous NH₂-MCM-41 adsorbent prepared by grafting aminopropyls on MCM-41 is selective towards gold and palladium adsorptions and can separate these precious metals from complex solutions containing other metal ions such as cobalt, nickel, copper and zinc. Adsorption is rapid and the adsorbent’s capacity for gold is better or comparable to most carbonaceous adsorbents including activated carbons. Furthermore, NH₂-MCM-41 can separate palladium from gold solution at pH1.0 with excellent selectivity and capacity. Thus, it is possible to design a two steps separation process for the separation of palladium and then gold from the complex solution. A simple acid wash was sufficient to recover the adsorbed palladium and gold as concentrated, high purity (i.e., > 95%) metal salt solutions and the regenerated adsorbent was reused without lost of performance.     

Gel electrolytes containing several kinds of particles used in quasi-solid-state dye-sensitized solar cells

Composite gel electrolytes containing several kinds of particles used as the quasi-solid-state electrolytes in dye-sensitized solar cells (DSSCs) were reported. Mesoporous particles (MCM-41) with unique structures composed of ordered nanochannels were served as a new kind of gelator for quasi-solid-state electrolytes. MCM-41, hydrophobic fumed silica Aerosil R972 and TiO2 nanopatricles P25 were dispersed into gel electrolytes respectively. The solar energy-to-electricity conversion efficiency of these cells is 4.65%, 6.85% and 5.05% respectively under 30 mW·cm-2 illumination. The preparation methods and the particles sizes exert an influence on the performance of corresponding solar cells. Owing to unique pore structures and high specific BET surface area, mesoporous silica MCM-41 was expected to have the potential to afford conducting nanochannels for redox couple diffusion.     

Ti-（纳米MCM-41）复合材料的制备与表征

采用水热合成法，溴化十六烷基三甲基铵为模板剂，正硅酸四乙酯为硅源，制备出纳米MCM-41分子筛。以钛酸四丁酯为钛源用液相移植法浸渍煅烧后的纳米MCM-41分子筛，制得了Ti-（纳米MCM-41）复合材料。采用粉末XRD，化学分析，N2吸附-解吸附技术，IR，评价了制备方法的有效性及对纳米MCM-41分子筛孔结构的影响。结果表明：钛已并入MCM-41分子筛中，MCM-41内表面上的硅羟基团是钛并入的主要位置，部分钛在分子筛孔道内。制得的材料Ti-（纳米MCM-41）保持高度有序的介孔一维结构。Ti-（纳米MCM-41）样品的紫外．可见扩散漫反射吸收光谱相对于体相TiO2发生明显蓝移，这是由于TiO2粒子组装在纳米分子筛MCM-41孔道内的结果。     

模板法-脱合金制备低密度、分级多孔金及其电催化性能

本文提出了以模板法-脱合金复合方法制备低密度分级多孔金。在该方法中,以直径为700 nm的二氧化（SiO2）微球作为模板,通过化学镀的方法依次制备了Ag@SiO2和Au@ Ag@ SiO2核壳粒子,并通过冷压-烧结方法制备了Au@ Ag@ SiO2合金块材。通过连续改变腐蚀溶液,SiO2模板以及Ag元素从Au@ Ag@ SiO2合金中完全去除。将SiO2从Au@ Ag@ SiO2微球完全去除从而得到了大尺寸空心球壳（直径约为675 nm）,将Ag元素脱合金去除从而在球壳表面形成了许多小尺寸的孔结构（直径约为75nm）。TEM图像表明,块状金样品中的韧带由具有多晶特性的纳米晶粒组成。这种具有低密度1.1 g/cm3（相对密度为5.7%）和高表面积4.24 m2/g的分级纳米多孔金材料在碱性溶液中对甲醇电氧化具有优良的催化活性以及快速的传质速率,表明其在催化领域具有广阔的应用前景。     

介孔SiO2负载和包覆的纳米金属颗粒的制备与研究

制备了以SiO2为核、介孔SiO2为壳的核一壳颗粒负载纳米金属颗粒以及介孔SiO2壳层包覆SiO2负载的纳米金属颗粒。结果表明,十六烷基三甲基溴化胺（CTAB）作为模板剂,有助于介孔SiO2壳层包覆SiO2核的结构形成,介孔SiO2壳层的孔径方向垂直于SiO2核的表面;在聚乙烯吡咯烷酮（PVP）的稳定作用下,Pt纳米颗粒能均匀地分布在介孔SiO2壳层的表面。单分散SiO2颗粒经过3-氨丙基三乙氧基硅烷（APS）功能化后,可负载纳米金属颗粒。进一步研究表明,以SiO2负载纳米金属颗粒为核,NH3·H2O,乙醇和水为分散剂,CTAB为模板剂,正硅酸乙酯（TEOS）为硅源,还能制备介孔SiO2壳包覆SiO2负载的纳米金属颗粒,而且介孔SiO：壳层的厚度可通过TEOS的含量调节。     

Au/Co_3O_4的制备、表征及加氢催化性能研究

采用化学浸渍法制备出Au/Co_3O_4纳米复合材料,用透射电子显微镜(TEM)、X射线能谱(EDS)和X射线粉末衍射(XRD)等对其结构和组成进行了表征,并考察了其在对硝基苯酚加氢反应中的催化性能。表征结果表明,Au纳米粒子很好地分散在Co_3O_4载体上。催化性能测试表明,Au/Co_3O_4纳米复合材料对于对硝基苯酚加氢反应表现出优异的催化活性,TOF值为5.01 min~(-1);此外,催化剂经过5次循环仍然保持优异的催化性能。     

Influence of the structure of TiO2, CeO2, and CeO2-TiO2 supports on the activity of Ru catalysts in the catalytic wet air oxidation of acetic acid

Ru catalysts, supported on TiO 2 , CeO 2 , and CeO 2 -TiO 2 , were prepared by the impregnation method. The effect of the structure of the supports on the activity of Ru catalysts was investigated in the catalytic wet air oxidation (CWAO) of acetic acid under 230℃ and 5 MPa in a batch reactor. Physical properties including the surface area, crystalline phase, and surface components of the Ru catalysts were characterized by N 2 adsorption, X-ray powder diffraction (XRD), and X-ray photoelectron spectroscopy ...     

酸催化硅溶胶的粘度研究(英文)

采用酸/碱两步催化法制备多孔二氧化硅膜,通过将酸性硅溶胶和碱性硅溶胶按一定比例混合得到所需镀膜溶胶,但其稳定性较差。主要对混合硅溶胶的稳定性进行了研究,较详细讨论了碱性胶/酸性胶摩尔比、酸性胶陈化时间和碱性胶陈化时间对混合溶胶胶凝时间的影响,并对影响凝胶稳定性的原因进行了分析。     

Gold supported on iron oxy-hydroxides: a versatile tool for the synthesis of fine chemicals

A comprehensive overview on gold supported on iron oxy-hydroxides as tool for the synthesis of fine chemicals is given. We will discuss on the catalytic activity of gold supported on iron oxy-hydroxides in several reactions of potential industrial interest, comprising the selective oxidation of primary alcohol to aldehyde, the selective reduction of α,? unsaturated aldehydes and ketones to the corresponding a,b unsaturated alcohols. Furthermore, a significant application of gold supported on iron oxy-hydroxides is the direct synthesis of hydrogen peroxide from H₂ and O₂. The versatility showed by Au supported on oxy-hydroxides catalysts is an aspect of great importance for industrial applications.     

STUDY ON PREPARATION, COMPLEX PERMITTIVITY,PERMEABILITY AND MICROWAVE PROPERTIES OF BaZnZCo2-ZFe16O27／SiO2 MICROCRYSTALLINE GLASS CERAMICS

BaZnzCo2-zFe16O27/SiO2 microcrystalline glass ceramics with Z=0.0, 0.5, 0.8 and 1.1 were prepared at temperature 1200℃ for 5h by citrate sol-gel process. The complex dielectric constant and complex permeability of BaZnzCo2-zFe16 O27/SiO2-paraffin wax composites had been measured. Both the complex dielectric constant and dielectric loss exhibit almost no variation with frequency in 0.1-6.0GHz. The real part of permeability decreases with increasing frequency for all samples, and the imaginary part of permeability exhibits a clear resonance peak at 1.44GHz for Co2 W/SiO2, 1.32GHz for Zn0.5Co1.5 W/SiO2, 1.20GHz for Zn0.8Co1.2W/SiO2, and 1.08GHz for Zn1.1 Co0.9 W/SiO2. It is also showed that the content of zinc has a close effect on the magnetic properties of BaZnzCo2-zFe16O27/SiO2 microcrystalline glass ceramics, the greater the zinc content, the higher the values of imaginary part of permeability and magnetic loss.     

Tungstophosphoric heteropolyacid supported onto neutral alumina： characterization and synthesis of acetals and ketals

Tungstophosphoric acid （HPW） catalyst supported on the neural alumina was studied. It was prepared by means of an equilibrium and incipient wetness impregnation technique. Solution of HPW in 50% V/V ethanol-water was used to impregnate Al2O3 at 25℃. It was found that the catalyst containing 30% PW by calcination at 500℃ showed a higher catalytic activity in the synthesis of acetals and/or ketals. In the following condition, that is, the molar ratio of aldehyde/ketone to glycol being 1：1.5, the mass fraction of the catalyst used was 0.5%, and the reaction time was 1.0 h; the yields of ketals and acetals could reach up to 60.5%-86.7%. Moreover, it could be easily recovered and reused.     

磁性纳米光催化剂的制备及其光催化性能

以Fe3O4为载体,制备了易于固液分离回收的磁性复合纳米光催化剂,采用SEM,元素分析,XRD等方法表征催化剂的表面形貌,晶体结构,结果表明,二氧化钛包裹在Fe3O4的表面,其包裹量越大,粒径越大,锐钛矿峰越强,利用光催化降解甲基橙的效果来考察磁性复合光催化剂的活性,直接包裹在Fe2O4表面的TiO2活性低于纯TiO2的,而在Fe3O4与TiO2之间包裹SiO2,可以有效地提高其光催化活性,其活性与纯TiO2接近。     

Surface structure and catalytic activity of electrodeposited Ni-Fe-Co-Mo alloy electrode by partially leaching Mo and Fe

1 Introduction The chlorine alkaline industry and the production of hydrogen by electrolyzing water have disadvantages of high cost and energy consumption, so it is especially important to study and develop a high catalytic activity and good stability el…     

Preparation and properties of transition metal nitrides caged in N-doped hollow porous carbon sphere for oxygen reduction reaction

A series of transition metal nitrides (M_xN_y, M=Fe, Co, Ni) nanoparticle (NP) composites caged in N-doped hollow porous carbon sphere (NHPCS) were prepared by impregnation and heat treatment methods. These composites combine the high catalytic activity of nitrides and the high-efficiency mass transfer characteristics of NHPCS. The oxygen reduction reaction results indicate that Fe₂N/NHPCS has the synergistic catalytic performance of higher onset potential (0.96 V), higher electron transfer number (~4) and higher limited current density (1.4 times as high as that of commercial Pt/C). In addition, this material is implemented as the air catalyst for zinc-air battery that exhibits considerable specific capacity (795.1 mA·h/g) comparable to that of Pt/C, higher durability and maximum power density (173.1 mW/cm²).     

Novel Coated Pt@SnO2/Al2O3 Catalyst for Propane Dehydrogenation

采用了连续还原超声波震荡负载的方法制备了新型包裹负载型Pt@SnO2/Al2O3催化剂,特殊的包裹结构使其具有较好的抗聚集和耐烧结性能并利用了透射电镜对其结构进行了表征.相比传统浸渍负载型的催化剂来讲,当铂锡的摩尔比为1∶1.5时制备的Pt@SnO2/A12O3催化剂展现出优异的丙烷催化脱氢性能和高温稳定性,这也进一步证实了SnO2壳和Pt核之间强烈的相互作用.     

制备条件对Au/AC催化分解臭氧性能的影响

研究了活性炭负载的金催化剂(Au/AC)对低浓度臭氧的催化分解性能,考察了前驱体溶液pH值、干燥方式、焙烧温度等制备条件对催化剂活性的影响,以及空速对臭氧分解率的影响。结果表明,在金前驱体溶液pH值为10、经微波辐射干燥、200℃氢气还原制备的催化剂,金颗粒在活性炭表面的分布更加均匀,尺寸更小,具有更高的催化活性。在室温、相对湿度45%和空速72000h-1时,对浓度为50mg/m3臭氧的分解率保持在90%以上(在2400min内)。N2吸附-脱附和XPS表征结果表明,活性炭载金催化剂在催化分解臭氧后,比表面积和孔体积略有下降;Au4f的XPS峰虽稍向高能方向移动,但仍保持催化活性;活性炭表面碳含量显著下降而氧含量大幅增加,说明活性炭上负载的Au在自身催化分解臭氧的同时,还起到了促进臭氧与单质碳反应的作用。     

Selective synthesis and characterization of metallic cobalt, cobalt/platinum, and platinum microspheres

Metallic cobalt microspheres have been successfully synthesized via a facile hydrothermal method in the presence of poly (N-vinyl-2-pyrrolidone) (PVP), and the diameters of these spheres are in the range of 1-2 μm. Bimetallic Co/Pt microspheres and hollow noble metal Pt microspheres have also been selectively synthesized by adjusting the amount of reactants of replacement reaction in which corresponding noble metal compound and metallic cobalt microspheres are used as starting materials. The study on catalytic activities of the as-prepared metallic microspheres on hydrolysis of ammonia-borane for hydrogen generation reveals that Co/Pt (molar ratio 5:1) bimetallic microspheres are far more active than the hollow noble metal Pt microspheres.     

New gold catalysts for liquid phase oxidation

A pre-requisite for good catalytic activity with supported gold is that the metal is present as nanoparticles, but no suitable method for depositing gold on carbon as nanoparticles has previously been reported. The deposition precipitation method which has been used successfully for catalyst preparation with other supports, produces large aggregates with carbon. It is now shown, however, that pre-reduced gold sol is a satisfactory method for preparing gold on carbon catalysts as long as an appropriate choice of sol is made. In this paper the activity of gold on carbon catalysts prepared in a number of different ways is compared in a standardized liquid phase organic oxidation reaction. The activity for Au/C catalysts prepared by the sol method can show a two-fold increase compared with a similar catalyst prepared by deposition precipitation.     

Fe-MCM-41 from Coal-Series Kaolin as Catalysts for the Selective Catalytic Reduction of NO with Ammonia

Fe-MCM-41, one kind of high-ordered mesoporous materials catalysts, with molar ratio of Fe/Si = 0.01-0.1, was synthesized by hydrothermal method from coal-series kaolin. Fe-MCM-41 catalysts were characterized by Fourier transform infrared spectroscopy, high resolution transmission electron microscopy, N₂ adsorption-desorption, x-ray photoelectron spectroscopy, and UV-vis spectroscopy. The results clearly indicated that: (1) all the samples exhibited typical hexagonal arrangement of mesoporous structure; (2) the incorporation of tiny amount of Fe³⁺ onto the surface and pore channel of MCM-41 mesoporous materials could efficiently promote the deNO _x activity of these catalysts. Moreover, the Fe-MCM-41 mesoporous materials were evaluated in the selective catalytic reduction of NO with NH₃. The results showed that Fe-MCM-41 catalyst with Fe/Si = 0.05 showed the highest catalytic activity at 350 °C, a gas hourly space velocity of 5000 h^?1, n(NH₃)/n(NO) = 1.1, and O₂% = 2.5%.