Pd/γ-Al2O3复合膜的制备工艺研究

本文研究了采用Sol-Gel法制备用于H     

CaO/γ-Al2O3吸附剂吸附CO2的性能研究

采用浸渍法制备了以γ-Al2O3为载体的CaO/γ-Al2O3吸附剂,并在自制吸附剂评价装置上,研究了不同CaO负载量对CaO/γ-Al2O3吸附剂吸附性能的影响。利用XRD及BET对CaO/γ-Al2O3吸附剂的物相及结构进行了表征。实验结果表明,CaO/γ-Al2O3吸附剂对CO2有较好的吸附性能,并且CaO/γ-Al2O3吸附剂的比表面积、孔容随着CaO负载量的增大而减小。当CaO的负载量为25%(wt,下同)时,CaO/γ-Al2O3吸附剂的静吸附容量达到最大值,4.95mol/kg。     

Synthesis and structure characterization of Ru nanoparticles stabilized by PVP or γ-Al2O3

Uniform and stable Ru nanoparticles were synthesized by reduction of RuCl₃ in ethylene glycol (EG) in the presence of poly(N-vinyl-2-pyrrolidone) by using microwave-assisted solvothermal method. The obtained materials were characterized by UV-vis, FT-IR, XPS, XRD and TEM techniques, and used as precursors of heterogeneous metal colloid catalysts. Characterization by TEM showed that as-prepared PVP-stabilized Ru nanoparticles have small average diameters (below 2 nm) and narrow size distributions (1-3 nm). Diffraction data confirmed that a crystallite size is around 2.0 nm. A colloidal Ru/γ-Al₂O₃ catalyst was obtained by two different methods: immobilization of the PVP-stabilized Ru colloid on the support or by in situ deposition of Ru colloid, e.g., reduction of RuCl₃ with EG in the presence of the γ-alumina. It was found that both synthesis methods produced the Ru/γ-Al₂O₃ catalysts with narrow size distributions of metallic nanoparticles, that are distributed uniformly over the support. However, only in situ preparation of the colloidal Ru/γ-Al₂O₃ catalyst results in chlorine free system with high activity for hydrogen chemisorption. The H₂ uptake on the Ru(PVP)/γ-Al₂O₃ catalyst was very low because the ruthenium surface was strongly occluded with a thin layer of polymer molecules.     

γ-Al2O3多孔膜的制备与性能研究

以无机盐AlCl3·6H2O为初始原料,采用溶胶-凝胶法通过调节pH值控制溶胶体系的稳定性制备出具有耐高温、耐腐蚀性的γ-Al2O3微孔膜,利用差热、BET和SEM对薄膜的组成、结构和表面形貌进行了分析表征.并对溶胶制备过程中的主要影响因素以及膜制备过程中膜性能的各种影响因素进行了深入探讨.     

微波水热合成γ-AlOOH和γ-Al2O3纳米片

以九水合硝酸铝和尿素为原料,聚乙烯吡咯烷酮为表面活性剂,在180℃微波水热条件下反应30min,制备了γ-AlOOH片状结构产物。此前驱物经600℃热分解2h,得到γ-Al2O3纳米片。采用SEM、TEM、SAED和XRD等方法对样品进行表征,并测试了γ-Al2O3纳米片对刚果红染料的吸附性能。实验结果表明,采用微波水热法可以得到长度约为1μm,厚度为30nm的γ-AlOOH纳米片,该产物经煅烧处理后可以得到微观形貌保持不变的γ-Al2O3纳米片,且片状结构表面存在介孔结构。γ-Al2O3纳米片状结构表现出对废水中刚果红污染物的强吸附性能。     

MgAl2O4-γ-Al2O3 solid solution interaction: mathematical framework and phase separation of α-Al2O3 at high temperature

Although existence of MgAl₂O₄-γ-Al₂O₃ solid solution has been reported in the past, the detailed interactions have not been explored completely. For the first time, we report here a mathematical framework for the detailed solid solution interactions of γ-Al₂O₃ in MgAl₂O₄ (spinel). To investigate the solid solubility of γ-Al₂O₃ in MgAl₂O₄, Mg-Al spinel (MgO-nAl₂O₃; n = 1, 1.5, 3, 4.5 and an arbitrary high value 30) precursors have been heat treated at 1000°C. Presence of only non-stoichiometric MgAl₂O₄ phase up to n = 4.5 at 1000°C indicates that alumina (as γ-Al₂O₃) present beyond stoichiometry gets completely accommodated in MgAl₂O₄ in the form of solid solution. γ → α alumina phase transformation and its subsequent separation from MgAl₂O₄ has been observed in the Mg-Al spinel powders (n > 1) when the 1000°C heat treated materials are calcined at 1200°C. In the mathematical framework, unit cell of MgAl₂O₄ (Mg₈Al₁₆O₃₂) has been considered for the solid solution interactions (substitution of Mg²⁺ ions by Al³⁺ ions) with γ-Al₂O₃. It is suggested that combination of unit cells of MgAl₂O₄ takes part in the interactions when n > 5 (MgO-nAl₂O₃).     

室温离子液体辅助制备中孔γ-Al2O3

液相反应条件下,以薄姆石溶胶为铝源,室温离子液体1-甲基-3-丁基咪唑四氟硼酸盐([BMIM][BF4])存在下制备了晶态结构中孔γ-Al2O3.采用N2物理吸附,X射线衍射,透射电子显微镜,27Al魔角固体核磁共振对所制备的样品进行了结构表征.结果表明:通过调节[BMIM][BF4]的用量,得到了孔道结构呈脚手架状、比表面积较大、平均孔径在12nm左右、孔容在1.0cm3/g以上,孔径分布较宽的介孔氧化铝;[BMIM][BF4]加入能够明显改善氧化铝的孔道结构.     

La2O3/γ-Al2O3复合产物的浸渍-燃烧法制备及表征

采用浸渍-燃烧法制备了La2O3/γ-Al2O3复合产物,原料为La(NO3)3.6H2O(A.R)、一水合柠檬酸和工业级的拟薄水铝石.以六水合硝酸镧和一水合柠檬酸分别为镧源和燃烧剂,柠檬酸与六水硝酸镧的摩尔比为5∶6左右.将拟薄水铝石研磨成粉末并溶于柠檬酸和镧的配合物溶液中,搅拌至凝胶状,110℃干燥2h,再放入马弗炉中焙烧2 h得到产物.采用XRD、BET、XPS进行分析和表征,结果表明La3+的加入提高了γ-Al2O3的热稳定性,随着样品焙烧温度升高,比表面积下降,孔容、孔径变大.随着La3+的量的增加,样品的比表面积增大,孔径尺寸分布变宽.通过控制La3+加入的量以及焙烧温度,可调控多孔γ-Al2O3粉体的比表面积、孔容、孔径大小及孔径分布.     

TiO2/γ-Al2O3复相脱硝催化剂载体的制备研究

以二氧化钛、氧化铝和高岭土为主要原料,加入适量的添加剂,通过柱塞式挤压成型设备制得大型蜂窝陶瓷。实验结果表明,2号样品即TiO2和Al2O3的质量分数比为0.27时综合性能最佳,浸渍催化剂后催化活性最高到98.08%。另外,实验还确定了多种干燥方式结合的干燥制度以及最佳烧成制度,样品经850℃煅烧后,BJH脱附平均孔径为51.3nm,BET比表面积为53m2/g,BJH脱附累积孔容为0.14cm3/g,该吸脱附等温线属于Ⅳ型等温线,是介孔物质的吸附类型。     

K2CO3/γ-Al2O3催化玉米油制备生物柴油成分的定性分析

采用等体积浸渍法制备了负载型固体碱催化剂K2CO3/γ-Al2O3,并将其用于催化玉米油与甲醇酯交换反应制备生物柴油。采用气相色谱质谱联用仪对其成分进行了定性分析。通过分析质谱图的分子离子峰和特征离子峰,确定所制备的生物柴油主要由四种脂肪酸甲酯组成,分别为棕榈酸甲酯、亚油酸甲酯、油酸甲酯和硬脂酸甲酯。     

负载型Fe2O3/γ-Al2O3催化剂的制备及其对煤微波热解的催化活性

为实现低变质煤资源化的目标,在低变质煤微波热解的基础上采用超声浸渍-焙烧法制备负载型Fe2O3/γ-Al2O3催化剂,采用场发射扫描电镜(SEM)及X射线能谱(EDS)对催化剂进行表征,研究了其对煤微波热解过程中的催化效果及机理,考察焙烧时间、焙烧温度等因素对催化剂催化活性的影响,通过气-质联用(GC-MS)及煤气分析仪对焦油及气体组分和含量进行测定。结果表明,Fe2O3/γ-Al2O3催化剂的加入提高了煤微波热解制氢气及焦油产率,超声浸渍条件下400℃焙烧4h制备的产品催化活性最佳。     

Low-temperature mechanochemical–thermal synthesis of α-Al2O3 nanocrystals

The great capability of high-energy ball milled basic polyaluminium chloride gel (PACl) which consisted of the monomeric Al³⁺ ions and polymerized Al³⁺ species such as [Al₁₃O₄(OH)₂₄(H₂O)₁₂]⁷⁺ with a Keggin like structure to enhance the phase transformation into α-Al₂O₃ nanocrystals at low temperature was verified. PACl gel 10 min milled and annealed at 400 °C, partially transformed to nanocrystalline α-Al₂O₃ with the mean XRD crystallite size in the range of 15–17 nm, embedded in an amorphous or transition alumina matrix. Further crystal growth up to ∼50 nm and phase pure α-Al₂O₃ powder was obtained when heat-treated at 1000 °C. In contrast to this, the non-milled PACl gel transforms to the transition θ-Al₂O₃ phase at 1000 °C. The evolution of α-Al₂O₃ nanocrystals was studied by XRD, TEM, selected area electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM) methods.     

Fabrication of Al-Zn/α-Al2O3 nanocomposite by mechanical alloying

In this study fabrication and characterization of alumina particles reinforced aluminum-based metal matrix nanocomposite by mechanical alloying were investigated. Aluminum and zinc oxide powders mixture milled by a planetary ball mill in order to produce Al-13.8 wt.% Zn/5 vol.% Al₂O₃ nanocomposite. The structural evaluation milled and annealed powders studied by X-ray diffraction, SEM observation and hardness measurement. The aluminum crystallite size estimated with broadening of XRD peaks by Williamson-Hall formula. The results showed that milling of aluminum and zinc oxide for 60 h led to displacement reaction of the zinc oxide and aluminum to produce Zn and Al₂O₃ phases. The milled powder had a microstructure consisting of nanosized Al₂O₃ particles in an Al-Zn solid solution with a nanoscale grain size of 40 nm. Microhardness of this nanocomposite was found to be about 190 HV.     

Bimodal mesoporous γ-Al2O3: A promising support for CoMo-based catalyst in hydrodesulfurization of 4,6-DMDBT

Bimodal mesoporous γ-Al₂O₃ (BMA) synthesized by a simple hydrothermal route was applied as support for CoMo-based catalyst. The materials were characterized and evaluated for hydrodesulfurization of 4,6-Dimethyldibenzothiophene (4,6-DMDBT) in a fixed-bed reactor. BMA displayed simultaneously high surface area, large porosity and particular hierarchically mesoporous structure after calcination at 550 °C. By taking advantage of these properties, CoMo-BMA catalyst bearing high active species dispersion, good reducibility and enhanced diffusibility was used in this work to compare with commercial γ-Al₂O₃ supported catalyst. The obtained results showed that BMA had a good potential as support for hydrodesulfurization catalysts.     

Synthesis of nanostructured palladium films on porous α-Al2O3 substrates

The lamellar lyotropic liquid crystalline phases of Brij56 nonionic surfactants were used to template the deposition of nanostructured palladium films on α-Al₂O₃ substrates. The reaction between hydrazine hydrate and Pd²⁺ dissolved within the aqueous domains of the liquid crystalline phase generated the nanostructured palladium. The X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission election microscopy (TEM) studies indicated that the resulting films possessed regular arrays of channels with periodicity of 1 nm, which was obviously smaller than that of the templates. The size mismatch might arise from the discharge of nitrogen during the reaction and the relatively low Pd²⁺ concentrations.     

Meso-macroporous monolithic CuO–CeO2/γ-Al2O3 catalysts and their catalytic performance for preferential oxidation of CO

Meso-macroporous monolithic CuO–CeO₂/γ-Al₂O₃ catalysts were prepared and tested for preferential oxidation of carbon monoxide in hydrogen-rich gases. The catalysts were characterized with photographs, SEM, N₂ adsorption–desorption, XRD, HRTEM, and TPR techniques. CuO–CeO₂ catalysts were evenly coated onto the walls of γ-Al₂O₃ monolith macropores with ceria and copper oxide highly dispersed. The prepared meso-macroporous monolithic CuO–CeO₂/γ-Al₂O₃ catalysts can remove CO from H₂-rich gases to ppm level at high space velocity, indicating that they are a kind of promising structured catalyst.     

二步煅烧法制备超细α-Al2O3粉

经由二步煅烧法制备了超细     

原位诱导结晶低温制备α-Al2O3纳米粉体

为了研究在较低的温度下制备α-Al2O3纳米粉体工艺路线,以Al(NO3)3.9H2O和NH3.H2O溶液为原料,经改进的沉淀反应和原位诱导结晶,制备了分散性能良好的α-Al2O3纳米粉体.用XRD、TEM等技术研究了产物的物相、组成和形貌.结果表明,改进的沉淀反应和原位诱导结晶相结合,可有效的降低煅烧温度.在900℃煅烧2 h,即可得到尺寸分布均匀,结晶性好,分散性能良好的α-Al2O3纳米粉体.NH4NO3的存在对于α相变具有明显的促进作用.     

纳米-Al2O3/SiO2加入量对MgO-Al2O3-SiO2复相陶瓷烧结机理的影响

为了探究纳米-Al₂O₃/SiO₂加入量对MgO-Al₂O₃-SiO₂复相陶瓷烧结行为的作用机理。以微米级MgO、纳米级Al₂O₃和SiO₂为主要原料制备陶瓷基复合材料。通过XRD和 SEM等检测手段对烧后试样的物相组成和微观结构进行测试与表征,重点研究Al₂O₃/SiO₂的加入对复相陶瓷物相组成、微观结构及烧结性能的影响。结果表明:随着Al₂O₃/SiO₂加入量的增大,试样烧后相对密度和烧后线变化率呈先增大后减小再增大的趋势,加入15%Al₂O₃/SiO₂(质量分数)的试样经1 500 ℃烧结后,其相对密度可以达到94%。引入的Al₂O₃/SiO₂与基体中的MgO生成镁铝尖晶石与镁橄榄石相,原位反应伴随的体积膨胀,抵消部分烧结过程中的体积收缩。Al₂O₃/SiO₂加入量为75%(质量分数)的试样经1 400 ℃烧结后,基体中有大量堇青石相生成,随着煅烧温度提高到1 500 ℃,堇青石分解所产生的高温液相促进了试样的烧结收缩。     

Microstructures formed during devitrification of Na2O·Al2O3·B2O3·SiO2·Fe2O3 glasses

Soda alumina borosilicate glasses of composition (24-y)Na₂O·yAl₂O₃·14B₂O₃·37SiO₂·25Fe₂O₃, y = 8, 12, 14, 16 mol%, were melted using Fe₂O₃ as raw material. Besides, samples with y = 12 and Fe₂O₃ concentrations of 14.32, 17.8, and 25.0 mol% were prepared from FeC₂O₄·2H₂O as raw material. The X-ray diffraction analyses showed the presence of magnetite for the samples from all the investigated compositions. Transmission electron microscopy (TEM) evidenced that all the samples are phase separated and droplets in the diameter range 100–1000 nm, enriched in iron, are formed. Inside these droplets, numerous small magnetite particles, with size in the 25–40 nm interval, are crystallized.