稀土固体超强酸SO∧2—4／TiO2／La∧3＋的制备及其催化酯化作用

制备了稀土固体超强酸SO∧2-4/TiO2/La∧3 ,研究了以其为催化剂,葵二酸和无水乙醇为原料合成葵二酸二乙酯,并考察了影响反应的因素。结果表明,它是一种良好的酯化催化剂。     

SO_4~(2-)/ZrO_2-Nb_2O_5固体超强酸催化剂的制备与IR表征

引入元素Nb对SO42-/ZrO2进行改进,制备了SO42-促进的Zr-Nb新型二元氧化物固体超强酸催化剂SO42-/ZrO2-Nb2O5。以合成乙酸正丁酯为探针反应,考察了该催化剂的制备工艺,确定了最适宜的制备条件:催化剂中Nb2O5的质量分数为3%,浸渍液硫酸浓度为1.0mol·L-1,焙烧温度为600℃时,酯化率可达到95.3%。采用IR光谱法分析了不同制备条件下催化剂的性能。     

燃烧-比浊法测碳酸钴中SO_4~(2-)含量的研究

硫酸钡比浊法检测碳酸钴中SO_4~(2-)含量,因碳酸钴溶解后是深红色溶液,对比浊产生严重干扰。本文采用管式炉高温通氧燃烧的方式,将碳酸钴中的硫分离出来,用H_2O_2溶液吸收,将SO_2和SO_3转化为硫酸,在HCl介质中,SO_4~(2-)与Ba~(2+)生成硫酸钡,用乙醇做稳定剂,形成悬浮液,用分光光度计进行吸光度测定,对H_2O_2溶液用量和浓度、HCl溶液用量、BaCl_2溶液用量、乙醇溶液用量,BaSO4沉淀稳定时间和分光光度计检测波长等分析条件进行试验,选择最佳条件:H_2O_2溶液1.5 m L,HCl溶液2 m L,BaCl_2溶液2 m L,乙醇溶液5 mL,分光光度计波长380 nm,用SO_4~(2-)标准溶液制作分析曲线,根据分析曲线计算碳酸钴中SO_4~(2-)的含量。此方法简便,分析线性良好,重复测量的标准偏差为0.000 2%,相对标准偏差为9.93%,SO_4~(2-)量回收率为96.70%-104.0%。     

镀铝液中SO_4~(2-)离子浓度测定方法的改进

按传统方法做镀铬液中SO_4~(2-)离子浓度测定时,指示剂颜色变化慢终点指示不明显。针对这一问题,对镀铬液中SO_4~(2-)离子浓度测定做了一些改进使滴定终点易于观察,从而提高了实验精度。     

介孔SO_4~(2-)/W-TiO_2@SiO_2可见光催化剂的制备及催化性能

以P123作为模板剂,采用溶胶-凝胶法合成介孔SO42-/W-TiO2@SiO2(WSTS)可见光响应光催化剂。以甲基橙为模型物,考察其在可见光及紫外光区的光催化活性。采用X射线衍射(XRD)、环境扫描电子显微镜(SEM)、高分辨透射电子显微镜(HRTEM)、X射线光电子能谱(XPS)、低温氮物理吸附(BET)、紫外-可见漫反射光谱(UV-Vis)、傅里叶变换红外光谱(FTIR)、热重分析(TG)和荧光光谱(PL)对样品的结构及性能进行表征。结果表明:W掺杂不但可以提高样品的比表面积、孔容,而且可以抑制晶型从锐钛矿向金红石转变。与光催化剂P25及未掺杂的样品相比,光催化活性明显提高。且W的最佳掺杂量为n(W)/n(Ti)=0.002 5,其在可见光(λ400 nm)和紫外光区辐照40 h和60 min后,甲基橙的脱色率分别是91.7%和98.9%。     

新型Bi_(2)O_(3)/ZnFe_(2)O_(4)光阳极的制备及其光电催化降解有机物性能EI北大核心CSCD

采用化学水浴法制备Bi2O3薄膜,并通过电沉积结合后退火工艺在其表面负载ZnFe2O4进行改性,通过XRD、SEM、Raman、XPS、UV-vis等对Bi2O3样品及Bi2O3/ZnFe2O4复合薄膜进行表征。以制备的薄膜作为光电极,研究其光电化学性能,并首次报道其在光电催化降解有机污染物中的应用。结果表明:ZnFe2O4的复合拓宽Bi2O3的吸光范围,提高光吸收系数,抑制光电化学反应过程中光生载流子的复合,从而使Bi2O3/ZnFe2O4复合薄膜在Na2SO4溶液中的光响应电流密度是纯相材料的4倍左右,AM1.5光照下的光电降解亚甲基蓝性能相比于Bi2O3有明显提高。     

绿色发光材料NaLa(MoO_4)_2:Tb~(3+)的微波辅助溶胶-凝胶法制备及其性质

采用微波辅助溶胶-凝胶法制备了系列绿色发光粉NaLa31-x(MoO4)2:Tb+x(x=0.02,0.1,0.15)。用X射线粉末衍射仪和荧光分光光度计等分析和表征所合成样品的物相结构和发光性质。结果表明:所合成的NaLa(MoO4)2:Tb3+晶体结构与NaLa(MoO4)2相似,属四方晶系结构;样品的激发光谱为位于250~350 nm的1个宽带,最大激发峰位于300 nm处;发射光谱由一系列尖峰组成,最强的发射峰位于544 nm处,归属于Tb3+的5D4-7F5跃迁。NaLa(MoO4)2:Tb3+的发光强度随Tb3+掺杂浓度的增加逐渐加强,当Tb3+浓度为10 mol%时发光强度最大,而后随Tb3+浓度的增加而降低,发生浓度猝灭。根据Dexter能量共振理论,该浓度猝灭系Tb3+的电偶极-电偶极的相互作用所致。通过含氧酸根阴离子(SO2-4)的掺杂有效提高了NaLa(MoO4)2:Tb3+体系的发光亮度。     

固相-水热法制备LiFePO4-Li3V2（PO4）3复合材料及其电化学性能（英文）

分别采用固相-水热法和球磨法制备磷酸亚铁锂-磷酸钒锂复合正极材料(LiFePO4-Li3V2(PO4)3)。电化学性能测试表明,LiFePO4-Li3V2(PO4)3复合正极材料的电化学性能远远高于 LiFePO4和 Li3V2(PO4)3单独作为正极材料的性能,并且以固相-水热法制备的复合材料性能优于以球磨法制得的复合材料。研究发现 LiFePO4-Li3V2(PO4)3复合材料有 4 个氧化还原峰,相当于 LiFePO4 和 Li3V2(PO4)3 氧化还原峰的叠加。采用固相-水热法制备的LiFePO4-Li3V2(PO4)3 复合材料形貌较为规则,且有新相物质产生,这是导致其电化学性能较好的原因。     

重碳酸盐溶液中SO_4~(2-)和Cl~-对低碳钢活化/钝化腐蚀行为的影响

在除O_2的0.1 mol/L NaHCO_3,0.1 mol/L NaHCO_3+0.1 mol/L Na_2SO_4以及0.1 mol/L NaHCO_3+0.1 mol/L NaCl溶液中,用恒电位法在低碳钢电极表面制备腐蚀产物,并原位监测低碳钢的开路电位,用SEM观察腐蚀形貌,用XRD确定腐蚀产物的相组成.结果表明.在0.1 mol/L NaHCO_3溶液中,低碳钢的开路电位最终处于再钝化区间,其表面未观察到明显的腐蚀现象;在0.1 mol/L NaHCO_3+0.1 mol/L Na_2SO4溶液中,低碳钢的开路电位最终处于再活化区间,其表面发生均匀腐蚀;在0.1 mol/L NaHCO_3+0.1 mol/L NaCl溶液中,低碳钢的开路电位最终亦处于再活化区间,而其表面却发生局部腐蚀,XRD结果表明,低碳钢表面的腐蚀产物主要为Fe_3O_4和α-FeOOH.     

La、Ba的添加对Pd/Y2O3-ZrO2催化氧化CH4性能的影响

以浸渍法制备了1.0%Pd/Y2O3-ZrO2催化剂,考察了Pd负载过程中La和Ba的添加对Pd/Y-ZrO2催化氧化CH4性能的影响,用BET、XRD、CO脉冲、TEM和H2-TPR等方法对所制备的催化剂进行表征。结果表明,La和Ba的添加降低了Pd/Y2O3-ZrO2催化剂氧化CH4的活性。催化剂中活性金属的分散度及体相PdO的还原性影响催化剂对CH4的氧化活性,La、Ba的添加降低了Pd/Y2O3-ZrO2催化剂中活性金属Pd的分散性,使Pd在高温老化后更容易团聚,同时增强了PdO与载体的相互作用,使PdO不容易被还原。     

Preparation of SO_4~(2-)/TiO_2-WO_3 solid superacid and its catalytic activity in acetalation and ketaltion

SO42-/TiO2-WO3 was prepared and its catalytic activity under different synthetic conditions was discussed with esterification of n-butanoic acid and n-butyl alcohol as probing reaction. The optimum conditions are found that the mass fraction of H2WO4 used in the compound is 12.5%, the calcination temperature is 580℃, the     

Preparation of SO2-4/TiO2-WO3 solid superacid and its catalytic activity in acetalation and ketalation

SO2-4/TiO2-WO3 was prepared and its catalytic activity under different synthetic conditions was discussed with esterification of n-butanoic acid and n-butyl alcohol as probing reaction. The optimum conditions are found that the mass fraction of H2WO4 used in the compound is 12.5%, the calcination temperature is 580℃, the calcination time is 3 h, and the soaked consistency of H2SO4 is 1.0 mol.L-1. Then SO2-4 /TiO2-WO3 was applied as the catalyst in the catalytic synthesis of eight similar important ketals and acetals under the optimum conditions and revealed high catalytic activity. On condition that the molar ratio of aldehyde/ketone to glycol is 1:1.5, the mass fraction of the catalyst used in the reactants is 0.5%, and the reaction time is 1.0 h, the yields of ketals and acetals can reach 64.2%-95.1%. Moreover, it can be easily recovered and reused.     

掺杂Fe~(3+)与La~(3+)离子的TiO_2薄膜光反应活性的研究(英文)

利用溶胶-凝胶技术在载玻片衬底上制备了透明的TiO2薄膜。为了增强TiO2薄膜的光反应活性,对TiO2薄膜分别进行了不同浓度的Fe3+和La3+离子掺杂。离子掺杂的TiO2薄膜在可见光区有良好的透光性,通过降解罗丹明B染料溶液,评估了掺杂Fe3+和La3+离子的TiO2薄膜的光反应活性。结果表明,当Fe和La的原子分数比为0.5at%时增强了TiO2薄膜的光反应活性。     

Pt-Rh-Pd/CeO2-La2O3/Al2O3催化剂的制备与表征

用共浸渍法制得了Pt-Rh-Pd/CeO2-La2O3/Al2O3催化剂,采用X射线衍射(XRD)对催化剂进行表征,使用配气测试系统对催化剂的活性进行评价。正交试验结果表明,对CO的氧化,选择最佳催化剂的配比为Pt-Rh-Pd 0.1%,CeO2 5%,La2O3 4%,对NO的还原,其最佳配比为Pt-Rh-Pd 0.1%,CeO2 4%,La2O3 4%。稀土氧化物(La2O3、CeO2)作为助剂,能改善Pt-Rh-Pd/CeO2-La2O3/Al2O3催化剂的催化性能,但不能起主要作用。     

Synthesis of Y2O3：Eu^3＋ phosphors by surface diffusion and their photoluminescence properties

Y2O3:Eu3+ phosphors were synthesized by the surface diffusion method (SDM). X-ray diffractometry (XRD), scanning electron microscopy (SEM), and energy dispersive spectrometry (EDS) were used to characterize the structure, morphology and component of Y2O3:Eu3+ phosphors. The photoluminescent (PL) properties were also investigated. The results reveal that the PL intensity of Y2O3:Eu3+ phosphors prepared by the surface diffusion method (SDM) is much higher than that prepared by homogeneous co-precipitation. Th...     

Effect of rare earth Pr on microstructure and mechanical properties of Al2O3-SiO2（sf）/Al-Si composites

The Al₂O₃-SiO₂(sf) (volume fraction, 20%)/Al-12.6Si metal matrix composites(MMCs) with or without rare earth Pr addition were fabricated by infiltration squeeze method. Effect of Pr addition on microstructures and fractographs of Al-Si MMCs was investigated by SEM and TEM. Tensile properties at room temperature and 200 °C were tested. It is shown that the addition of Pr is favorable to produce uniform microstructures and modify the eutectic Si crystal effectively. Compounds/intermetallics with high content of Pr are formed at the interface between short fiber and matrix. Yield strength(σ_0.2), ultimate tensile strength(σ_b) and fracture elongation of Al-Si MMCs are improved by adding suitable amount of Pr. Compared with those values of Al-Si based MMC at 200 °C, σ_0.2 and σ_b of MMC with 0.29% Pr are increased by 33% and 55%, respectively. The tensile fracture surface of Al-Si MMCs with Pr addition presents ductile fracture features.     

La~(3+)掺杂Y_2O_3透明陶瓷制备及发光性能

以Y2O3为基质材料,掺杂不同含量的La3+,采用机械力化学法制备纳米粉,粉体压制后在真空度1×10-3Pa下烧结得到La3+掺杂Y2O3透明陶瓷。采用透射电子显微镜(TEM)观察粉体一次颗粒形貌,扫描电镜(SEM)观察样品表面形貌,HV-1000型维氏硬度计测定样品硬度和断裂韧性,阿基米德法测定烧结后试样的相对密度,自动记录分光光度计测定试样透过率。结果表明:制备的La3+∶Y2O透明陶瓷透光率可达80%,掺杂La3+可以显著降低La3+∶Y2O3透明陶瓷的烧结温度;随着La2O3添加量的提高,样品透光率逐渐提高,但La2O3添加量过大会造成点阵畸变严重;随着La2O3添加量的提高,样品相对密度、维氏硬度和断裂韧性均逐渐提高,最后趋于平稳;随着保温时间延长,样品透光率也逐渐增大,继续增大保温时间,透光率趋于平缓。结合样品的透光率、相对密度、维氏硬度和断裂韧性考虑可知La2O3适合掺杂量、烧结温度和保温时间分别为10at%、1550℃和3h。     

Complex Solid Superacid Catalyst WO_3-ZrO_2-SO_4~(2-) Structure of Acid Sites on the Catalyst

A new type of complex solid superacid catalyst WO_3-ZrO_2-SO_4~(2-)with an acid strength H_0≤-16.04 wasprepared by kneading Zr(OH)_4 or amorphous ZrO_2 with tungstic acid(H_2WO_4)(W/Zr=0.15),followed byexposing this complex hydroxides to 0.5 tool/L H_2SO_4,calcining in air at 700～800℃ for 3h.This catalystpossesses both strong Bronsted acidity and strong Lewis acidity experimentally showed by IR observation ofpyridine absorbed on it.XPS and AES techniques were employed to examine the valence states of tungsten,zirconium,sulfur and their interactions.The structure of sulfur species was studied by infrared spectroscopyand a structure model of active site was proposed upon these results.