异丁醛氧化制丙酮热导气相色谱分析

本工作用２米４０１有机担体填充柱，在带四臂热导检测器的国产１０３型气相色谱仪上，仅８分钟将原料异丁醛、产物丙酮及水进行良好分离，并采用内标法定量，其最大平均偏差在±２％以内。方法简单、快速、准确     

Preparation and characterization of oxygen deficient perovskites,BaBiO3−x

Oxygen nonstoichiometry in the distorted perovskite BaBiO₃ has been studied by thermogravimetric analysis using controlled oxygen pressures. Three distinct regions of nonstoichiometry are observed with composition ranges which narrow as the temperature is lowered. Samples isolated from each region were shown by powder X-ray diffraction to retain the perovskite subcell but show different types of framework distortion. Low temperature reoxidation of the oxygen deficient phases is also described.     

氧气液相氧化一元取代甲苯制备芳香醛

研究了在酸碱不同体系下气氛液相氧化对氯甲苯、邻硝基甲苯制取相应芳香醛的反应 ,比较了反应温度、反应时间、氧气流量、底物浓度对各自反应的影响。初步研究了反应在酸碱不同条件下的反应机理 ,认为在醋酸体系下是自由基反应 ,而在有机胺体系下应是碳负离子反应。     

乙烯直接氧化合成乙酸

用常规固定床反应器考察了Pd-SiW12/SiO2催化剂还原条件对乙烯直接氧化合成乙酸催化性能的影响。催化剂用H2在200－300℃还原后Pd 的分散度较高，其催化活性远高于肼在液相中还原的催化剂，在乙烯气相氧化合成乙酸反应的原料气中，适量1，2－二氯乙烷的存在有助于提高乙酸的选择性和时空产率，初步考察了Pd-Se-SiW12/SiO2催化剂连续206h运转的稳定性，结果表明，催化剂中Pd晶粒的长大和硅钨酸的流失是造成催化剂失活的主要原因。     

Vanadium species in new catalysts for the selective oxidation of methane to formaldehyde: Activation of the catalytic sites

New vanadium oxide supported on mesoporous silica catalysts for the oxidation of methane to formaldehyde were investigated by infrared and Raman spectroscopies to identify and characterize the molecular structure of the most active and selective catalytic sites. In situ and operando experiments have been conducted in order to understand the redox and hydroxylation/dehydroxylation processes of the vanadium species. (SiO)₂VO(OH) species were identified in these catalysts in reaction conditions and shown to undergo a deprotonation at 580 °C under vacuum, leading to a site giving a photoluminescence band at 550 nm attributed to reverse radiative decay from the excited triplet state:

(V⁴⁺–O⁻)^*  (V⁵⁺O²⁻). An activation mechanism of vanadium monomeric species with electrophilic oxygen species is proposed.     

甲醇氧化制甲醛铁钼催化剂的研究

采用共沉淀法制备甲醇氧化制甲醛无载体铁钼催化剂,并考察了催化剂制备老化条件、焙烧温度、外型尺寸以及活性测试反应温度、空速对催化剂性能的影响。该催化剂在280~300℃、气空速7000 h-1~8000 h-1、进料φ(甲醇)为5.5%的下,可获≥98%的甲醇转化率,≥92%的甲醛选择性和≥90%的甲醛产率。催化剂活性高,强度好,性能稳定。     

Long-term stability of an Au/Al2O3 catalyst prepared by incipient wetness in continuous-flow glucose oxidation

A 0.3% Au/Al₂O₃ catalyst prepared by the incipient wetness (IW) method was investigated in the continuous-flow liquid-phase glucose oxidation. Therefore, a continuous stirred tank reactor (CSTR) system equipped with an ultrasonic separator was used. The continuous-flow glucose oxidation was carried out at 40 °C, pH 9 and 1 bar oxygen partial pressure. Residence time and glucose concentration were varied. The IW gold catalyst showed very high activity and selectivity to gluconic acid within its 110 days of operation and, thus, an excellent long-term stability. Even after severe microbial contaminations of the catalyst, its activity could be completely restored by in situ regeneration with 2-propanol.     

Internal-oxide-band formation during oxidation of Ag-Mg alloys

Ag-3a/oMg was oxidized in air over the range of 400–900°C. Internal-oxide bands of MgO formed approximately parallel to the surface, the first band appearing at some finite, but irregular depth below the surface. The region between the surface and the first band appeared to be free of precipitates, but TEM showed that very small clusters, about 50 Å in diameter, formed in the PFZ, causing significant hardness (greater than 300 VHN). The clusters contain more oxygen than that corresponding to stoichiometric MgO. The hardness between oxide bands was also high, but not as high as in the PFZ. The kinetics of thickening of the internal-band region followed the parabolic rate law between 400 and 700° C, with departures from the parabolic law occurring at higher temperatures. The activation energy for the parabolic rate constants was 19.4 Kcal/mol, a value less than the total for oxygen diffusion and oxygen dissolution. The reaction front was planar and parallel to the surface prior to band formation at temperatures of 400–600° C. Nucleation of the first band resulted in nonplanar and nonparallel oxide. Little or no correlation existed between grain boundaries and oxide formation. Nodules of virtually pure silver formed on the surface initially at grain boundaries and subsequently within grains. Nodule formation is attributed to stress-enhanced (resulting from strains associated with precipitation) diffusion of silver to the surface via dislocation pipes. Internal-band formation is discussed in terms of prior data in the literature and various models. It is thought that stress effects (induced by precipitation), nucleation, and clustering of oxygen with Mg play significant roles in causing internal-band formation.     

Influence of silicon on the oxidation of titanium between 550 and 700°C

The oxidation behavior of Ti-Si alloys (0.25, 0.5, and 1 Wt. % Si) was investigated between 550 and 700°C; in oxygen by continuous thermogravimetry for a maximum duration of about 500 hr and, in air by daily weighing for durations from a few hundred to several thousand hours. The kinetics results revealed that the presence of silicon leads to a decrease in oxidation rate which is more evident when the temperature is raised and the silicon content is increased. Morphological and structural examinations revealed that silicon modifies the internal architecture of oxide layers when compared with unalloyed titanium; in particular, reduced porosity in the layers is observed. Analysis showed that silicon is uniformly distributed in the oxide layer. However, while part of the silicon is in solid solution in the rutile, some is also precipitated as small crystals ( <1 m at 850°C) of SiO₂, of cristobalite structure. The adherence of oxide layers to the metal substrate was measured after cooling of samples; the addition of silicon has been observed to modify, in a manner dependent on its content, the adherence of oxide layers.     

Preparation of micro-arc oxidation coatings on magnesium alloy and its thermal shock resistance property

1. Introduction Due to their high specific strength, good electro-magnetic shielding characteristics, high damping characteristics, good cast ability, and excellent pol-ishing capability, magnesium alloys are extensively used in aeronautical, automobile, and electro- communication industries [1-3]. But magnesium has some disadvantages, such as low chemical stability, high negative electric potential, and low hardness, so it is necessary to use surface disposal to accommo-date the demand for re…