3-羰基-雄甾-4-烯-17β-酸的合成

以脱氢异雄酮(DHEA)为原料,经过Wittig反应、硼氢化-氧化反应、Oppenauer反应和Jone's氧化反应合成了重要甾体中间体3-羰基-雄甾4-烯-17β-酸,总收率达23.0%,并采用核磁、质谱和红外表征了产物结构.     

蓖麻油裂解制癸二酸生产工艺研究进展

论述了近年来蓖麻油裂解制癸二酸生产工艺的研究进展,重点介绍了生产工艺的改进、含酚废水的治理、癸二酸的提纯等方面的最新研究成果,并指出目前癸二酸生产中仍存在的问题和进一步研究的方向.特别提出了回收游离碱的新观点.     

化学交换精馏法分离硼同位素分解反应实验研究

三氟化硼-苯甲醚的分解反应是三氟化硼-苯甲醚络合物化学交换精馏法分离硼同位素不可缺少的步骤。由于三氟化硼-苯甲醚络合物分解过程中伴随苯甲醚的分解,使过程变得复杂,文中理论分析了苯甲醚分解的原因,用逆流多级串联装置研究了分解反应,并用高效液相色谱对产物进行分析;为获得反应的最佳操作条件,测定了反应时间和温度对络合物分解反应的影响,并分析了产生这种结果的原因。结果表明,当反应时间为0.5—1 h、温度为150℃时产物中苯甲醚的质量分数可达到97%以上,从而使络合物完全分解而苯甲醚最小程度的分解,确保了整个分离系统的正常连续运转。     

Experimental evaluation of Pt/TiO2/rGO as an efficient HER catalyst via artificial photosynthesis under UVB & visible irradiation

The study investigated the synergistic effects of rGO and Pt over TiO₂ for the HER via artificial photosynthesis under UVB and visible light irradiation. The introduction of glycerol and industrial wastewater to the system as sacrificial reductants signifies that the major reaction pathway is photocatalytic partial water splitting. The material characterizations revealed successful heterojunction formation and provided insight into chemistry behind the activity of the photocatalysts. Amongst various combinations of rGO on TiO₂, 1GNT exhibited an HER yield five times that of bare TiO₂ under UVB light. Addition of Pt led to the formation of a strong Schottky barrier at the heterojunction and consequently boosted HER performance. 1P0.5 GT presented the highest of 28.5 mmol g⁻¹ h⁻¹ with glycerol and 9.6 mmol g⁻¹ h⁻¹ with wastewater under UVB light respectively. For both binary and ternary photocatalysts, the HER performances dwindled under visible light irradiation, accentuating the insufficient activation of the TiO₂. In addition, 1PT outperformed all the other photocatalysts thereby elucidating the impression that rGO and Pt does not work well together in enhancing HER despite quenching the exciton recombination rate of TiO₂ significantly. The role of pH in the synthesis and the experiments has been discussed. Finally, the underlying mechanisms in the photodeposition and photoreformation have been proposed.     

Pepsin-induced changes in the size and molecular weight distribution of bovine casein during enzymatic hydrolysis

Bovine casein was digested with pepsin at pH 2.0 in a batch-stirred tank reactor. To investigate the effect of peptic digestion on the aggregate size and molecular weight distribution of bovine casein, the resulting hydrolysates were examined by size-exclusion chromatography coupled with multiangle laser light scattering and dynamic light scattering. Casein was resolved by size-exclusion chromatography into 2 major peaks corresponding to aggregates and monomers, both of which showed a continuous decrease as hydrolysis proceeded. However, the ratio of aggregates to monomers was maintained at almost 1 (2:2.5) during the initial 30-min hydrolysis, indicating that the caseins in solution were in a type of equilibrium between aggregates and monomers. Upon peptic hydrolysis, casein aggregates increased in size and molecular weight, and exhibited a decrease in intermolecular repulsion. This finding was confirmed by dynamic light scattering measurements, which traced the changes in the hydrodynamic radii and light scattering intensities of casein hydrolysates. In addition, the release kinetics of peptide fractions with different molecular weights was also examined. It was concluded that the increase in hydrophobic attraction and the reduction in intermicellar repulsion might promote the growth in aggregate size of bovine casein during the limited hydrolysis.     

Comparison of different methods to prepare MgO whiskers

Magnesia whiskers have been made by hydrolysis of MgCl₂–KCl melt and conversion of magnesium hydroxide whiskers. The morphology of MgO whiskers was examined by SEM and TEM. Composition of products was identified by XRD. Comparisons have been made on the morphology and quality of the products by different methods. Discussions have been made on the efficiency, product quality control and scale-up feasibility of these methods. Whiskers prepared by hydrolysis have uniform diameter but other shapes of magnesia are often found. Conversion of Mg(OH)₂ whiskers to MgO whiskers is simple and easy to scale-up, but the product often has many defects caused by decomposition. Nevertheless, the single crystal structure can be reserved as revealed by electron diffraction. XRD results show that the purity of products by hydrolysis is better than that by conversion. The conversion method is more hopeful for industrial production.     

A generalized hybrid transfinite element computational approach for nonlinear/linear unified thermal-structural analysis

The paper describes the development of a new hybrid computational approach for nonlinear/linear thermal-structural analysis. The proposed transfinite element approach is a hybrid scheme as it combines the modeling versatility of contemporary finite elements with transform methods and the classical Bubnov-Galerkin schemes. Application of the proposed formulations for nonlinear analysis is also developed. Several test cases are presented to include nonlinear/linear unified thermal-stress and thermal-stress wave propagations. Comparative results validate the fundamental capabilities of the proposed hybrid transfmite element methodology.     

Scanning tunneling microscope combined with scanning electron microscope

A scanning tunneling microscope (STM) has been installed in a usual scanning electron microscope (SEM) with a vacuum of 10⁻⁶ Torr. The STM image is displayed on the cathode ray tube of the SEM, 512 × 512 pixels, with a scanning rate of 80 s/picture. The spatial resolution of the STM is about 1 Å, while that of the SEM is several tens of ångströms. The combined scanning microscope covers a wide magnification range from 10 to 10⁷, where STM covers the high magnification region from 10⁵ to 10⁷.     

GO/PEDOT复合材料修饰阳极的制备及其在MFC中的应用

微生物燃料电池（MFC）是一种利用微生物将有机物中的化学能直接转化成电能的装置,通过改善阳极特性可以有效提高微生物燃料电池的产电性能。通过恒电流法电沉积制备了氧化石墨烯/聚3,4-乙烯二氧噻吩（GO/PEDOT）复合材料修饰碳毡（CF）阳极。通过循环伏安法和交流阻抗法考察了电极特性。将其应用到微生物燃料电池中,对其产电性能进行评价。结果表明,GO/PEDOT-CF电极具有较大的比表面积和优良的电化学性能;以GO/PEDOT-CF为阳极的微生物燃料电池,产电性能良好,其最大功率密度和最大电流密度达到1.138 W·m^-2和4.714 A·m^-2,分别是未修饰阳极的4.80倍和5.51倍。因此,GO/PEDOT复合材料是一种优良的阳极修饰材料,可有效提高MFC的产电性能。     

Efficient synthesis of titania nanotubes and enhanced photoresponse of Pt decorated TiO2 for water splitting

We investigated the effect of HMT (hexamethylenetetraamine) on the anodic growth of TiO₂ nanotube arrays. The tube length increases to 4.3 μm with HMT concentration increasing to 0.04 mol·L⁻¹. Adsorption of HMT on the TiO₂ surface is shown to markedly decrease the chemical dissolution rate of tube mouth, resulting in longer nanotube length. Furthermore, Pt nanoparticles were successfully deposited on the surface of TiO₂ nanotubes by ac electrodeposition method. The TiO₂/Pt composites were characterized by field emission scanning electron microscope (FESEM), X-ray photoelectron spectra (XPS), and photoelectrochemistry. An enhancement in photocurrent density has been achieved upon modification of TiO₂ nanotubes with Pt nanoparticles.