3-三氟甲基-5,6,7,8-四氢-1,2,4-三唑[4,3-α]吡嗪盐酸盐的合成

乙二胺与氯乙酸乙酯经取代、环合反应制得2-哌嗪酮,2-哌嗪酮与Boc酸酐进行氨基保护反应后,再与五硫化二磷进行硫代反应制得4-(N-叔丁氧羰基)-2-哌嗪硫酮,其与三氟乙酰肼经取代、环合、脱叔丁氧羰基成盐,得标题化合物,总收率为45.7%(以氯乙酸乙酯计)。为磷酸西他列汀中间体的工业化生产提供了一条较理想的工艺路线。     

Porous sunflower plate-like NiFe2O4/CoNi–S heterostructure as efficient electrocatalyst for overall water splitting

Constructing high-efficient and nonprecious electrocatalysts is of primary importance for improving the efficiency of water splitting. Herein, a novel sunflower plate-like NiFe₂O₄/CoNi–S nanosheet heterostructure was fabricated via facile hydrothermal and electrodeposition methods. The as-fabricated NiFe₂O₄/CoNi–S heterostructure array exhibits remarkable bifunctional catalytic activity and stability toward oxygen evolution reaction (OER) and hydrogen evolution reaction (HER) in alkaline media. It presents a small overpotential of 219 mV and 149 mV for OER and HER, respectively, to produce a current density of 10 mA cm^?2. More significantly, when the obtained electrodes are used as both the cathode and anode in an electrolyzer, a voltage of 1.57 V is gained at 10 mA cm^?2, with superior stability for 72 h. Such outstanding properties are ascribed to: the 3D porous network structure, which exposes more active sites and accelerates mass transfer and gas bubble emission; the high conductivity of CoNi–S, which provides faster charge transport and thus promotes the electrocatalytic reaction of the composites; and the effective interface engineering between NiFe₂O₄ (excellent performance for OER) and CoNi–S (high activity for HER), which leads to a shorter transport pathway and thus expedites electron transfer. This work provides a new strategy for designing efficient and inexpensive electrocatalysts for water splitting.     

Study on the Height of the Mining-Induced Water-Conducting Fracture Zone Under the Q 2l Loess Cover of the Jurassic Coal Seam in Northern Shaanxi,China

A method to calculate the height of a water-conducting fractured zone (HWCFZ) was developed based on the plate and shell theory, and the development of the HWCFZ in bedrock and Q2l loess strata is discussed in detail. First, the subsidence-deflection curve equation of the overlying stratum is theoretically derived, and then the ultimate deflection and free space height of rock strata are calculated. Moreover, the strata tensile strain is calculated by using integral calculus. In addition, the failure state of the rock is analyzed by comparing the theoretically calculated tensile strain with the experimentally measured yield tensile strain, allowing one to attain the maximum value of HWCFZ. This approach was tested at the Jinjitan coal mine; the theoretically predicted, experimentally measured, and numerically computed maximum HWCFZ values were 189.5, 187.3, and 188.5 m, respectively, demonstrating the accuracy of the proposed method. These results are highly significant for safe and environment-friendly coal mining in northwest Shaanxi, China.     

Design and Fabrication of Concentration‐Gradient Generators with Two and Three Inlets in Microfluidic Chips

A simple and low‐cost method for designing and fabricating concentration‐gradient generators with two and three inlets is proposed which can generate different concentration gradients at varying flow velocities. The microchannel structure was designed in S‐shape and left‐right symmetry. The concentration‐gradient generator was simulated based on the finite element method. The microchannels were processed on a computer numerical control (CNC) engraving and milling machine on poly(methylmethacrylate) substrate, and then two concentration‐gradient generators were fabricated by hot bonding technology. The results of experiment and simulation were compared to prove the feasibility of the method. Flow velocity was an important factor for generating different concentration gradients. The concentration‐gradient profiles of the generators with two and three inlets present approximately linear and quadratic curves.     

Tailoring the electron-blocking layer by addition of YSZ to Ba-containing anode for improvement of ceria-based solid oxide fuel cell

The in-situ fabrication of an electron-blocking layer between the Ba-containing anode and the ceria-based electrolyte is an effective approach in suppressing the internal electronic leakage in ceria-based solid oxide fuel cell (SOFC). To improve the thickness of the electron-blocking layer and to research the effect of the layer thickness on the improvement of SOFC, a Ba-containing compound (0.6NiO-0.4BaZr_0.1Ce_0.7Y_0.2O_3-δ) modified by Y stabilized zirconia (YSZ) was employed as a composite anode in this research. SEM analyses demonstrated that the thickness of the interlayer can be simply controlled by regulating the proportion of YSZ at anode. The in-situ formed interlayer in the cell with the anode modified by 20?mol% YSZ possesses a thickness of 0.9?µm which is more suitable for the cell achieving an enhanced performance.     

Transesterification of Palm-based Methyl Palmitate into Esteramine Catalyzed by Calcium Oxide Catalyst

The technology for transesterification reactions between methyl esters and alcohols is well established by using classical homogeneous alkaline catalysts, which provide high conversion of methyl esters to specialty or nonindigenous esters. However, in certain products where the purity of the esters is of concern, the removal of homogeneous catalysts after the completion of the reaction is a challenge in terms of production cost and water footprint. Therefore, a study to investigate the potential of heterogeneous catalysts was conducted on reactions between methyl palmitate and triethanolamine. The degree of basicity and active surface area of calcium oxide (CaO), zinc oxide (ZnO), and magnesium oxide (MgO) were first characterized by using temperature-programmed desorption (TPD-CO₂) and Brunauere–Emmett–Teller (BET), respectively. Among the metal oxides investigated, the CaO catalyst showed the best catalytic activity toward the transesterification process as it gave the highest conversion of methyl palmitate and yielded fatty esteramine compositions similar to the conventional homogeneous catalyst. The optimum transesterification condition by using the CaO catalyst utilized a lower vacuum system of approximately 200 mbar, which could minimize a considerable amount of energy consumption. Furthermore, low CaO dosage of 0.1% was able to give a conversion of 94.5% methyl ester and formed esteramine at 170 °C for 2 h. Therefore, the production of esterquats from esteramine may become more economically feasible through the methyl ester route by using the CaO catalyst, which can be recycled three times.