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。     

铜基化合物的可见光催化研究进展

与传统贵金属光催化剂相比，铜基光催化剂具有价格低廉、绿色环保、反应条件温和、光催化活性可调节等优势，受到合成化学家们广泛关注。本文简述了铜基催化剂的光催化历史，回顾了近五年来铜基化合物在可见光催化领域的研究成果与进展，总结了铜基催化剂的独立光催化机理与协同光催化机理；简要阐述了铜催化剂在不同类型反应中的应用，重点讨论了铜(Ⅰ)催化剂在烯烃官能化、碳-碳偶联、碳-杂偶联、原位催化等反应中的应用研究，表明铜基化合物在光催化合成领域具有很大的应用潜力。对未来的研究工作进行了展望，指出拓展催化剂的反应适用性、探索催化剂的氧化还原能力、进一步开发催化剂在手性合成中的应用将是该领域的研究重点。     

A facile method for preparation of PGS@ZB‐N and gas‐sol alternating synergistic effect for fire resistance of EVA

Through the simple precipitation of palygorskite (PGS) by zinc borate (ZB) (to make PGS@ZB) and the decoration of PGS@ZB by dodecylamine (N), a novel organic‐inorganic@inorganic hybrid flame retardant of PGS@ZB‐N was prepared and was incorporated with ethylene vinyl acetate copolymer (EVA) to improve its flame retardance. The structure and morphology of PGS@ZB‐N were characterized by Fourier transform infrared (FTIR) spectroscopy, X‐ray diffraction (XRD), and scanning electron microscopy (SEM), and it was confirmed that the PGS@ZB‐N hybrid had been successfully prepared. The flame retardancy and burning behavior of EVA/PGS@ZB‐N/EG (EG = expandable graphite) composite were studied through thermogravimetric analysis (TGA), limiting oxygen index (LOI), UL‐94 (by the vertical burning test), and cone calorimeter test (CCT) characterizations. The prepared EVA/PGS@ZB‐N/EG composite obtained an LOI value of 41.2% with the addition of 30 wt% PGS@ZB‐N/EG. It was found that EVA/PGS@ZB‐N/EG was protected through a gas phase and condensed phase alternating synergistic effect mechanism.     

基于3D打印技术复制砂浆节理的剪切试验及峰值抗剪强度模型

为进一步研究节理三维形貌特征与节理峰值抗剪强度的关系,首先采用巴西劈裂试验获取了自然劈裂岩石表面,通过三维扫描技术获取了节理面形态的高精度点云,通过逆向建模得到了自然岩石表面的立体模型,结合3D打印技术制作出了与自然岩石表面一致的PLA模具,以3D打印获得的底模通过水泥砂浆浇筑了含有自然结构面形貌的相似节理面试样。PLA模具与复制材料差异较大,复制材料在凝结过程中不易与PLA模具黏结,进而使脱模过程较为方便,不会破坏节理面。同时PLA模具可重复进行相似材料复制工作,具有可重复使用的优点。然后进行了具有5组形貌面的20个水泥砂浆节理面在4种不同法向荷载情况下的结构面剪切试验,得到了结构面剪切位移-荷载曲线。研究了结构面峰值抗剪强度、峰值位移、剪切刚度影响因素。节理经过剪切后形貌面出现不同程度的磨损,其磨损范围与等效高差分布范围基本一致,并且在等效高差为剪断破坏模式且成片的区域磨损较为严重。在新粗糙度指标基础上提出了新的峰值抗剪强度模型,经试验对比显示出新模型的有效性。在新模型基础上提出了一个简化模型。对比发现新模型简化后其计算精度较新模型有所降低但由于所需参数减小计算较为方便,新模型简化结果精度虽然有所下降但是还是比Barton公式精度高。     

上榆泉煤矿煤泥水多参数在线检测系统应用研究

针对上榆泉煤矿煤泥水性质参数人工检测周期长、误差大、滞后性严重的问题,采用多参数传感器和PLC,开发了煤泥水多参数在线检测系统。经过8 h稳定运行,平均结果显示该厂煤泥水参数为pH值为7.71、浓度9.45%、中值直径(D50)39.56μm、流量2 440 m3/h、水质硬度428.94 mg/L,与人工检测结果相一致。应用结果表明,该检测系统能够实现煤泥水多参数在线监测和数据分析功能,使煤泥水的处理更高效。     

金属多孔材料喷墨制备法的研究与进展

喷墨三维打印作为金属增材制造技术的一种重要方法,已广泛应用于金属多孔材料的制备,具有成本低、操作简单、成型材料范围广、孔结构设计灵活性大,较好的制件精度和结构精细度等优点.系统地总结了钛及钛合金、不锈钢、镍基合金、铝合金等多孔材料喷墨三维打印技术制备工艺与组织结构的国内外最新研究进展、目前存在的问题,以及应用前景.     

基于UG的正交车铣加工回转体表面微观残留仿真

正交车铣加工的回转体表面由铣刀与工件的复合相对运动形成,其形成机理独特,多个参数影响其表面微观形貌。为研究切削参数对正交车铣回转体表面微观残留的影响,基于UG建立了正交车铣回转体表面的仿真加工方法,并通过Vericut构建了虚拟五轴车铣加工环境,由此仿真研究了周向每齿进给量对正交车铣回转体表面微观残留的影响,发现已加工表面微观残留高度随周向每齿进给量增加显著增大。     

Single-Crystalline TiO2(B) Nanobelts with Unusual Large Exposed {100} Facets and Enhanced Li-Storage Capacity

The {100} facet of single-crystalline TiO₂(B) is an ideal platform for inserting Li ions, but it is hard to be obtained due to its high surface energy. Here, the single-crystalline TiO₂(B) nanobelts from H₂Ti₃O₇ with nearly 70% {100} facets exposed are synthesized, which significantly enhances Li-storage capacity. The first-principle calculations demonstrate an ab in-plane 2D diffusion through the exposed {100} facets. As a consequence, the nanobelts can significantly accommodate Li ions in LiTiO₂ formula with specific capacity up to 335 mAh g⁻¹, which is in good agreement with the electrochemical characterizations. Coating with conductive and protective poly(3,4-ethylenedioxythiophene)-poly(styrenesulfonate), the cut-off discharge voltage is as low as 0.5 V, leading to a capacity of 160.7 mAh g⁻¹ after 1500 cycles with a retention rate of 66% at 1C. This work provides a practical strategy to increase the Li-ion capacity and cycle stability by tailoring the crystal orientation and nanostructures.