2，4-二溴苯酚的合成实验

研究了以苯酚为原料,在乙醇一水介质中,进行溴化反应生成2,4-二溴苯酚的优化工艺条件。合成最佳反应条件为：苯酚、溴素与双氧水的物质的量比为1：0．98：0．98,演化反应温度为0—5℃;反应时间为2h;洗涤温度为40—50℃。优化条件下,收率可达96％,产品经质谱验证及气相色谱分析,百分含量为98．3％。     

2-丁烯醛生产工艺改进研究

简单介绍了2-丁烯醛的用途、国内外生产概况及传统生产工艺,建立了2-丁烯醛的清洁生产工艺,并与传统工艺进行了比较。新工艺克服了传统缩合法能耗高、污染重的问题,可在同行业中起示范作用,具有一定的推广前景。     

(3R,4R)-3-[(1′R)-叔丁基二甲基硅氧乙基]-4-乙酰氧基-2-氮杂环丁酮的合成

以化合物(3S,4S)-3-[(1′R)-叔丁基二甲基硅氧乙基]-4-羧基-1-对甲氧基苯基-2-氮杂环丁酮为主要原料,以卟啉锰为催化剂,经氧化脱羧,再由O3氧化脱保护基制得(3R,4R)-3-[(1′R)-叔丁基二甲基硅氧乙基]-4-乙酰氧基-2-氮杂环丁酮(4AA),两步反应总收率达到83.7%.采用卟啉锰做催化剂进行脱羧氧化反应,使该步反应收率达到了93.0%.用FT-IR、1HNMR对最终产物结构进行了表征.     

乙酸(酯)-甲醛缩合制丙烯酸(酯)研究进展

近年来,通过乙酸（酯）和甲醛缩合制备丙烯酸的新路线吸引了学术界和工业界的广泛关注。此新路线的优点是过程简单,原料可从天然气、煤化工产品中获得,成本低廉,对可持续生产丙烯酸具有十分重要的意义。国内外研究者针对这一反应开发了多种类型的催化剂,包括钒磷氧（VPO）类催化剂、负载型碱金属/碱土金属以及离子液体等。本文综述了不同种类催化剂近期的研究成果,总结了三类催化剂的优缺点。指出均相的离子液体催化剂具有反应温度低、能耗少、选择性高的特点,但反应为间歇操作,产物分离困难、催化剂较难重复利用,催化效率偏低。VPO类催化剂和碱金属/碱土金属类催化剂,反应温度较高（320～400℃）,但可实现连续反应,产物分离方便,催化效率较高。相比于VPO类催化剂,碱金属/碱土金属类催化剂涉及的反应较少,对目标产物的选择性较高,但整体催化效能低于VPO类催化剂,且失活催化剂再生困难。最新的研究结果表明,经典的有机相法制备VPO前体可以被更加简便、经济与环境友好的一锅水相法取代。空气氛中简单焙烧即可完成催化剂前体的活化。不仅大大简化了催化剂制备,而且所得催化剂的小试性能优异,从而为后续应用奠定了重要基础。     

Truss-arch model for shear strength of seismic-damaged SRC frame columns strengthened with CFRP sheets

Carbon fiber reinforced polymer (CFRP) materials are important reinforcing substances which are widely used in the shear strengthening of seismic-damage steel reinforced concrete (SRC) frame structures. To investigate the shear strength of SRC frame columns strengthened with CFRP sheets, experimental observations on eight seismic-damaged SRC frame columns strengthened with CFRP sheets were conducted at Yangtze University and existing experimental data of 49 SRC columns are presented. Based on the existing experiments, the theories of damage degree, zoning analysis of concrete, and strengthening material of the column are adopted. To present the expression formula of the shear strength of SRC frame columns strengthened with CFRP sheets, the contributions of strengthening material and transverse reinforcement to shear strength in the truss model are considered, based on the truss-arch model. The contribution of arch action is also considered through the analysis of the whole concrete and that of the three zones of the concrete are also considered. The formula is verified, and the calculated results are found to match well with the experimental results. Results indicate that the proposed whole analysis model can improve the accuracy of shear strength predictions of shear seismic-damaged SRC frame columns reinforced with CFRP sheets.     

磨木木素在硫酸盐法蒸煮过程中的反应

在木糖存在的条件下,采用硫酸盐法蒸煮的方法对蓝花楹磨木木素(milled wood lignin,简称MWL)进行处理,然后对处理后的产物进行红外光谱和13C-NMR分析,研究蓝花楹MWL的结构变化,探讨在硫酸盐法蒸煮过程中木素-碳水化合物复合体(lignin-carbohydrate complexes,简称LCC)的形成情况。研究发现:蓝花楹MWL结构单元之间的α-烷基芳基醚键、β-O-4型连接键很容易发生断裂,而在这些连接键发生断裂的同时,形成的木素中间体与糖产生化学键的结合,蒸煮液中有新的LCC结构形成。     

Effect of Ti on microstructure and properties of electromagnetic stirred Al-18wt.%Mg2Si alloy

By adding different amounts of Ti into the electromagnetic stirred Al-18wt.%Mg₂Si alloy, the effect of Ti element on the microstructure and mechanical properties of the alloy was studied. The experimental results show that the microstructure is refined after modification with Ti, which is related to the heterogeneous nucleation of TiAl₃ particles on the α-Al matrix. With the increase of Ti content and holding time after stirring, the primary Mg₂Si phase is refine...     

杂环轮烯类化合物密度泛函理论研究

运用量子化学中的密度泛函和含时密度泛函理论法,计算了四种加共轭环的脱氢苯[15]轮烯衍生物的几何构型、电子结构、前线分子轨道和电子光谱性质。计算结果表明当脱氢苯[15]轮烯分子(M)被杂环取代或增加分子的共轭性,对轮烯的键长和键角等结构参数的影响不大,这与轮烯具有较强的共轭性有关。当母体中的苯环被嘧啶环取代时,最大吸收波长蓝移;当母体中的苯环被萘取代时,最大吸收波长与母体中的苯被吡嗪取代时的最大吸收波长相近。     

Polyoxomolybdate-derived MoS2/nitrogen-doped reduced graphene oxide hybrids for efficient hydrogen evolution

Integrating MoS₂ with carbon-based materials, especially graphene, is an effective strategy for preparing highly active non-noble-metal electrocatalysts in the hydrogen evolution reaction (HER). This work demonstrates a convenient hydrothermal method to fabricate molybdenum disulfide nanosheets/nitrogen-doped reduced graphene oxide (MoS₂/NGO) hybrids using polyoxomolybdate as the Mo precursor. Introducing more defects and expanding interlayer spacing of MoS₂ can be achieved through decreasing the pH value of the reactive system due to the existed high-nuclear polyoxometalate clusters. MoS₂/NGO hybrids prepared at low pH exhibit superior HER activity to those obtained at high pH. MoS₂/NGO-pH1.5 exhibits an ultralow overpotential of 81 mV at 10 mA cm⁻², a low Tafel slope of 60 mV·dec⁻¹ and good stability in alkaline electrolyte. Such excellent electrocatalytic activity is contributed by the abundant HER catalytic active sites, the increased electrochemically-accessible area and the synergetic effects between the active MoS₂ catalyst and NGO support.     

基于嵌入式技术的拉曼光纤激光器控制研究

为提升拉曼光纤激光器控制稳定性,提出了基于嵌入式技术的拉曼光纤激光器控制系统.拉曼光纤激光器的输出电压模拟信号经A/D模块转换为数字信号后,传送到FPGA控制单元,FPGA控制单元基于接收到的数字信号与控制电压之间偏差,利用粒子群算法改进模糊PID控制器实施优化,处理误差信号,实现拉曼光纤激光器控制,同时采用并行通信方...