功能化酸性离子液体催化甲醛与烯烃的Prins缩合反应

研究了以功能化酸性离子液体为催化剂,甲醛与烯烃Prins缩合反应生成1,3-二噁烷及其衍生物,水解得到1,3-二元醇.对不同结构的离子液体、催化剂用量和反应条件进行了考察.结果表明,该体系具有良好的催化性能,反应可在较温和的条件下进行,实现了高活性和高选择性的目标.产物易分离,催化剂重复使用6次,其催化活性基本不变.     

UHPLC-Quadrupole/Orbitrap MS同步检测十字花科植物中的游离氨基酸

采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱联用技术(UHPLC-Quadrupole/Orbitrap MS)结合柱前衍生法建立了可同时测定28种游离氨基酸的分析方法,并对十字花科植物中的游离氨基酸进行检测和分析。样品用超纯水提取后,经6-氨基喹啉基-N-羟基琥珀酰亚胺基甲酸酯(AQC)衍生,采用Waters BEH C18柱作为色谱柱,以pH 5.0乙酸铵缓冲溶液和80%乙腈水溶液作为流动相进行梯度洗脱。质谱检测器采用电喷雾离子源,在正离子模式下进行检测。实验结果表明,十字花科植物中含有25种以上游离氨基酸,其中包括人体必需的8种氨基酸。25种氨基酸在线性范围内相关性良好,平均加标回收率为80.5%~104.4%,相对标准偏差为0.6%~4.4%。不同氨基酸检测灵敏度不同,定量下限为0.01~1.45μmol/L。该方法杂质干扰小,分析速度快,灵敏度高,适用于植物样品中游离氨基酸的同步检测。     

高效液相色谱法测定柑橘汁中的柠檬苦素和柚皮苷

柑橘汁的苦味主要是由于柚皮苷和柠檬苦素的存在所致,其含量的测定可用于控制柑橘类果汁的质量。采用高效液相色谱法在KR100-5C18(4.6 mm i.d.×250 mm,5 μm)上,分别以乙腈-四氢呋喃-水(体积比为17.5∶17.5∶65)和甲醇-冰醋酸-水(体积比为40∶1∶59)为流动相（流速均为1 mL/min）,在207 nm和283 nm检测波长下分别测定了柠檬苦素和柚皮苷。实验结果表明,柠檬苦素在1.00～50.00 mg/L时线性关系良好(r=0.9992),检出限为0.07 μg,平均加标回收率为98.69%,相对标准偏差（RSD）为2.5%;柚皮苷在20.00～160.00 mg/L时线性关系良好(r=0.9988),检出限为0.14 μg,平均加标回收率为100.13%,RSD为1.5%。用该法检测柑橘汁样品中的柠檬苦素与柚皮苷,方法简便、快速、准确。     

羧基膦－钯－酸体系催化烯烃氢酯基化反应

以钯－膦－酸体系催化烯烃氢酯基化的反应日显重要，而膦配体是决定此反应的重要因素，用二苯基膦乙酸（ＤＰＡ）为配体的钯催化剂体系，对烯烃的氢酯基化反应作了研究。对影响反应的各种因素如反应温度、反应压力、不同的溶剂、膦配体及酸助剂的量等作了考察，发现此配体对烯烃的区域选择性有改善。并用此催化体系对不同结构的烯烃进行了研究，发现有如下的活性顺序：环烯烃＞直链端烯＞直链内烯。     

Synthesis of nanosize europium oxide particles by using W/O microemulsion

Europium hydroxide particles with an average diameter of 10 run and a BET surface area of 127 m2 /g have been prepared by controlled precipitation in the polyoxyethylene octylphenol (Triton X-100) (hex-anol)/cyclohexane/water microemulsion system. After calcination in air at 750℃, the obtained europium hydroxide particles were readily converted to the nanosize Eu2O3 particles with an average size of 30 nm and a high BET surface area of 36.5 m2/g.     

Effect of Hydrogen Implantation on SIMOX SOI Materials

Hydrogen ions were implanted into separation by implantation of oxygen (SIMOX) silicon-on-insulator (SOI) wafers near the oxygen-implantation-induced damage peak under different conditions of energy and dose. It was found that the implanted hydrogen ions not only accelerate the diffusion of oxygen atoms from the annealing ambience into the wafer but also cause an outward diffusion of oxygen atoms in the buried oxide (BOX) layer. Thus, greatly broadened buried oxygen-rich (BOR) layers were formed in our experiments, which are 18%-79% broader than the BOX layer of standard SIMOX SOI wafers under the same conditions of oxygen implantation. The mechanism was discussed. A potential low cost method to fabricate SIMOX SOI wafers is proposed.     

大电流碳纳米管场发射阴极研究

报道了在较大发射面积上获得较大场发射电流的碳纳米管场发射阴极。为了加强场发射电流,在丝网印刷浆料中增加一种金属纳米颗粒,金属颗粒增强了碳纳米管发射体和衬底的接触,提高碳纳米管和衬底的粘附作用。利用改进后的丝网印刷方法制备了大电流碳纳米管场发射阴极,测得最大发射电流为68.0 mA,阴极有效发射面积约1.1 mm2,发射电流密度约6.2 A/cm2;并成功将改进方法制备的大电流场发射碳纳米管阴极应用于场发射真空器件原型。实验证明这种具有较大发射电流和较大发射电流密度的场发射能够满足部分大功率电子器件的需求。收稿日期:; 修订日期:     

基于色度传感器的“酒精检测”实验探究

探究了基于色度传感器的酒精检测实验, 尝试将实验从定性层面上升到定量层面, 发展成为酒精检测的探究性和创新性实验, 以期为传感技术应用于高中化学实验教学提供一些借鉴和思考。色度传感器在本实验中提供了即时、直观的数据支持, 拓展了实验原理在生活中的应用;开阔了学生的视野, 培养了学生的创新意识。     

Effect of solution temperature and cooling rate on microstructure and mechanical properties of laser solid forming Ti-6Al-4V alloy

The effect of solution temperature and cooling rate on microstructure and mechanical properties of laser solid forming (LSF) Ti-6Al-4V alloy is investigated.The samples are solutions treated at 900,950,and 1000°C,followed by water quenching,air cooling,and furnace cooling,respectively.It is found that the cooling rate of solution treatment has a more important effect on the microstructure in comparison with the solution temperature.The martensite α'formed during water quenching results in the higher hardnes...