An in situ Raman study of the intercalation of supercapacitor-type electrolyte into microcrystalline graphite

An initial Raman study on the effects of intercalation for aprotic electrolyte-based electrochemical double-layer capacitors (EDLCs) is reported. In situ Raman microscopy is employed in the study of the electrochemical intercalation of tetraethylammonium (Et₄N⁺) and tetrafluoroborate (BF₄⁻) into and out of microcrystalline graphite. During cyclic voltammetry experiments, the insertion of Et₄N⁺ into graphite for the negative electrode occurs at an onset potential of +1.0 V versus Li/Li⁺. For the positive electrode, BF₄⁻ was shown to intercalate above +4.3 V versus Li/Li⁺. The characteristic G-band doublet peak (E_2g2(i) (1578 cm⁻¹) and E_2g2(b) (1600 cm⁻¹)) showed that various staged compounds were formed in both cases and the return of the single G-band (1578 cm⁻¹) demonstrates that intercalation was fully reversible. The disappearance of the D-band (1329 cm⁻¹) in intercalated graphite is also noted and when the intercalant is removed a more intense D-band reappears, indicating possible lattice damage. For cation intercalation, such irreversible changes of the graphite structure are confirmed by scanning electron microscopy (SEM).     

Y-TZP/Al_2O_3超细粉末的研究

用共沉淀法制备了3mol％Y_2O_3-ZrO_2-20Wt％Al_2O_3超细粉末。利用热分析、X射线、粒度分析仪、透射电镜和扫描电镜等研究了粉末的性能。实验结果表明:制备的粉末组分均匀,颗粒粒度为10nm,粒度分布窄,团聚体尺寸小,烧结活性高。粉末的相组成为t-ZrO_2。烧结体显微结构致密细晶,具有优异的力学性能。     

Synthesis,characterization, and thermal behavior study of methyl methacrylate polymers containing 4‐carbazole substitutes

A new polymerizable monomer, [4‐(9‐ethyl)carbazolyl]methyl methacrylate ( 2 ), was synthesized by reacting of methacrylic acid and 4‐hydroxymethyl‐9‐ethyl carbazole ( 1 ) by esterification procedure in the presence of N,N′‐dicyclohexylcarbodiimide. The resulting monomer was then polymerized free‐radically to form the poly(methyl methacrylate) containing 4‐(9‐ethyl)carbazolyl pend ent groups. Also, copolymerization of monomer 2 with various acrylic monomers such as methyl methacrylate, ethyl methacrylate, methyl acrylate, ethyl acrylate, and n‐butyl acrylate by azobisisobutyronitrile as a free radical polymerization initiator gave the related copolymers in high yields. The structure of all the resulted compounds was characterized and confirmed by FTIR and ¹H NMR spectroscopic techniques. The average molecular weight of the obtained polymers was determined by gel permeation chromatography using tetrahydrofurane as the solvent. The thermal gravimetric analysis and differential scanning calorimeter instruments were used for studying of thermal properties of polymers. It was found that, with the incorporation of bulky 4‐(9‐ethyl)carbazolyl substitutes in side chains of methyl methacrylate polymers, thermal stability and glass transition temperature of polymers are increased. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 4989–4995, 2006     

吲哒帕胺的合成进展

简要概述了吲哒帕胺在医学上的研制、药用价值和市场应用情况及前景;介绍了吲哒 帕胺的物理性质,详细综述了以2,3-二氢-2-甲基-1H-吲哚和4-氯-3-磺胺基苯甲酰氯为 原料的合成方法和工艺,分析了其优点和缺点。     

5-氰基-4-氨基咪唑的合成与热性能

咪唑基含能化合物是目前高能化合物的重要研究方向，而5-氰基-4-氨基咪唑是设计、合成新型咪唑联四唑类高能高氮化合物的关键中间体。以5-甲酰胺基-4-氨基咪唑（AICON）为原料，经其与三氯氧磷（POCl3）的脱水反应获得了5-氰基-4-氨基咪唑（AICN），通过优化反应体系、反应温度、反应时间以及物料物质的量比，使得AICN的收率>65%，纯度（HPLC）>99.5%。此外，采用NMR、IR和元素分析对其进行了结构确征，利用热重分析法研究其热性能。结果表明：AICN的最佳反应条件为以POCl3为脱水剂，n(AICON)：n(POCl3)为1:10，反应升温模式为先快速升温至80~85 ℃，维持反应30 min，然后降温至70~75 ℃，维持反应1~1.5 h；AICN在40~1000 ℃温度区间存在两个失重过程，对应的热分解温度区间分别为40~400 ℃和400~1000 ℃、热失重分别为19.8%和60.7%、热分解峰温分别为256.5和698.4 ℃，表明其具有良好的热稳定性。     

光催化法处理含Cr(VI)废水的研究

采用P 25 TiO2作为光催化剂,研究了废水的pH值、Cr(VI)的初始浓度、气氛及有机物等因素对含铬废水中Cr(VI)去解率的影响。结果表明,在pH值为3.0时,光催化反应速率最大;反应气氛对该体系中Cr(VI)的光催化还原无明显影响;苯酚、葡萄糖等有机物的存在能有效地促进Cr(VI)的光催化还原,当加入与Cr(VI)等物质的量的苯酚或葡萄糖时,150 mL反应液[Cr(VI)浓度为0.96 mmol/L],0.15 g光催化剂,经12 W紫外灯照射反应120 m in,Cr(VI)完全被去除,相对于在反应体系中不加有机物时,Cr(VI)光催化还原效率提高了近100%;Cr(VI)的光催化还原符合L-H动力学规律。     

4,4′-二氨基苯磺酰苯胺的合成

该文对4,4′-二氨基苯磺酰苯胺(Ⅰ)的合成进行了研究。对硝基苯胺在90~95℃的水中用铁粉还原为对苯二胺,收率约90%;乙酰苯胺与氯磺酸〔n(乙酰苯胺)∶n(氯磺酸)=1∶4〕在60~65℃及氨基磺酸催化下,反应3 h生成对乙酰氨基苯磺酰氯,收率85%;乙酰氨基苯磺酰氯与对苯二胺在四丁基溴化胺催化下,于30~35℃反应12 h,生成4-乙酰氨基-4′-氨基苯磺酰苯胺;最后在95℃用氢氧化钠水解,得到4,4′-二氨基苯磺酰苯胺。高效液相色谱测得w(Ⅰ)>98.5%,总收率约75%。该路线生产成本比协作单位已有的生产工艺节省10%,已成功用于年产150 tⅠ的工业生产中。     

电热化学炮膛压测试系统的电磁兼容设计

由于电热化学炮发射时存在强电磁干扰和地电位浮动,膛压测试系统的测试准确性和仪器的安全性均受到了严重的影响。针对这一问题,根据恶劣条件下的动态测试理论,利用PCB的电磁兼容技术,不同材料多层组合的屏蔽技术,接地技术,滤波技术以及光电隔离技术,完成了基于电热化学炮膛压测试系统的电磁兼容设计。并通过试验验证了这种设计能有效解决电磁干扰问题,确保获得可靠的膛压数据,对分析电热化学炮结构的合理性,炮架的强度和刚度设计等有重要意义。     

钇铝石榴石粉体制备方法综述

综述了目前YAG粉体材料的几种合成方法,包括高温固相法、溶胶-凝胶法、燃烧法、喷雾热解法和化学沉淀法(化学共沉淀法、分步沉淀法和改进的化学共沉淀法),总结了每种方法的优缺点,并对YAG粉体材料新的合成工艺进行了展望。     

2,6-二氯-4-三氟甲基苯胺的研究进展

2，6－二氯－4－三氟甲基苯胺可以作为制备高效、低毒、低残留农药和新型高效除草剂的中间体，其重要性日益为有机化学家和农药生产企业所重视。本文介绍合成该化合物的各种方法对各自的优缺点进行了比较，并对由其合成的各种农药、除草剂的特性和用途进行了综述。