La2O3对氧化铝透明陶瓷显微结构和透光性能的影响

采用传统无压烧结工艺在氢气氛下制备Al2O3透明陶瓷。实验结果表明：MgO和La2O3复合添加时，随着La2O3掺杂量的增加体积密度总体上保持上升的趋势。随着保温时间的延长，陶瓷的致密化程度增大，残余气孔逐步排出，晶粒进一步长大。采用La2O3和MgO复合添加比单独掺入MgO陶瓷样品透过率更高，掺杂效果更好。在烧结温度为1750℃，保温时问为1h条件下，在波艮为300～800nm测试范围内，陶瓷样品的全透过率大于82％，最大值为86％。     

Development of an alcohol optode membrane based on fluorescence enhancement of fluorescein derivatives

A new type of optode membrane for the determination of alcohols, such as methanol, ethanol, propan-1-ol and propan-2-ol etc, is presented that can be exploited in optical and fibre-optic sensors. It is based on the use of a new lipophilic fluorescent reagent, namely fluorescein octadecyl ester (FODE), which is immobilized in a plasticized PVC membrane. The response mechanism relies on the fact that FODE can reversibly recognize alcohol molecules due to the hydrogen bonding formation between FODE and alcohol molecules. The analytical information in this membrane is the enhancement of the relative fluorescence intensity measured at 527 nm (463 nm, excitation). Under the optimum condition, the membrane has a wide measuring range for alcohol samples. The membrane has been applied to determine the concentration of ethanol in alcoholic drinks with satisfactory results.     

新型含金属元素二胺的合成与表征

本文分别用液相法和固相法合成了一系列含不同金属元素的二胺,并通过红外光谱,~1HNMR、~(13)CNMR,紫外光谱,电化学分析及元素分析对其进行表征,还通过DSC和TG对其热性能进行了研究,结果发现这些二胺具有良好的耐热性,是合成一些耐热高聚物的优良原料.     

自动化流动注射停流动力学分析仪的研制及其性能测试

本文研制了一套自动化流动注射停流动力学分析仪，该仪器由苹果Ⅱ型微机通过１２位ＡＤ／ＤＡ卡，流动注射停流控制仪及用ＢＡＳＩＣ语言编制的软件控制泵的起动和停止，试样的输送和混合，数据采集和处理，结果显示和打印，通过以铁（Ⅲ）与硫氰酸盐的反应体系采用固定时间法和以钒（Ｖ）的胶束催化反庆体系采用安始速法的现场测试证明，该仪器具有结构简单，操作方便，恒温性能好，通用性强等特点。     

全氟辛基磺酸酸度函数H0的测定

It is reported in this paper that the acidity function H_0 of perfluorooctanesulfonic acid (POSA) is -12.11±0.03, which was measured first time by ~1H NMR method, in term of the α-H chemical shifts of the acid-ether systems, using 98% to 100% H_2SO_4 as reference standards. This method provides a new procedure for measuring the H_0 value of solid perfluoroalkanesulfonie acid C_nH_(2n+1)SO_3H(n>7).     

Facile cyclic ammonium salt with the smallest size for high performance electric double layer capacitors

A novel cyclic ammonium salt, N,N-dimethylpyrrolidinium tetrafluoroborate (P₁₁-BF₄), was successfully synthesized for the first time. The smallest cyclic structure of P₁₁-BF₄ induced high solubility and conductivity in PC, which can easier enter the micropores of activated carbon and occupy more surface area during charge/discharge process.     

混合价聚十五钒酸盐[V_(15)O_(36)Cl](NH_4)_3Na_7·30H_2O的合成与晶体结构

以XRD法确定制得的标题晶体属空间群D_(3A)~3,a=13.111,c=11.130。结构由帕特逊-极小函数法结合差值法解出,经精修得一致性因子R_w=0.0344。晶胞中坐落在6m2特殊位置上的是包合1个Cl~-的聚十五钒酸根[V_(15)O_(36)Cl]~(10-),配合键价法确认这是四价钒占主导地位的一类特种混合价同多酸根。     

铈杂多配离子-水滑石超分子层柱材料ZnAl-Ce(PMoV)2的插层组装、表征及催化性能

以十四酸根阴离子柱撑Zn-Al水滑石Zn0.77Al0.22(OH)2.0.22C13H27COO.0.81 H2O(记为ZnAl-14A)为预撑前体,在水溶液中用离子交换法将以2∶17缺位杂多酸根离子(P2Mo16VO61)11-记为(P Mo V)为配体的稀土杂多配阴离子Ce(P2Mo16VO61)219-(记为Ce(PMoV)2)插层组装到水滑石层板间,合成了一种具有大的层间距(3.37 nm)的超分子插层材料Zn0.77Al0.23(OH)2.0.0105[Ce(P1.9Mo15.7V1.1O61)2].0.011C13H27COO.0.83H2O(记为ZnAl-Ce(PMoV)2)。用ICP,IR,XRD和DTA对产物的组成和结构进行了表征。结果表明,该产物中Ce(PMoV)2配阴离子沿其长轴垂直于层板的方向分布于水滑石层间;产物具有规整的层状结构和热稳定性;产物对乙酸与正丁醇的酯化反应,二甘醇的脱水-环化反应和H2O2氧化环己烷的反应有良好的催化性能,且易于回收重复使用。     

Synthesis and photoluminescence properties of 8-hydroxyquinoline derivatives and their metallic complexes

Three new 8-hydroxyquinoline derivatives, i.e. 5-[(4-styryl-benzylidene)-amino]-quinolin-8-ol (1), 5-[(4-bromo-2-fluoro-benzylidene)-amino]-quinoline-8-ol (2) and 2-[2-(9-ethyl-9H-carbazol-2yl)-vinyl]-quinolin-8-ol (3), and their metallic complexes were synthesized and identified by ultraviolet-visible (UV-Vis), ¹H nuclear magnetic resonance (¹H NMR), Fourier transform infrared spectrometer (FTIR), mass spectrometry (MS) spectra and elemental analyses. Their fluorescence properties were studied by photoluminescence, which indicated that the luminescence wavelength of 5-and 2-substitued-8-hydroxyquinoline derivatives shifted to red in comparison with that of 8-hydroxyquinoline. Meanwhile, the fluorescence lifetime of 2-[2-(9-ethyl-9H-carbazol-2yl)-vinyl]-quinolin-8-ol and its zinc complex showed long lifetime in benzene solution. __________ Translated from Chinese Journal of Organic Chemistry, 2007, 27(3): 402–408 [译自: 有机化学]