Synthesis, crystal structure and properties of (Z)-3-triphenylstannyl-1,1-diphenyl propenol

Five new organotin compounds were synthesized and characterized, X-ray crystal structure analysis of (Z)-3-triphenylstannyl-1,1-diphenyl propenol was performed, The crystal belongs to space group P2(1)/n. The cell parameters are: a = 1.235 7(2) nm, b = 0.987 4(2) nm, c = 2.208 1(4) nm, beta = 95.23(3)degrees, V = 2.683 0(9) nm(3), Z = 4, R = 0.027 9, R-w = 0.064 5. The tin atom of the molecule exists in a distorted tetrahedron, Z isomer of double bond is obtained.

Synthesis and imidization of poly(amic methyl ester)s

The synthesis and characterization of a series of poly(amic methyl ester)s from five aromatic dianhydrides and a diamine, 4,4'-oxydianiline (ODA), are described. These poly(amic ester)s are obtained by the low-temperature polycondensation from dianhydrides derived diester-diacyl chlorides and ODA in DMAc solution with the inherent viscosities in the 0.5-0.9 dL/g range. These precursors are readily soluble in aprotic solvents. A detailed thermal study of the imidization process is presented, based on dynamic and isothermal TGA measurements, FTIR spectroscopy, and dynamic mechanical analysis. (C) 1997 John Wiley & Sons, Inc.

复合氧化物La_(2-x)(Sr,Th)_xCuO_(4±λ)——一种新型的苯酚羟化催化剂

二酚(邻苯二酚,对苯二酚)是重要的化工原料,二酚生产一直是人们所关注的课题,70年代以前主要采用的一些污染严重的生产过程正被逐渐淘汰。目前,利用过氧化氢和苯酚为原料联产邻苯二酚和对苯二酚,在化工生产中占有重要的地位。常见的催化剂有等。但这些催化剂也具有明显的不足之处,前两者具有均相催化反应本身难以克服的缺点,后者虽具有多相催化过程的优点,但由于此类催化剂难以制取,而且此类催化剂主要反应孔道的孔径较小(<0.9 nm),反应物和生成物难以在孔道中扩散,使得反应速度较慢。当前国际上还正在积极寻找新的催化体系以达到高效无污染生产二酚的目的。

Ionic conductivity of polymer gel electrolytes based on poly(polyethylene glycol dimethacrylate)

Gel electrolytes have been prepared by thermal polymerization of poly(polyethylene glycol dimethacrylate) (P(PEGD)) in the presence of propylene carbonate (PC) and alkali metal salts, such as LiClO4, LICF(3)SO(3) and LiBF4. The conductivity was studied by means of impedance spectroscopy, and it is found that the temperature dependence of conductivities follow a Arrhenius relationship when the molar percentage of PC is higher than 75% or LiClO4 concentration is lower than 0.9 mol/l. However, when LiCF3SO3 or LiBF4 is used instead of LiClO4 as the salt, the situation is different. For LICF(3)SO(3), the Arrhenius relationship almost holds true for all the salt concentrations studied; while for LiBF4, the Arrhenius equation hardly fits for any salt concentration. The dependence of activation energy on salt concentration is also examined, both for LiClO4 and LiCF3SO3, the values of E(a) tend to reach a minimum value with increasing salt concentration. Copyright (C) 1996 Elsevier Science Ltd.

Li_8SiN_4-Li_3N-BN体系中立方BN转化行为的研究

研究了高温高压下x·Li_8SiN_4-0.1(1-x)·Li_3N-0.9(1-x)·BN体系中立方氮化硼(cBN)的转化行为。Li_8SiN_4的存在可显著改善cBN晶体的发育,提高晶体质量。在4.2～5.5GPa,1340～1750℃范围内确定了x=4.8％时体系的cBN转化区,并对转化区内cBN转化率、平均生长速度、成核速度及破碎强度与转化温度和压力的关系进行了研究。

DETERMINATION OF AMINOPYRINE AND ITS METABOLITE BY CAPILLARY ELECTROPHORESIS ELECTROCHEMICAL DETECTION

An electrochemical pretreatment regime for a cylindrical carbon fibre microelectrode was optimized for the determination of aminopyrine (AM) and its metabolite 4-aminoantipyrine (AAN) by capillary electrophoresis (CE)-electrochemical detection (ED). Under optimized conditions, a response of high sensitivity and stability was obtained for AM and AAN at a detection voltage as low as 0.9 V following CE-ED, by which AM and AAN were separated satisfactorily. The calibration graph was linear over three orders of magnitude and the limits of detection for AM and AAN were in the femtomole range.

A STUDY OF CATALYTIC PROPERTIES OF PEROVSKITE-TYPE OXIDES LAMNYCO1-YO3 .1. THE RELATIONSHIP BETWEEN THE TYPE OF OXYGEN SPECIES AND THE CATALYTIC PROPERTY IN AMMONIA OXIDATION

The type of oxygen species in perovskite-type oxides LaMnyCo1-yO3 (y = 0.0, 0.1, 0.3, 0.5, 0.7, 0.9, 1.0) has been studied by means of XRD, XPS and TPD. The catalytic activity in ammonia oxidation was also investigated. It was found that there were three desorption peaks in TPD curve corresponding to three types of oxygen species (alpha, beta, beta'). The desorption temperatures were 293 K less-than-or-equal-to T(alpha) less-than-or-equal-to 773 K, 773 K less-than-or-equal-to T(beta) less-than-or-equal-to K and T(beta') greater-than-or-equal-to 1073 K respectively. The relationship among the composition, structure and the catalytic property of.the catalyst was correlated and could be explainned with a model based on solid defect reaction and the interaction between Co and Mn ions. The adsorption strength and quantity of a oxygen are proportional to the catalytic activity. The, result indicates that the synergetic effect between B-site ions seems to the benefit of the ammonis oxidation reaction.

Li-Ni-La-O系复合氧化物催化剂上甲烷氧化偶联的研究

考察了Li-Ni-La-O系催化剂的组成、结构及反应条件对甲烷氧化偶联反应活性的影响.在780℃、CH_4:O_2:N_2=2:1:7、空速15000h~(-1)时,C_2烃收率可达25.8％.XRD、IR、XPS及SEM等的结构分析表明,在LiLa_(1-x)Ni_xO_2催化剂中,当0.1≤x≤0.9时,该催化剂由LiNiO_2和LaNi_(1-y)Li_yO_(4-λ)两相组成,x<0.3时出现了LiLaO_2相,La_2Ni_(1-y)Li_yO_(4-λ)是甲烷氧化偶联的主要活性相,活性位Li~+-O~--Ni~(2+)数量的增加是活性提高的主要原因.LiNiO_2和LiLaO_2也有催化活性,它们与La_2Ni_(1-y)Li_yO_4间的协同作用也可能是催化活性增强的原因.

YVO_4∶RE~(3+)(RE∶Pr、Sm、Tb、Es、Dy)晶体的研究

本文探讨了助熔剂法生长 YVO_4:RE~(3+)(RE:Pr,Sm,Tb,Er,Dy)晶体的工艺。讨论了助熔剂 V_2O_5,Pb_2P_2O_7和温度对晶体生长习性和缺陷的影响。测定了晶体的结构参数和光谱。Y_(0.9)Sm_(0.1)VO_4和 Y_(0.95)Dy_(0.05)VO_4晶体具有很好的光谱特性。

ELECTROCHEMICAL-BEHAVIOR OF YTTRIUM ION IN LICL-KCL-NACL EUTECTIC MELT

The electrochemical reduction of yttrium ion on a molybdenum electrode in a LiCl-KCl-NaCl eutectic melt at 723 K was found to be almost reversible and to proceed by a one-step three electron reaction. The diffusion coefficient D of the Y(III) ion was measured to be (3.3 +/- 0.4) x 10(-6) cm2 s-1 by cyclic voltammetry, (5.0 +/- 0.9) x 10(-6) cm2 s-1 by the rotating disk electrode method, and (7.1 +/- 0.7) x 10(-6) cm2 s-1 by chronopotentiometry. The D values obtained by the latter two methods are in fairly good agreement with each other. The rather low D value obtained by cyclic voltammetry might be attributed to the fact that yttrium metal can dissolve slightly in the chloride melt. The standard potential of Y(III)/Y(0) couple was determined to be (-3.174 +/- 0.006) V (vs. Cl2/Cl-) by open-circuit potentiometry, (-3.15 +/- 0.02) V (vs. Cl2/Cl-) by the rotating disk electrode method and (-3.16 +/- 0.02) V (vs. Cl2/Cl) by chronopotentiometry. These three values are in good agreement with each other. Several types of Ni-Y intermetallic compounds were found to be formed on a nickel electrode.

红外变可见上转换材料薄膜的研制

上转换材料是一种能将看不见的红外光变为可见光的一种新型功能材料,其能将几个红外光子合并成一个可见光子、也称为多光子材料。这种反Stokes发光材料具有重要的理论意义和实用价值,为此,自1966年Auzel提出以后就引起人们的重视,近年来又有许多新的报导。不同的上转换材料能将红外光转变成红、绿或兰等颜色可见光,由于绿光处于视觉函数的峰值部份,且一般发绿光的上转换材料相对强度较好,因此研究与应用较多。国内外曾将红外变可见上转换材料用于固体灯,而我们首先将其用于Nd~(3+)激光和0.9μm半导体激光显示,已取得良好的效果,并作为某些激光器的配件。目前所使用的上转换材料显示片是将上转换材料涂在铝片或玻璃片上,铝片不能透光限制了它的应用,而玻璃片易碎和容易脱

合成食用色素柠檬黄选择性电极的研制和应用

本文研究了以十二烷基三庚基碘化铵-柠檬黄缔合物为活性材料的PVC膜电极和涂丝电极,两电极对柠檬黄浓度在1.0×10~(-6)～1.0×10~(-3)mol/L间的响应符合Nernst关系式,斜率为20.0±1.0mV/PC(22℃),pH范围为4.0～9.4,电极的选择性、重现性和稳定性良好。对样品的测定结果与分光光度法测定结果基本一致。该方法简便、准确、可靠。

在镍系钙钛矿(ABO_3)型催化剂上的氨氧化 Ⅲ.焙烧温度对催化剂结构和活性的影响

本文探讨了焙烧温度对催化剂结构及氨氧化活性的影响。得出:La_(0.9)Sr_(0.1)NiO_(3-λ)在1223K后分解,生成具有K_2NiF_4结构的La_2NiO_4相,NiO相和LaNiO_3相。催化活性相主要是具有钙钛矿结构的组分。最佳活性相在1273K形成。

LnVO_4:Eu发光中有关的化学因素

本文讨论了LnVO_4:Eu(Ln_(0.9)Eu_(0.1)VO_4,Ln=La~(3+)、Gd~(3+)、Y~(3+)、Sc'+和Lu_(3+))多晶粉末中Eu~(3+)离子~5D_0→~7F_2电偶跃迁(618.4nm)发光与化学组成、晶体结构和R—O键强之间的变化规律。

La_xBa_(1-x)SnO_3的敏感性质

本文介绍自行合成的LaxBa_(1-x)SnO_3(x=0～0.2)的结构、电学性质、温敏性质和气敏性质,其结构均为立方晶体,晶胞参数随镧含量的增加而减少.La_(0.1)Ba_(0.9)SnO_3在室温至600℃温区内,电阻随温度升高而线性下降,有可能用作温敏元件.当La_(0.1)Ba_(0.9)SnO_3作成旁热式气敏元件时,有可能用于(10～10000)10~(-6)乙醇蒸汽的检测,而不受煤气、液化汽、汽油和烟的干扰.