Synthesis and Crystal Structure of N-[1-(4-Chlorophenyl)- 1,4-dihydro-4-oxe-6-methylpyridazine-3-carbonyl]- N'-benzoylhydrazine

1 INTRODUCTION Pyridazinone derivatives represent one of the most active classes of compounds possessing a wide spectrum of biological activity. It was widely used in pharmaceuticals and agrochemicals[1, 2]. Rohm Haas Company had reported that pyridazinones exhibit useful plant growth regulating effects [3,4]. It was also reported that diacylhydrazines exhibit excellent insecticides [5~7]. In view of these facts, it was contemplated to synthesize compounds con- taining both pyridazinone …     

Synthesis and Crystal Structure of 13-Phenyl-1,10- dithia-4,7-dioxa-13-aza-15-Crown-5

1　ＩＮＴＲＯＤＵＣＴＩＯＮＣｒｏｗｎａｎｄａｚａｃｒｏｗｎｅｔｈｅｒｈａｖｅｂｅｅｎｕｓｅｄｗｉｄｅｌｙａｓｈｏｓｔｓｆｏｒｒｅｃｏｇｎｉｚｉｎｇｇｕｅｓｔｍｅｔａｌｉｏｎｓ.[1～ 4] Ｔｈｉａｃｒｏｗｎｅｔｈｅｒｓｉｎｃｏｒｐｏｒａｔｉｎｇｏｎｌｙｓｕｌｆｕｒａｔｏｍｓｉｎｒｉｎｇａｌｓｏｈａｖｅｂｅｅｎｓｔｕｄｉｅｄａｓｅｘｔｒａｃｔｉｎｇｒｅａｇｅｎｔｓｆｏｒｓｏｍｅｓｏｆｔｍｅｔａｌｉｏｎｓ.[5] Ｏｎ ｌｙｆｅｗｓｔｕｄｉｅｓｏｎｍｉｘｅｄ ｄｏｎｏｒｃｒｏｗｎｅｔｈｅｒｃｏｎｔａｉｎ ｉｎｇ…     

On the Mechanism of Condensation between 5—Amino—4,6—dichloro—2—methylpyrimidine and 1—Acetyl—2—imidazolin—2—one

The condensation reaction between 5-amino-4,6-dichloro-2-methylprimidine and 1-acetyl-2-imidazolin-2-one using POCl3 as solvent gave 4,6-dichloro-2-methyl-5-(1-acetyl-tetra-hydro-imidazo-2-ylidene)-aminopyrimidine predominantly and 4,6-dichloro-2-methyl-5-{1-1-(2-oxo-tetrahydro-imidazolyl)]-acetene}-aminopyrimidine as by-product. No 4,6-dichloro-2-methyl-5-(1-acetyl-2-imidazolin-2-yl)-aminopyrimidine was found. The result indicated an esterifi-cation-addition-elimination mechanism.     

2-氨基-4-氯-5-甲基苯磺酸的合成研究

2 氨基 4 氯 5 甲基苯磺酸是合成染料和颜料的重要中间体 ,主要用于合成Ｃ .Ｉ.颜料红等[1] 。目前该产品的合成是以对硝基甲苯为原料 ,经氯化、还原、磺化而成[2 ] 。磺化过程需在压力容器中进行 ,存在成本高 ,溶剂及副产物二氯苯、多氯联苯有毒等问题[3,4] 。为此采用无毒、价廉的汽油和石油醚作为混合溶剂 ,常压下合成 2 氨基 4 氯 5 甲基苯磺酸是本工作的目的。1　实验部分1 .1　主要仪器和药品Ｘ4熔点测定仪 ,日本 2 6 0 5 0型红外光谱仪 ,日本ＬＣ 6Ａ高效液相色谱仪 ,ＪＥＯＬＦＸ 90Ｑ型核磁共振光谱仪 ,美国ＰＥ 2 4 0 0自动元…     

Fe—Ce—N—O,Fe—Y—N—S溶液的热力学研究

本文主要研究了在1570～1650℃范围内Fe-Ce-N-O、Fe-Y-N-S溶液的热力学性质,得到主要结果如下:(1)铈、钇增加氮的溶解度,氧轻微地增加氮的溶解度,硫轻微地减少氮的溶解度;(2)铈、钇、氧、硫与氮的相互作用系数与温度的关系。e_N~(Ce)=(-6230/T) 2.670,e_N~Y=(-6640/T) 2.986,e_N~O=(-3497/T) 1.650,e_N~S=264/T-0.128;(3)铈、钇脱氮产物为CeN、YN;(4)铈、钇脱氮常数与温度的关系:1gK_(CeN)-(-20960/T) 7.972,1gK_(YN)=(-20440/T) 7.863。     

La0.7Sr0.3Co1-xFexO3催化剂氮氧化物储存及抗硫性能

采用溶胶-凝胶法通过在静态空气中700°C焙烧制备了不同Fe掺杂量的La0.7Sr0.3Co1-xFexO3(x=0,0.2,0.6,1.0)系列钙钛矿催化剂.考察了Fe掺杂量对催化剂的结构、氮氧化物储存、抗硫及再生性能的影响.研究结果表明:在La0.7Sr0.3CoO3钙钛矿B位用Fe部分取代Co,可有效提高SrCO3物相的分散,X射线衍射(XRD)结果显示样品中基本为钙钛矿物相.随着Fe掺杂量的增加,催化剂的NOx储存量(NSC)下降.对预硫化样品进行NOx储存测试,发现La0.7Sr0.3CoO3催化剂由于表面沉积了硫酸盐,同时钙钛矿结构也遭到了部分破坏,使得NOx储存量和NO氧化能力均大幅度下降,NOx储存量下降了64.2%,NO-to-NO2转化率从72.8%降至43.4%.掺杂Fe元素后,催化剂的抗硫性能都有不同程度的提高,特别是Fe掺杂量为60%的样品具有最佳的抗硫性能和可再生性能.与新鲜样品相比较,再生后样品的NOx储存量仅下降16.6%,而NO-to-NO2转化率为69.1%,几乎与新鲜样品相同.     

La0.7-xDyxSr0.3MnO3(0.00≤x≤0.30)体系低温磁行为和电阻率的反常

By measuring M-T curves, ρ-T curves and MR-T curves of the samples under different temperatures, the influence of Dy doping (0.00 ≤ x ≤0.30) on the magnetic and electric properties of La0.7-xDyxSr0.3MnO3 has been studied. The experimental results show that, with the increase of the Dy content, the system undergoes a transition from long range ferromagnetic order to the cluster-spin glass state and further to antiferromagnetic order. For the samples with x=0.20 and 0.30, their magnetic behaviors are abnormal at low temperature, and their resistivities at low temperature have a minimum value. These peculiar phenomena not only come from the lattice effect induced by doping, but also from extra magnetic coupling induced by doping.     

Synthesis and Properties of Pr1-xRbxMnO3 (0.05≤x≤0.08) with Perovskite-Type Structure

Rb-substitued Pr_1-xRb_xMnO₃ (0.05≤x≤0.08) was successfully synthesized by solid state reaction. Powder X-ray diffraction showed that all the compounds were orthorhombic with the space group of Pnma. Spin glass behaviors were observed for all the compounds at low temperature, suggesting the competition between ferromagnetic and antiferromagnetic. The temperature dependence of the resistivity for the compound Pr_0.92Rb_0.08MnO_3.02 at 0 and 2 T magnetic field was also investigated. The compound shows semiconducting behavior, and the band gap is 0.3 eV. The maximum magnetoresistance is about 30% at 2 T magnetic field near 116 K.     

低温熔盐法制备球状多孔 La1-xSrxMn0.8Fe0.2O3（0≤x≤0.6）及其催化 CO氧化性能

汽车尾气中 CO, HC, NOx,硫化物及其颗粒粉尘严重危害人们身体健康和大气环境,是大气环境的主要污染源之一.目前,尾气净化是其减排的最主要方式.汽车尾气催化剂的发展经历了几代的研究,一直以来广泛采用 Pt, Pd和 Rh等贵金属,但因其资源匮乏,价格昂贵,容易被 S和 P中毒,因此人们逐渐将目光投向非贵金属催化剂的研发.钙钛矿复合氧化物因具有独特的物理化学性质以及灵活的“化学剪裁”特性而在材料研究等领域颇受青睐,有望成为贵金属催化剂的替代品.一般而言,催化剂的比表面积越大,表面活性位点越多,其催化活性越高,且会明显降低起燃温度.目前,一些制备工艺,如水热法、共沉淀法、微乳液法和硬模板法,虽可在一定程度上提高催化剂的比表面积,但却存在费时、耗能及制备工艺复杂等缺点.因此,如何简单有效地制备出大比表面积的钙钛矿型催化剂依然是一个难题.本文以合成的分级多孔δ-MnO2微球为模板,采用熔盐法制备出球状多孔 La1-xSrxMn0.8Fe0.2O3(0≤x≤0.6)钙钛矿氧化物,研究了球状多孔钙钛矿氧化物的形成过程和合适的制备温度,以及 B位 Fe3+掺杂量为20%时 A位 Sr2+掺杂量对钙钛矿催化剂结构和催化活性的影响.采用 X射线粉末衍射、扫描电子显微镜、透射电子显微镜、N2吸附-脱附、傅里叶红外光谱(FT-IR)和 X射线能谱(XPS)等方法对催化剂进行了表征.在固定床石英管反应器上评价了催化剂催化 CO氧化活性及稳定性,采用气相色谱联接氢火焰离子化检测器检测了产物和反应物的组成.结果表明,以分级多孔δ-MnO2微球为模板,采用熔盐法在450oC反应4 h制备出的球状多孔 La1-xSrxMn0.8Fe0.2O3(0≤x≤0.6)钙钛矿氧化物具有良好的结晶性、较大的比表面积(55.73 m2/g)和孔体积(0.37 cm3/g).其球状多孔结构的形成可分为两个阶段：原位形成钙钛矿相和纳片表面析出钙钛矿晶粒及钙钛矿晶粒的再生长.另外, FT-IR光谱表明, Fe3+和 Sr2+成功进入 A, B位.同时, CO转化曲线表明, B位 Fe3+的掺杂量为20%时, A位 Sr2+的掺杂量高于30%时可以明显改善催化剂催化 CO氧化活性： La1-xSrxMn0.8Fe0.2O3(0≤x≤0.3)的T50和T90分别在180和198oC左右;而 La0.55Sr0.45Mn0.8Fe0.2O3和 La0.4Sr0.6Mn0.8Fe0.2O3的T50均低于125oC; La0.55Sr0.45Mn0.8Fe0.2O3的T90为181oC,而 La0.4Sr0.6Mn0.8Fe0.2O3却仍低于125oC. XPS结果则证明,较高的催化活性得益于 La0.4Sr0.6Mn0.8Fe0.2O3表面存在较多的 Mn4+、氧空位及吸附氧.最后, La0.55Sr0.45Mn0.8Fe0.2O3和 La0.4Sr0.6Mn0.8Fe0.2O3的稳定性测试结果表明,采用熔盐法以δ-MnO2为模板在450oC焙烧4 h制备的多孔球状钙钛矿具有较好的催化稳定性.虽然催化剂制备工艺简单,周期短,但比表面积最大只有55.73 m2/g,为硬模板法的1/2,因此提高比表面积将是今后研究的方向.     

Enhanced magnetoresistance in La0.7Sr0.3MnO3 nanoscaled granular composites

By soft chemical processing, two kinds of nanoscaled lanthanum manganite granular composites, La0.7Sr0.3MnO3/CoFe2O4 (LSMO/CF) and La0.7Sr0.3MnO3 / Nd0.7Sr0.3MnO3 (LSMO/ NSMO), were fabricated. Enhancement in magnetoresistance is observed in both of the composites. Different magnetic compounds, CF and NSMO, embedded in LSMO matrix, result in different temperature ranges where the enhancement occurs. It is considered that the phenomenon is associated with electron tunneling between sorts of grains as well as spin-dependent scattering.     

Gd掺杂对La0.67 Sr0.33 CoO3、La0.67 Sr0.33 MnO3体系磁行为的影响

M~T curves and M~H curves of the systems La0.67Sr0.33CoO3, La0.67Sr0.33MnO3 (x=0.00, 0.05, 0.10, 0.20, 0.30, 0.40, 0.50, 0.60, 0.67) were studied by experiments. Experimental results show that the magnetic structure of La0.67-xGdxSr0.33CoO3 system exhibits the cluster glass state with doping Gd increasing. The M~T curves of samples x>0.10 exhibit a peculiar phenomenon that M value rises sharply at low temperature range. The magnetic structure of La0.67-xGdxSr0.33MnO3 system changes from the long rang ferromagnetic order to the cluster glass state, and anti ferromagnetic state. The M~T curves of samples x≥0.50 decline sharply at low temperature range. The different phenomena shown by the two systems come from different coupling function between Gd and Co, Mn and from spin state transition of Co.     

Effects of isovalent substitution in the manganese sublattice on magnetic, thermal, and structural properties of BiMnO3: BiMn1-xMxO3 (M=Al, Sc, Cr, Fe, Ga; 0<or=x<or=0.2)

Solid solutions BiMn1-xMxO3 with M=Al, Sc, Cr, Fe, and Ga and 0相似文献   

(La1-xREx)2/3Sr1/3MnO3(RE=Y,Sm,Eu,Tb;x=0.1～0.5)的晶体结构及磁性质研究

采用空气中固相反应烧结法制备了一系列钙钛矿结构的(La1-xREx)2/3Sr1/3MnO3(RE=Y,Sm,Eu,Tb;x=0.1～0.5)稀土锰氧化物多晶样品.X射线衍射(XRD)分析表明掺杂RE部分替代La以后,样品的晶体结构为正交结构,空间群为Pbmm.在室温(300K)和液氮温度(77K)下分别测试了样品的磁性质,发现磁性质的改变与RE的掺入量以及RE的离子半径有关.在掺Tb的样品中明显存在巨磁电阻效应,磁场为2 T,温度为300和77 K分别测得(La0.6Tb0.4)2/3Sr1/3MnO3和(La0.7Tb0.3)2/3Sr1/3MnO3的磁电阻(MR)为80%和85%.随着Tb掺杂量的增加,在不同的磁场下,样品电阻-温度关系曲线的峰均向高温方向移动.     

复合阴极材料La1-xSrxCuO3-δ-SDC的制备及电学性能

合成具有单相正交钙钛矿结构的La1-xSrxCuO3-δ(x=0.15, 0.2, 0.3, 0.4)系列样品, 碘量滴定法实验结果表明, 随着Sr掺入量的增加, Cu3+离子的含量逐渐增加. 电学性能研究结果表明, La0.7Sr0.3CuO3-δ电导率最高, 与La0.6Sr0.4CoO3-δ相比, La0.7Sr0.3CuO3-δ具有更好的电化学性能, 可作为一种新的中温固体氧化物燃料电池(IT-SOFC)阴极材料. 将La0.7Sr0.3CuO3-δ与不同质量比的中温电解质Ce0.85Sm0.15O2-δ(SDC) 固相混合, 制备复合阴极材料, 电化学性能测试结果表明, 掺入适量的SDC有利于降低La0.7Sr0.3CuO3-δ电极的极化, 获得性能更优越的IT-SOFC阴极材料, 提高在中温区单电池的输出功率.     

Ionic transport in (La,Sr)CoO3-δ ceramics

Journal of Solid State Electrochemistry - Increasing Sr2+ concentration and the creation of A-site deficiency in La1-x-ySrxCoO3-δ (x = 0.3–0.7, y = 0–0.05)...