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Sm(NO_3)_3·6H_2O热分解过程的研究工作虽有文献报道,但结果不尽相同。文献[2]不同于文献[1,3],认为分解过程中存在无水盐阶段;文献[3]不同于文献[1,2],认为分解过程中存在低水合物。而且文献尚缺低水合物热分解机理的报道。我们也曾做过一些工作,但脱水阶段也不详尽。为此,我们详细地研究了Sm(NO_3)_3·nH_2O(n= 相似文献
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稀土配合物能使极性和非极性单体聚合[1] .虽然目前已测定了几乎所有的三 (环戊二烯基 )稀土配合物及部分三 (取代环戊二烯基 )稀土配合物的晶体结构 ,但有关三 (茚基 )稀土配合物的报道较少 .第一个三 (茚基 )稀土配合物是无水三氯化稀土与 3倍物质的量的茚基钠 C9H7Na在四氢呋喃中反应而得 ,但未报道其晶体结构[2 ] .后来用同样的反应却分离出以氯为桥的二聚体离子对配合物[Na( THF) 6][Ln( η5- C9H7) 3μ( Cl) Ln( η5- C9H7) 3]( Ln=Nd,Sm) [3] .无水三氯化稀土与 Mg( C9H7) 2 或C9H7K等物质的量反应则生成非溶剂化的 ( C9H7… 相似文献
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稀土配合物能使极性和非极性单体聚合[1].虽然目前已测定了几乎所有的三(环戊二烯基)稀土配合物及部分三(取代环戊二烯基)稀土配合物的晶体结构, 但有关三(茚基)稀土配合物的报道较少. 第一个三(茚基)稀土配合物是无水三氯化稀土与3倍物质的量的茚基钠C9H7Na在四氢呋喃中反应而得, 但未报道其晶体结构 [2]. 后来用同样的反应却分离出以氯为桥的二聚体离子对配合物 [Na(THF)6] [Ln(η5-C9H7)3μ(Cl)Ln(η5-C9H7)3](Ln=Nd, Sm) [3]. 无水三氯化稀土与Mg(C9H7)2或C9H7K等物质的量反应则生成非溶剂化的(C9H7)3Sm[4], 而与茚基钠和环辛四烯钾(C8H8K)以1∶2∶1物质的量比反应时, 则得到(C9H7)3Ln(THF)(Ln=Nd, Gd) [5]. Bottomley [6]曾用(C9Me7)K(七甲基茚基钾)与LnCl3(物质的量比3∶1)反应制备(C9Me7)3Nd(THF)5和(C9Me7)3Er@(THF)3, 但未报道晶体结构. 因为取代茚的空间阻碍比茚的大, 三(取代茚基)稀土配合物较难合成. 迄今未见有关单晶结构报道. 本文首次报道三(环戊基茚基)钐配合物的合成及晶体结构. 相似文献
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近年来 ,有许多文献报道茂金属催化剂的负载化及其在烯烃聚合中的应用 ,这对发展新型茂金属催化剂和开发新型高分子材料有重要意义 [1,2 ] .我们 [3]曾报道壳聚糖负载稀土催化剂用于甲基丙烯酸甲酯的配位聚合有优良性能 .以五甲基环戊二烯为配体的有机稀土配合物 ,如 [Sm H( C5Me5) ]2 ,[C5Me5]Ln Me( THF) ( Ln=Sm,Yb)等在甲苯中单组分引发甲基丙烯酸甲酯聚合及内酯开环聚合具有许多优异性能[4 ,5] ,但是经负载化的该类催化剂的聚合性能尚未见报道 .本文报道将 [C5Me5]2 Sm Me·( THF)负载于二氧化硅 ,引发甲基丙烯酸甲酯聚合的结… 相似文献
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Reactions of SmI2 in THF with ArSSAr produced two binuclear samarium thiolate complexes [(THF)3I2- Sm(μ-SAr)]2 [Ar=Ph (1), 4-Me2NC6H4 (2)] in high yields. The structure of 2 was characterized by single crystal X-ray crystallography. The crystal of 2 belongs to the triclinic system with space group P 1 and a=0.95705(13) nm, b= 1.22287(14) nm, c= 1.26450(14) nm, a=64.194(11)°, B=78.491(13)°, y=76.176(12)°, V= 1.2860(3) nm^3, Z= 1,μ=4.783 mm^-1, Dc= 1.964 Mg/m^3, M= 1521.19, S= 1.046, R1=0.0358, wR2=0.0910. X-ray analysis revealed that 2 is a thiolate-bridged dimer in which each Sm atom adopts a distorted pentagonal bipyramidal coordi- nation geometry. 相似文献
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Samarium diiodide (SmI2) was found to be an efficient catalyst for the condensation of o-phenylenediamine and ketones to afford the corresponding 2,3-dihydro-1H-benzo[b][1,4]-diazepines in moderate to excellent yields under very mild and solvent-free conditions. The real active species here was suggested to be a Sin(Ⅲ) intermediate formed in situ and the mechanism of the present reaction was proposed. 相似文献
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SmCl3-CaCl2-LiCl体系相图的研究 总被引:5,自引:0,他引:5
利用DTA研究了SmCl3-CaCl2-LiCl三元体系的相图。发现该体系有对应SmCl3,CaCl2, LiCl, 2SmCl3·LiCl的四个液相面、五条两次结晶线、一个三元低共熔点E[23.0(mol%)SmCl3, 19.5(mol%)CaCl2, 282℃]、一个三元转熔点P[28.5(mol%)SmCl3,22.0(mol%)CaCl2, 370℃]。 相似文献
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稀土离子在生物体内有特殊作用,氨基酸是体内蛋白质的结构单元。因此,研究稀土氨基酸配合物有重要意义。相平衡的研究可为配合物的制备提供理论依据。有关稀土-氨基酸-水三元体系的报道甚少,而且多为稀土的高氯酸盐和盐酸盐。本文采用相平衡手段研究了标题体系在35℃时的溶解度性质,得到相应溶度图和饱和溶液折光率-组成曲线。1 实验部分1.1 主要试剂和议器 Sm(NO_3)_3·nH_2O按文献[3]制备;DL-α-Alanine为生化试剂( 相似文献
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A complex of samarium with glymine, [Sm(Gly)2Cl3·3H2O], was synthesized and characterized by DSC, TG and DTG. A possible mechanism of thermal decomposition of this complex was suggested. The heat capacities of the complex were measured by a precision adiabatic calorimeter over the temperature range from 82 to 375 K. The solution enthalpies of reactants [SmCl3·6H2O+2Gly] and the products [Sm(Gly)2Cl3·3H2O+3H2O] were determined by an isoperibel solution- reaction calorimeter at 298.15 K, respectively; the standard molar enthalpy of formation of [Sm(Gly)2Cl3·3H2O] was calculated through a designed thermochemical cycle. 相似文献
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Luminescence of Nanosized Supramolecular Material of Mesoporous Molecular Sieve and Samarium (Ⅲ) Complex 总被引:2,自引:0,他引:2
YIN Wei ZHANG Mai-sheng ** School of Chemistry Chemical Engineering Sun Yat-sen 《高等学校化学研究》2003,19(4):504-507
IntroductionThe synthesis of mesoporous silica has greatlyexpanded the possibilities for the design of the porestructure materials[1] . Because of their large sur-face areas and porosity,these materials have greatpotential application in environmental and industri-al fields.A greatmany significant advanced resultshave been achieved in this field including the syn-theses of the related materials[2— 4] ,the develop-ment of the novel properties[5— 8] ,the discovery ofnew theories on synthetic c… 相似文献
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Nonisothermal Kinetics of Dehydration Process of [Sm(m-CIBA)3phen]2·2H2O and [Sm(p-CIBA)3phen]2·2H2O
REN Ning ;WANG Xi-e ;ZHANG Jie ;ZHANG Jian-jun ;XU Su-ling ;ZHANG Hai-yan 《高等学校化学研究》2008,24(2):210-214
Compounds [Sm(m-CIBA)3phen]2.2H20 and [Sm(p-CIBA)3phen]2·2H20(m-CIBA=m-chlorobenzoate, pClBA=p-chlorobenzoate, phen=l,10-phenanthroline) were prepared. The dehydration processes and kinetics of these compounds were studied from the analysis of the DSC curves using a method of processing the data of thermal analysis kinetics. The Arrhenius equation for the dehydration process can be expressed as lnk=-38.65-243.90×l0^3/RT for [Sm(m-CIBA)3phen]2·2H2O, and lnk=38.70-172.22×103/RT for [Sm(p-CIBA)3phen]2·2H2O. The values of △H^1, △G^1, and △S^1 of dehydration reaction for the title comnonnds are determined respectively. 相似文献
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A new unsymmetrical Schiff base zwitterion (Ⅲ) was synthesized using L-lysine, salicylaldehyde and 2-hydroxy-l-naphthaldehyde. Samarium(Ⅲ) complex of this ligand [SmL(NO3)]NO3·2H2O has been prepared and characterized by elemental analyses, IR, UV and molar conductance. The thermal decomposition kinetics of the complex for the second stage was studied under non-isothermal condition by TG and DTG methods. The kinetic equation may be expressed as dα/dt=3/2Ae^E/RT(1-α)^2/3[1-(1 -α)^1/3)]^-1. The kinetic parameters (E, A), activation entropy △S^x and activation free-energy △G^x were also gained. 相似文献
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The complex [Sm(p-MBA)3phen]2 (p-MBA, p-methylbenzoate; phen, 1,10-phenanthroline) was prepared and characterized by elemental analysis, IR and UV spectra. The thermal decomposition process of [Sm(pMBA)3phen]2 was studied under a static air atmosphere by TG-DTG and IR techniques. Thermal decomposition kinetics was investigated employing a newly proposed method, together with the integral isoconversional non-finear method. Meanwhile, the thermodynamic parameters (AH#, △G# and AS#) were also calculated. The lifetime equation at mass-loss of 10% was deduced as In r=-24.7825+ 18070.43/T by isothermal thermogravimetric analysis. 相似文献
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本文采用正丁醇与水的混合溶剂合成一种新的以有机胺为模板剂的硫酸钐盐:[C2N2H10]1.5[Sm(SO4)3(H2O)].2H2O(1),并通过X-射线衍射、红外、热重及元素分析对其进行了表征。该化合物晶体属于单斜晶系,P21/c空间群。其中a=0.65515(9)nm,b=2.648 3(4)nm,c=0.996 15(13)nm,β=104.067 0(10)°,V=1.676 5(4)nm3,Z=4。晶体结构分析显示化合物1中的波浪形层状结构由SmO9多面体与SO4多面体构成,同时非配位水与乙二胺通过氢键连接相邻的两个层。化合物1具有较强的荧光。 相似文献
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报道了二价配合物(CH3C5H4)2Sm(THF)和SmI2(THF)x与异氰酸苯酯的反应. (CH3C5H4)2Sm(THF)和异氰酸苯酯反应生成配合物[(CH3C5H4)2(THF)Sm]2[μ-η4-(PhN)OCCO(NPh)]*2THF(1), 而SmI2(THF)x则被异氰酸苯酯氧化为[SmI2(THF)5][SmI4(THF)2]. (CH3C5H4)2Sm(THF)和配合物1都能催化异氰酸苯酯的齐聚反应.(CH3C5H4)2Sm(THF)和异氰酸苯酯作用生成配合物1的反应可以认为是 (CH3C5H4)2Sm(THF)催化异氰酸苯酯齐聚的引发反应, 而配合物1是该齐聚反应的活性中间体. X射线衍射分析表明, 配合物1是一个由草酰胺双负离子桥联的双金属化合物. 相似文献
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4β-氨基-4脱氧鬼臼毒素和4β-氨基-4脱氧-4'-去甲基鬼臼毒素的两种新合成方法 总被引:2,自引:0,他引:2
我们在研究抗肿瘤活性物质的基础上[1~ 5 ],注意到鬼臼类化合物具有抗癌活性 ,但其毒副作用较大 ,我们对其结构进行了改造 ,以研制活性更高而毒性更小的新的衍生物 .从以前有关鬼臼毒素及其类似物的构效关系研究中已得出以下几个方面的结构要求是保持其抗癌活性必须具备的条件 :(a)在4’ 位有一个酚羟基 ;(b)C 4取代基位是 β构型 ;(c)具有反式内酯环[6 ].研究表明 ,4 β 酰胺基的鬼臼衍生物具有较强的抗癌活性[7].而 4 β 氨基 4脱氧鬼臼毒素和 4 β 氨基 4脱氧 4’去甲基鬼臼毒素是合成此类衍生物的最重要中间体 .合成这两个化合物的… 相似文献
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以N,N'-二甲基乙酰胺为杂化配体,合成了稀土-铁氰根桥联配合物,测定了其中三个配合物的晶体结构和磁学性质,([SmFe)~n,Gd~2Fe,HoFe)。结果发现在相同的反应条件的一个系列中,呈现三种截然不同的晶体结构,分别为一维链状结构,三核结构和双核结构。同时发现这些配合物具有优良的磁化学性质,特别是[SmFe]~n呈现长程磁有序,临界温度(T~c=3.5K)和较大的矫顽力(H~c=1400Oe)。 相似文献