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1.
用TG-DTG-DSC热分析技术研究了三(O,O′-二异丙基二硫代磷酸酯)合钴(Ⅲ)、双(O,O′-二乙基二硫代磷酸酯)合镍(Ⅱ)及其后者与吡啶或4-甲基吡啶加合物在氮气气氛中的热行为;用传统的微商法(A-B-S)和积分法(C-R法)以及分别由Malek、Dollimore提出的两种新型的热分析动力学方法协同处理TG数据,获得了四种配合物的热分解反应动力学参数EA,确定了反应机理。对它们的热行为和分子结构之间的关系进行了讨论;并试就本文所用的几种数据处理方法作了比较。  相似文献   

2.
研究了1,10-双(1′-苯基-3′-甲基-5′-氧代吡唑-4-基)癸二酮-[1,10](BPMPDD,H2A)与三苯基氧化膦(TPPO,B)的氯仿溶液从硝酸介质中对Sm(Ⅲ)的协同萃取行为,计算了体系的酸性协萃系数RA和协萃系数R,用斜率法测得协萃合物的组成为SmA·HA·B,计算了协萃平衡常数,用萃取法制得了固态协萃合物,并对其组成、IR及TG-DTA进行了研究  相似文献   

3.
研究了1,9-双(1′-苯基-3′-甲基-5′-氧代吡唑-4′-基)壬二酮-(1,9)(BPMPND,H2A)与三辛基氧膦(TOPO,B)的氯仿溶液,从硝酸介质中对La(Ⅲ),Dy(Ⅲ)的协同萃取,计算了体系的酸性协萃系数RA和协萃系数R,用斜率法测得协萃合物的组成LaA.HA.B和DyA.HA.B计算了协萃取平衡常数,研究了温度对协萃反应的影响,用萃取法制得了固态协萃合物,并对其组成,IR及TG  相似文献   

4.
研究了1,10-双(1′-苯基-3′-甲基-5′-氧代吡唑-4-基)癸二酮-(1,10)(BPMPDD,H2A)与三苯基氧化膦(TPPO,B)的氯仿溶液从硝酸介质中对Sn(Ⅲ)的协同萃取行为,计算了体系的酸性协萃系数RA和协萃系数R,用斜率法测得协萃合物的组成为SmA.HA.B,计算了协萃平衡常数,用萃取法制得了固态协萃合物,并对其组成IR及TG-DTA进行了研究。  相似文献   

5.
Yb(ClO4)3-BAPHDCA-H2O的相平衡研究及其三元化合物的制备   总被引:2,自引:1,他引:1  
用相平衡法研究了三元体系Yb(ClO4)3-BAPHDCA-H2O(BAPHDCA,N,N-二安替比林-1,6-己二酰胺)在30℃时的相平衡,结果表明,体系中形成了未风物固液异组成三元化合物Yb(BAPHDA)2(ClO4)·4H2O。在相平衡结果的指导下制备了该化合物,并通过化学分析、元素分析、IR光谱,TG-DTG及X射线粉末射分析等对其进行了表征。  相似文献   

6.
本文用ASED-MO法研究了O,O′-2,2′-联苯基,S-苄基二硫代磷酸酯单个分子的构象,得到4种低能构象。分析了常温下4种构象的分布,稳定构象之间的转化以及与晶态分子构象之间的关系.  相似文献   

7.
HYDROLYTICCLEAVAGEOFACMET-GLYPROMOTEDBYCIS-[Pd(MET)(D2O)2](NO3)2¥XiaoHuaCHEN;LongGenZHU;N.M.Kostic(CoordinationChemistryInsti...  相似文献   

8.
A HIGHLY EFFICIENT SYNTHESTS OF (2E)-α,β-UNSATURATED AMIDES¥JinXingDU;XianHUANG(DepartmeotofChemistry,ZhejiangNormalUniversit...  相似文献   

9.
测定了三元体系La(ClO4)3-OCBAAP-H2O在30℃时的溶解度.结果表明,该体系有一个新固相(不一致溶解化合物)La(OCBAAP)4(ClO4)3·6H2O形成.参考该体系溶度图确定合成条件,合成了系列化合物Ln(OCBAAP)4(ClO4)3·nH2O(Ln=La,n=6;Ln=Pr,Nd,Sm,Gd,Yb,n=2).通过化学分析、元素分析、TG-DTG、IR和密度对化合物进行了表征,计算了La(OCBAAP)4(ClO4)3热分解过程各阶段的表观活化能.  相似文献   

10.
利用酯基锡与缺位Keggin结构杂多阴离子PW9O9-34反应,合成了6种新的杂多阴离子有机金属配合物M9[(R′OOCCHR″CH2SnOH2)3(PW9O34)2]·xH2O(M=(CH3)4N+,K+;R′=CH3_,CH3CH2_;R″=H,CH3_),通过元素分析、IR光谱、紫外电子光谱、1HNMR、31PNMP、183WNMR和TGA-DSC热分析等测试手段对标题配合物进行了表征和性质研究,确定该系列配合物为A-β-PW9型夹心配合物结构.  相似文献   

11.
Summary Tetrakisisopropoxytantalum(V) alkylene dithiophosphato complexes, (G=–CMe2CMe2–, –CHMeCHMe–, –CH2CMe2CH2– and –CH2CEt2CH2–) have been prepared from equimolar ratios of tantalum(V) isopropoxide and alkylene dithiophosphoric acids in benzene. These moisture-sensitive compounds, which are soluble in common organic solvents and are monomeric, have been characterized by elemental analysis, molecular weight determinations and by their i.r. and n.m.r. spectra. An octahedral geometry is suggested in which the ligand is bidentate.  相似文献   

12.
The synthesis of novel dithiophosphate derivatives has been achieved. Two O,O′-alkanediyl S-(N-phthalimidomethyl) dithiophosphates and two Zinc bis(O,O′-alkanediyl) dithiophosphates are synthesized by an easy and facile chemical synthetic route. Zinc bis[O,O′-(2-methylpentane-2,4-diyl) dithiophosphate] L1, Zinc bis[O,O′-(2-ethylhexane-1,3-diyl) dithiophosphate] L2, O,O′-(2-methylpentane-2,4-diyl) S-(N-phthalimidomethyl) dithiophosphate L3 and O,O′-(2-ethylhexane-1,3-diyl) S-(N-phthalimidomethyl) dithiophosphate L4 are synthesized from the respective ammonium salts. Compounds L1, L2, L3, and L4 are characterized by (CHN) elemental analysis, ESI mass, FT-IR, 1H, 13C, and 31P NMR techniques. The crystal structure of ammonium O,O′-(2-methylpentane-2,4-diyl) dithiophosphate is discussed. L1, L2, L3, and L4 were evaluated for antimicrobial activity. It was found that the phthalimide derivatives L3 and L4 showed much better antifungal potential against some species of fungus. The Zinc dithiophosphates L1 and L2 showed good antibacterial activity against Bacillus cereus and Escherichia coli.  相似文献   

13.
Abstract

Preparation and isolation of the polynuclear copper(II) complex, {[Cu(bipy)(maleato)] · 2H2O} n , was accomplished by reaction of an aqueous solution containing sodium maleate and an ethanolic solution of Cu(NO3)2·4H2O and bipy. The crystal structure of the title complex was determined by single-crystal X-ray methods. The structure consists of one-dimensional infinite chains. The copper atom is five-coordinate and presents a square-pyramidal coordination sphere, which consists of the two imine N atoms of bipy and two terminal carboxylate O atoms of a maleate2- ligand in the basal plane with Cu-N bond distances of 2.016(3) and 1.987(3) A and Cu-O distances of 1.909(2) and 1.947(2) Å, respectively. In the apical site an O atom of the maleate2- ligand from an adjacent complex coordinates to copper (2.264(2) Å). The coordination fashion of the maleato ligand is also confirmed by the IR spectrum.  相似文献   

14.
Four new nickel and copper complexes [ML{SSP(OC10H7-1)2}2], where M=Ni(Ⅱ), Cu(Ⅱ); L=5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene(hmtade) or 5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane(hmta); SSP(OC10H7-1)2=O,O′-bis(1-naphthy)dithiophosphate, were synthesized and characterized by elemental analysis, molar conductivity, infrared spectra, electronic spectra and TG-DTA thermal analysis. The complexes are non-electrolytes in DMSO. O,O′-bis(1-naphthyl) dithiophosphate ligand that behaves in monodentate fashion coordinates to metal ion.  相似文献   

15.
16.
17.
Summary Equimolar adducts of mononuclear oxomolybdenum(IV)O,O-dialkyl and alkylene dithiophosphates with heterocyclic amines, MoO[S2P(OR)2]2·L (where when R=Et,i-Bu; L=pyridine and when R=Et,n-Pr,i-Bu; L=2,2-bipyridyl, 1,10-phenanthroline) and (where G=CH2CMe2CH2, L=2,2-bipyridyl and when G=CMe2CMe2; L=pyridine) have been prepared by reacting the corresponding oxomolybdenum(IV) complexes with an excess of pyridine or with bipyridyl or phenanthroline in a 11 molar ratio.The complexes have been characterized by elemental analyses and molecular weight determinations. Their probable structures are proposed on the basis of i.r. and n.m.r. (1H,13C and31P) spectral data, which are consistent with a 6-coordinated octahedral structure for all the base adduct complexes.  相似文献   

18.
Summary Triisopropoxy bis(O,O-dialkyl dithiophosphates), (i-PrO)3M[S2P(OR)2]2 (M = Nbv, Tav; R = n-Pr, i-Pr, i-Bu and Ph) have been prepared by reacting the appropriate triisopropoxymetal(V)dichloride, (i-PrO)3MCl2 (1 mol) with sodium/ammonium dialkyl dithiophosphates (2 mols)in THF. The monomeric products which are viscous liquids, soluble in common organic solvents and highly susceptible to hydrolysis, were characterized by i.r. and n.m.r. spectra which indicate a bidentate mode of attachment of dithiophosphato groups to the metal.  相似文献   

19.
Abstract

A mixed ligand europium complex, [Eu(BA)3dmbpy]2, has been prepared, where BA = benzoate and dmbpy = 4, 4′-dimethyl-2, 2′-bipyridine. The complex crystallizes in the tri-clinic system, space group P ? 1. Its structure has been determined using X-ray diffraction methods. The two europium ions in the molecule are held together by four carboxylate groups of benzoic acid and each europium ion is further bonded to one bidentate carboxylate group and one 4, 4′-dimethyl-2, 2′-bipyridine molecule. Excitation and luminescence spectra observed at 77 K show that the europium site in the crystal has low symmetry and changes of the chemical surroundings of the europium ion in the molecule depend mainly on the flexibility of 4, 4′-dime-thyl-2, 2′-bibyridine.  相似文献   

20.
《合成通讯》2013,43(11):1715-1719
Stereoisomeric mixtures of 2- and 4-alkyl-cyclohexanols form complex with O,O′-dibenzoyl-(2R,3R)-tartaric acid. The diastereoisomer complex formation can be used for isomer and enatiomer separation as it is trans- and enantioselective in the case of 2-alkyl-cyclohexanols and trans-selective in the case of 4-alkyl-cyclohexanols.  相似文献   

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