有机锗化合物中碳氢的快速测定

报道了用Co3O4 作覆盖氧化剂分析有机锗化合物中碳氢元素的方法。通过对 9个样品的十几次分析 ,碳、氢的相对误差分别小于± 1.30 % ,4 .4 0 %。方法简便 ,结果稳定可靠 ,可用于含锗有机化合物的碳氢分析。     

聚2,3—二硫代吩噻嗪的电流变性质研究

聚２，３－二硫代吩噻嗪的电流变性质研究肖深初（湖南化工研究院长沙４１０００７）林源斌申东升王安民朱礼仁（湘潭大学化学系湘潭４１１１０５）关键词电流变流体电流变性质有机半导体中图分类号Ｏ６３１．２１电流变学（Ｅｌｅｃｔｒｏｒｈｅｏｌｏｇｙ）是研究在电场...     

Studies of ABS-graft-maleic anhydride/clay nanocomposites: Morphologies, thermal stability and flammability properties

ABS-g-MAH (maleic anhydride) with different grafting degree, ABS/OMT (organo montmorillonite) and ABS-g-MAH/OMT nanocomposites were prepared via melt blending. The grafting reaction, phase morphology, clay dispersion, thermal properties, dynamic mechanical properties and flammability properties were investigated. FTIR spectra results indicate that maleic anhydride was successfully grafted onto butadiene chains of the ABS backbone in the molten state using dicumyl peroxide as the initiator and styrene as the comonomer and the relative grafting degree increased with increasing loading of MAH. TEM images show the size of the dispersed rubber domains of ABS-g-MAH increased and the dispersion is more uniform than that of neat ABS resin. XRD and TEM results show that intercalated/exfoliated structure formed in ABS-g-MAH/OMT nanocomposites and the rubber phase intercalated into clay layers distributed in both SAN phase and rubber phase. TGA results reveal the intercalated/exfoliated structure of ABS-g-MAH/OMT nanocomposites has better barrier properties and thermal stability than intercalated ones of ABS/OMT nanocomposites. The T_g of ABS-g-MAH/OMT nanocomposites was also higher than that of neat ABS/OMT nanocomposites. The results of cone measurements show that ABS-g-MAH/OMT nanocomposites exhibit significantly reduced flammability when compared to ABS/OMT nanocomposites even at the same clay content. The chars of ABS-g-MAH/OMT nanocomposites were tighter, denser, more integrated and fewer surface microcracks than ABS/OMT residues.     

Proline catalyzed two-component, three-component and self-asymmetric Mannich reactions promoted by ultrasonic conditions

The proline catalyzed two-component and three-component asymmetric Mannich reaction with hydroxyacetone and self-Mannich reaction with propanal were performed successfully under ultrasonic conditions in 1 h to afford Mannich products in 90-98% isolated yields and 81-99% ees with excellent diastereoselectivities.     

A fluoroaryl substituent with spectator function: Reactivity and structures of cyclic and acyclic HF4C6-substituted phosphanes

The reactivity of a series of phosphanes with a fluoroaryl group (HF₄C₆-) carrying a spectator function in para position has been explored with respect to the formation of low coordinated and phosphorus rich phosphanes. An asymmetric diphosphene has been indentified as an intermediate in the synthesis of a linear 1,3-dihydrophosphane, while the symmetric diphosphene undergoes 2 + 2 cycloaddition under formation of the corresponding cyclotetraphosphetane for which a crystal structure could be obtained. Attempts to synthesize HF₄C₆-substituted iminophosphanes generally failed, which is attributed to the electronic nature of the corresponding precursors as suggested by quantum chemical calculations.     

Unerwartete Bildung von Monomesitylmolybdän(V,VI)-Verbindungen

Mesityl Oxo Molybdenum and Tungsten Compounds. II. Unexpected Formation of Monomesityl Molybdenum(V,VI) Compounds The synthesis of known MoO₂Mes₂ from MoO₂Cl₂ and MgMes₂ (1 : 1) in THF is accompanied by the formation of monomesityl molybdenum compounds. From ligand exchange and reduction arise [MesMoOCl₃]^– ( 3 a ) and [MesMoO₃]^– ( 3 c ). 3 a and 3 b crystallize in form of [(MesMoO₃)₂{Mg₂Cl₂(THF)₅}₂][MesMoOCl₃]₂(THF)₂, which has been characterized by X-ray structural analysis. In 3 two MesMoO₃ units are linked in a ring-like manner via magnesium ions. The anion 3 a , which possesses a distorted trigonal-bipyramidal arrangement, was also isolated as [Mg(THF)₆][MesMoOCl₃]₂ which was investigated by X-ray analysis. The reaction of MoO₂Cl₂ with MgMes₂ in a 1 : 0,5 ratio generates the compounds [Mg(THF)₄(MoO₃Cl)₂] and MoOCl₃(THF)₂. Reaction pathways which may lead to these compounds are discussed.     

Mesityloxomolybdän- und -wolfram-Verbindungen. I. Die Struktur von LiMoO2Me2Mes(OEt2)2

Mesityl Oxo Molybdenum and Tungsten Compounds. I. Structure of LiMoO₂Me₂Mes(OEt₂)₂ LiMoO₂Me₂Mes(OEt₂)₂ 2 is prepared by literature method [2] from MoO₂Mes₂ 1 and LiMe. Its x-ray structure and NMR-spectral data are presented. 2 adopts a dimer structure in which two [MoO₂Me₂Mes]^? anions are linked via two bridging [Li(OEt₂)₂]⁺ cations bonded to the oxo ligands. The resulting [‥OMoOLi‥]₂ ring is planar.     

Zur Bildung von Vinylverbindungen des Lanthans und Lutetiums

On Preparation of Vinyl Compounds of Lanthanum and Lutetium At reaction of permethyllanthanocene chloride with vinyl lithium coupling of vinyl groups takes place with formation of the butadiene complex [Li(dme)₃][Cp₂*La(C₄H₆)] ( 1 ). The corresponding lutetium compound yields the expected vinyl complex Cp₂*Lu(CH?CH₂) · LiCl · dme ( 4 ) with low stability. Furthermore, the more stable alkenyl compounds Cp₂*LaCPh?CMe₂ · 2 thf ( 2 ) and Cp₂*LuCPh?CMe₂ · MgCl₂ · dme ( 3 ) could be obtained. The new complexes were characterized by their ¹H and ¹³C-n.m.r. spectra.     

新型含硫阴离子表面活性剂的合成及其表面活性

合成了三种未见文献报道的阴离子表面活性剂，并研究了它们的表面活性。