Fe~(3 )、Zn~(2 )、Mn~(2 )、Cu~(2 )、Ca~(2 )、Mg~(2 )等离子共存体系中Ca~(2 )、Mg~(2 )的测定

叙述了Fe3 、Zn2 、Mn2 、Cu2 、Ca2 、Mg2 等离子共存体系中采用六次甲基四胺 -铜试剂沉淀除去Fe3 、Zn2 、Mn2 、Cu2 等干扰离子 ,用EDTA滴定钙镁的方法 ,该方法钙的回收率在 99.7%～ 10 0 .3 % ;镁的回收率在 10 0 .0 %～ 10 0 .4% ,标准偏差为 0 .0 2 2。     

Ag(I)(Et(2)PCH(2)CH(2)PPh(2))(2)]NO(3): An Antimitochondrial Silver Complex

The silver(I) complex [Ag(eppe)(2)]NO(3) (eppe = Et(2)PCH(2)CH(2)PPh(2)) is shown by X-ray crystallography to be tetrahedral with Ag - PEt(2) and Ag - P Ph(2) bond lengths of 2.482 and 2.518 A, respectively. The complex is selectively antimitochondrial and inhibits the growth of a number of yeast strains in non-fermentable media at concentrations as low as 2.5 muMu and induces the mitochondrial mutation petite The effect is largely reversed by the presence of aspirin. The complex is shown to be stable in the cell culture media and in the presence of glutathione, but readily reacts with disulfides of oxidized glutathione and serum albumin. Surprisingly, neither [Au(eppe)(2)]Cl nor [Au(eppe)(2)]Cl (dppe = Ph(2)PCH(2)CH(2)PPh(2)) showed any mitochondrial selectivity in the same screening protocol.     

Interaction of [Rh(2)(O(2)CCH(3))(4)(H(2)O)(2)] and [Rh(2)(O(2)CCH(OH)Ph)(2)(phen)(2)(H(2)O)(2)](O(2)C-CH(OH)Ph)(2) With Sulfhydryl Compounds and Ceruloplasmin

The interaction of binuclear rhodium(II) complexes [Rh(2)(OOCCH(3))(4)(H(2)O)(2)], [Rh(2){OOCCH(OH)Ph}(2)(phen)(2)(H(2)O)(2)] {OOCCH(OH)Ph}(2), [Rh(2)(OOCCH(3))(2)(bpy)(2)(H(2)O)(2)](OOCCH(3))(2) and [Rh(2)Cl(2)(OOCMe)(2)(bpy)(2)](3H(2)O) with ceruloplasmin, cysteine, glutathione and coenzyme A have been investigated using. UV-Vis and CD spectroscopies. The complexes containing phen or bpy at pH = 7.4 and 4.0 are readily reduced with sulfhydryl compounds, while rhodium(II) acetate is relatively stable in these conditions. Complex [Rh(2){OOCCH(OH)Ph}(2)(phen)(2)(H(2)O)(2)] strongly changes structure of ceruloplasmin leading to the decrease of of alpha-helix content and loss of oxidase activity.     

Copper (2+), Zinc (2+), and Nickel (2+) Uptake by Activated Sludge

Abstract

This paper reports the results obtained on copper, zinc, and nickel uptake by activated sludge in a completely mixed unit. Removal of these heavy metals from wastewater occurs by uptake and by precipitation, the latter being particularly important in the cases of copper and zinc. The amount of heavy metal taken up by the microorganisms at equilibrium varies with influent concentration for the three metals studied. The values obtained range from 2.3 mg/g VSS for copper at 1 mg/L in the influent to 57.4 mg/g VSS for nickel at influent 25 mg/L. Soluble metal removal from wastewater increases in percentage with influent concentration, being higher for copper and lower for nickel. Experiments with mixtures of these metals have also been carried out.     

氨噻肟酸与AE—活性酯

我国氨噻肟酸的总产量为300-400t/a,产品大部分用于生产AE-活性酯,部分直接出口。在氨噻肟酸生产中如何对反应过程进行实时监控,利用液氯替代价格较高同时危险性较大的液溴,以及如何控制氨噻肟酸产物中顺反异构体的比例、阻止二聚体的生成是今后有待解决的问题;在AE-活性酯的生产中,利用价格较低的原料代替昂贵的三苯基膦将对降低生产成本起到决定性的作用。     

H(2)O(2) in CO(2): sustainable production and green reactions

Hydrogen peroxide is a "green" oxidant whose relatively high cost has prevented it from being applied to commodity chemical processing. Interestingly, those attributes of the current H(2)O(2) process that contribute to the high cost also contribute to its nonsustainable features. We have consequently explored the generation of hydrogen peroxide both by the AQ route and directly from hydrogen and oxygen using liquid CO(2) as the solvent, because CO(2) provides some unique advantages to H(2)O(2) synthesis.     

N（2—甲苯基）—2—（2—甲苯氧乙酰基）氨基脲的合成

以固体氢氧化的钠作催化剂,用Ｎ－（２－甲苯基）三氯乙酰胺与２－本氧乙酰肼反应,合成一种新的氨基脲。     

A new binuclear Cr(III) citrate anion: Synthesis,characterization and crystal structure of [Cr(CO(NH2)2)6]2[Cr2(CO(NH2)2)2(C6H4O7)2]3

The new anion [Cr₂(CO(NH₂)₂)₂(C₆H₄O₇)₂]^2 − has been isolated in the complex [Cr(CO(NH₂)₂)₆]₂[Cr₂(CO(NH₂)₂)₂(C₆H₄O₇)₂]₃. The crystals of this complex were obtained by a one-pot synthetic method using 1:1 molar ratio of hexaureachromium(III) chloride and trisodium citrate in aqueous medium. It was characterized by elemental analysis, IR spectroscopy and single crystal X-ray diffraction analysis. The compound crystallizes in space group R‾3 of the trigonal system with three formula units in a cell of dimensions a = b = 24.7461(4) Å, c = 13.7204(3) Å and γ = 120°. The crystal structure comprises the columns consisting of [Cr(CO(NH₂)₂)₆]^3 + cations surrounded by a cylinder of complex anions, [Cr₂(CO(NH₂)₂)₂(C₆H₄O₇)₂]^2 − which are packed in a honeycomb-like manner. This supramolecular architecture is formed and stabilized by inter- and intramolecular NH⋯O hydrogen bonds.     

2-(2-氯苄基)-2-(1-氯环丙基)环氧乙烷的合成

报道了丙硫菌唑中间体2-(2-氯苄基)-2-(1-氯环丙基)环氧乙烷的合成方法。以1-氯-N,N-二甲基环丙基甲酰胺和邻氯氯苄为原料,经格氏反应制备2-氯苄基-(1-氯环丙基)酮;后者再与硫叶立德试剂反应得到相应的环氧化物。     

配合物Co(2-mpac)2(H2O)2的晶体结构与热稳定性

以2-甲基-5-羧基吡嗪为配体合成了标题化合物,并利用元素分析、红外光谱、单晶X-射线衍射以及热重分析对配合物进行了表征.晶体学数据:三斜晶系,P-1空间群,a=5.1068(7)(A),b=6.3725(8)(A),c=12.2900(16)(A),α=103.5740(10)°,β=91.057(2)°,γ=108...     

One novel polynuclear complex [Cu2(bpc)2(N3)4Ca(H2O)2Na2(H2O)2]n having three different transition and non-transition metal centres

The complex [Cu₂(bpc)₂(N₃)₄Ca(H₂O)₂Na₂(H₂O)₂]_n (1) (bpc²⁻=2,2^′-bipyridyl-3,3^′-dicarboxylate) has been prepared and characterised by elemental analyses, spectroscopic and single crystal X-ray diffraction study. Single crystal X-ray analysis revealed a novel polynuclear complex containing three different metal centres such as an alkali metal (sodium), an alkaline earth metal (calcium) and a transition metal atom (copper) connected together by azide and carboxylato groups.     

6-（6-（2-甲基-2H-四唑-5-基）吡啶-3-基）-2-（2-（甲磺酰基）乙基）酞嗪-1（2H）-酮的合成

以6-溴-2-(2-(甲磺酰基)乙基)酞嗪-1(2H)-酮和5-溴-2-(2-甲基-2H-四唑-5-基)吡啶为起始原料,经硼酸酯化和Suzuki偶联反应合成了6-(6-(2-甲基-2H-四唑-5-基)吡啶-3-基)-2-(2-(甲磺酰基)乙基)酞嗪-1(2H)-酮,收率为67.0%,产物的结构经IR、~1H NMR、~(13)C NMR和MS得到确证。     

氨噻肟酸乙酯的合成研究

以去甲氨噻肟酸乙酯(DMAT)为原料,对影响反应收率的反应温度、物料配比、相转移催化剂及其用量、甲基化试剂、反应时间等因素进行了研究。最佳反应条件为:反应温度20℃,NaOH为碱性试剂,DMAT∶NaOH∶(CH3O)2SO3为1∶1.2∶1.2,四丁基碘化铵作相转移催化剂,用量为底物摩尔数的7%,硫酸二甲酯为甲基化试剂,乙醇和四氢呋喃为溶剂,反应时间约为4 h,总收率为79%。     

3-碘-N1-(2-甲基-4-七氟异丙基苯基)-N2-(1,1-二甲基-2-甲砜基乙基)-1,2-苯二甲酰胺的合成

以邻苯二甲酸酐为原料,经酰胺化、氧化、碘化反应制得3-碘-N1-(2-甲基-4-七氟异丙基苯基)-N2-(1,1-二甲基-2-甲硫基乙基)-1,2-苯二甲酰胺。讨论了反应物料摩尔比、催化剂用量、反应温度、反应时间等因素对产品收率的影响。优化后四步反应总收率61.1%,含量96.5%。产物及中间体结构经1HNMR和ESI-MS确证。通过对钯碳的回收套用大大降低了成本。该合成路线具有原料易得,操作简便,收率高等优点,具有较好的工业化应用前景。     

First complex of the monoprotonated trioxodinitrate anion: synthesis and characterization of [Hg2(HN2O3)2(NO3)2(Ph2PNHPPh2)2]

The reaction of Hg(NO₃)₂·H₂O with bis(diphenylphosphino)amine, Ph₂PNHPPh₂ (dppam), produces [Hg₂(HN₂O₃)₂(NO₃)₂(dppam)₂] (1), which is the first complex containing the monoprotonated trioxodinitrate anion. 1 has been fully characterized by an X-ray structure analysis, NMR spectroscopy (¹⁹⁹Hg{¹H}, ³¹P{¹H}, ¹H), FAB mass spectrometry, IR spectroscopy, elemental analysis and melting point. 1 is the unique example of a face-to-face complex of five-coordinate Hg(II) centres with dppam including the first structural characterization of a rare tautomer of the monoprotonated trioxodinitrate anion.     

二氰基二硫纶·邻菲咯啉-5,6-二酮混配锰(Ⅱ)、铁(Ⅱ)、钴(Ⅱ)配合物的感光氧化特性

测定了二氰基二硫纶·邻菲咯啉-5,6-二酮混配锰(Ⅱ)、铁(Ⅱ)、钴(Ⅱ)配合物MLL'(M=Mn2+、Fe2+、Co2+；L=mnt2-,1,2-二氰基乙烯-1,2-二硫醇离子；L'=phen-5,6-dione,1,10-邻菲咯啉-5,6-二酮)在二甲基亚砜(DMSO)、丙酮(Acet)和氯仿(CHCl3)中的电子...     

3-碘-N1-(2-甲基-4-七氟异丙基苯基)-N2-(1,1-二甲基-2-甲砜基乙基)-1,2-苯二甲酰胺的合成

以邻苯二甲酸酐为原料,经酰胺化、氧化、碘化反应制得3-碘-N1-(2-甲基-4-七氟异丙基苯基)-N2-(1,1-二甲基-2-甲砜基乙基)-1,2-苯二甲酰胺。讨论了反应物料摩尔比、催化剂用量、反应温度、反应时间等因素对产品收率的影响。优化后4步反应总收率61.1%,产物HPLC纯度96.5%。产物及中间体结构经1HNMR和ESI-MS确证。通过对钯碳的回收套用降低了成本,该合成路线具有原料易得,操作简便,收率高等优点,具有较好的工业化应用前景。     

Organization of poly(2-ethyl-2-oxazoline)-block-poly(2-phenyl-2-oxazoline) copolymers in water solution

Diblock copolymers were prepared from 2-ethyl-2-oxazoline and 2-phenyl-2-oxazoline via living cationic polymerization using sequential addition of the monomers. Copolymer assemblies in aqueous solutions and on surface were studied with respect to changes in the hydrophilic-hydrophobic balance induced by increasing the length of the hydrophobic poly(2-phenyl-2-oxazoline) segment while the hydrophilic poly(2-ethyl-2-oxazoline) chain was kept constant with an average of 60 monomer units. The copolymer with a short segment of four 2-phenyl-2-oxazoline units assembled into highly hydrated aggregates that decreased twice in size after drying. Their structure was destroyed and network morphologies were formed upon spin-coating. The increase of the length of the hydrophobic segment resulted in aggregates that dissociated to micelle-sized particles when subjected to mechanical shear by spin-coating or filtering. These observations imply that the aggregates are multi-core structures originating from the assembly of primarily formed micelles. The copolymer self-assembly was evidenced by a combination of techniques: DLS, SLS, AFM and SEM.     

新型增塑剂对苯二甲酸二（二乙二醇丁醚）酯的合成工艺

以对苯二甲酸和二乙二醇丁醚为原料,在非酸性催化剂氯化亚锡的催化下,合成新型环保增塑剂对苯二甲酸二(二乙二醇丁醚)酯。考察了催化剂种类、原料配比、催化剂用量、带水剂用量、反应时间对酯化率的影响并通过FT-IR、GC-MS等进行产物表征。正交实验结果表明：当二乙二醇丁醚与对苯二甲酸的摩尔比为n(DGBE)∶n(PTA)=3.5∶1,催化剂氯化亚锡用量为5.00%（以PTA质量为准,下同）,带水剂用量为30.00%,反应时间为5.50h,搅拌转速300r/min时,产品的酯化率高达98.90%,精制后对苯二甲酸二(二乙二醇丁醚)酯的含量为99.03%。同时建立了该酯化合成的表观动力学模型,得到反应速率方程为：