丙二醇甲醚醋酸酯的合成研究

采用浓硫酸作催化剂,用丙二醇甲醚和冰醋酸酯化合成丙二醇甲醚醋酸酯,考察了醚和酸的比例、催化剂用量、带水剂用量与种类、反应时间和反应温度等因素对反应的影响。优惠反应条件为:冰醋酸∶丙二醇甲醚=1.3∶1(mol/mol),催化剂用量为反应液质量的1 0%,带水剂A用量为反应液质量的25%,反应温度104～110℃,反应时间3h。丙二醇甲醚醋酸酯的收率达96 5%。     

硫酸氢钠催化合成丙二醇甲醚醋酸酯的研究

以醋酸和丙二醇甲醚为原料,硫酸氢钠为催化剂,环己烷为带水剂合成丙二醇甲醚醋酸酯,考察了原料醇酸配比、催化剂用量、带水剂用量、反应时间等因素对转化率的影响。通过实验结果分析对比,得到较佳实验反应条件：在原料酸醇配比为1.5,催化剂用量为原料总质量的3%,带水剂用量为原料总质量的15%,反应时间为3 h的工艺条件下,丙二醇甲醚的转化率达到96%以上。     

稀土固体超强酸SO_4~(2-)/TiO_2/Ce(IV)催化合成环己酮1,2-丙二醇缩酮

以环己酮与1,2-丙二醇为原料,稀土固体超强酸SO42-/TiO2/Ce(IV)为催化剂,合成了环己酮1,2-丙二醇缩酮,考察了影响反应的因素。结果表明,在n(酮)n∶(醇)=1 1∶.5、催化剂用量占反应物总质量的1.7%、带水剂环己烷用量占反应物总质量的30%、反应时间1h的优化条件下,环己酮1,2-丙二醇缩酮收率可达84.28%。     

稀土固体超强酸SO2-4/TiO2/Ce(Ⅳ)催化合成环己酮1,2-丙二醇缩酮

以环己酮与1,2-丙二醇为原料,稀土固体超强酸SO24-/TiO2/Ce(Ⅳ)为催化剂,合成了环己酮1,2-丙二醇缩酮,考察了影响反应的因素.结果表明,在n(酮):n(醇)=1:1.5、催化剂用量占反应物总质量的1.7%、带水剂环己烷用量占反应物总质量的30%、反应时间1 h的优化条件下,环己酮1,2-丙二醇缩酮收率可达84.28%.     

强酸性离子交换树脂催化合成丙二醇乙醚乙酸酯

以强酸性001x7(732)阳离子树脂为催化剂合成丙二醇乙醚乙酸酯。考察了原料配比、催化剂的用量、带水剂的用量以及反应时间等因素对反应的影响。合成丙二醇乙醚乙酸酯优化条件为:n(丙二醇乙醚)∶n(乙酸)=1.0∶1.3,催化剂的用量为反应原料总质量的5%,带水剂的用量为反应原料总质量的20%,回流时间为5 h。优化条件下,产品收率75.3%。催化剂不经处理可以重复利用1~2次。     

纳米固体超强酸SO_4~(2-)/Fe_2O_3催化合成环己酮1,2-丙二醇缩酮

以纳米固体超强酸SO_4~(2-)/Fe_2O_3为催化剂,催化环己酮和1,2-丙二醇的缩合反应,合成了环己酮1,2-丙二醇缩酮。研究焙烧温度、反应时间、酮醇物质的量比、带水剂用量和催化剂用量等对反应的影响。较适宜的反应条件为:环己酮200 mmol,酮醇物质的量比为1:1.1,催化剂用量为200 mg(占反应物总质量的2.9%),甲苯30 mL,温度(120～130)℃,反应2.5 h,环己酮1,2-丙二醇缩酮收率达97.4%,纯度98%。     

固体超强酸催化合成苯乙酮1,2-丙二醇缩酮

研究了以专利SO2-4/MxOy型固体超强酸为催化剂催化合成苯乙酮1,2-丙二醇缩酮的反应.较系统地考察了反应温度、催化剂用量、反应时间以及带水剂对缩酮化反应的影响.实验结果表明:在n(1,2-丙二醇):n(苯乙酮)=1.4:1,固体超强酸催化剂用量为反应物总质量的8%,采用二甲苯作带水剂,反应3 h的优化条件下,苯乙酮1,2-丙二醇缩酮的收率可达94.67%.     

固体超强酸S2O82-/SnO2-SiO2催化环己酮1,2-丙二醇缩酮研究

以S2O82-/SnO2-SiO2为催化剂,用环己酮1,2-丙二醇合成缩酮.系统地研究了带水剂及其用量、酮醇摩尔比、催化剂用量、反应时间诸因素对产品收率的影响.通过正交实验得出适宜的反应条件为:n (环己酮) :n (1,2-丙二醇)=1∶1.6,催化剂用量为反应物总质量的2.0% ,带水剂环己烷5.0mL,反应时间50min.在上述条件下,缩酮收率可高达91.47% .     

活性炭负载柠檬酸催化合成环己酮 1,2-丙二醇缩酮

采用活性炭负载柠檬酸催化剂,以环己酮和1,2-丙二醇为原料,环己烷为带水剂合成了环己酮1,2-丙二醇缩酮,考察了原料配比、催化剂用量、反应时间等因素对反应收率的影响。得到较佳工艺条件为:n(环己酮)∶n(1,2-丙二醇)=1∶1.5,带水剂的用量为反应物总体积的35%,催化剂的用量为反应物总质量的3.1%,回流反应2.5 h,产品收率为89.4%。对催化剂的重复使用性进行了考查,实验结果表明:活性炭负载柠檬酸是合成环己酮1,2-丙二醇缩酮的良好催化剂,在优化条件下,催化剂重复使用5次产品收率基本不变。     

纳米固体超强酸SO2-4/Fe2O3催化合成环己酮1,2-丙二醇缩酮

以纳米固体超强酸SO2-4/Fe2O3为催化剂,催化环己酮和1,2-丙二醇的缩合反应,合成了环己酮1,2-丙二醇缩酮.研究焙烧温度、反应时间、酮醇物质的量比、带水剂用量和催化剂用量等对反应的影响.较适宜的反应条件为:环己酮200 mmol,酮醇物质的量比为1:1.1,催化剂用量为200 mg(占反应物总质量的2.9%),甲苯30 mL,温度(120-130)℃,反应2.5 h.环己酮1,2-丙二醇缩酮收率达97.4%,纯度>98%.     

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。