硫酸亚铁和高锰酸钾联合氧化深度处理酵母废水

采用硫酸亚铁与高锰酸钾联合氧化深度处理酵母废水,分别研究了在曝气条件下硫酸亚铁投加量、pH值、反应时间对COD去除率的影响,以及联合高锰酸钾情况下高锰酸钾投加量、pH值、反应时间对COD去除率的影响。结果表明,在曝气条件下,硫酸亚铁投加量为5.0 g.L-1、pH值为7.0、反应时间为50 min时,COD去除率可达60%~65%;在联合高锰酸钾条件下,高锰酸钾投加量为1.0 g.L-1、pH值为8.0、反应时间为10 min时,COD去除率可达75%左右。处理废水达到排放标准。     

The Crystal and Molecular Structure of Dianhydrogossypol

Dianhydrogossypol (4,4′-dihydroxy-5,5′-diisopropyl-7,7′-dimethyl-bis(3H-naphtho[1,8-bc]furan-3-one)) was made by refluxing gossypol in m-xylene. Proton NMR spectroscopy was used to confirm that complete conversion was achieved over a time period of several hours. Single crystals of the compound were obtained by slow evaporation from dichloromethane. Diffraction studies indicate that this crystal form is tetragonal with a I4₁/a space group and with cell dimensions of a = b = 33.8265(4) Å, c = 9.1497(2) Å, V = 10469.4(3) Å³ at 100 K. The structure was solved by direct methods and was refined to an R1 value of 0.0415 on 6,408 independent reflections. Dianhydrogossypol exists as a pair of enantiomers within this structure. The two fused planar ring systems are oriented at a 117° angle to each other (i.e., close to perpendicular), and the isopropyl groups are oriented with the ternary carbon hydrogen atoms pointed inward toward the center of the molecule. Repeating groups of four molecules (of the same chirality) pack to form a helical structure that is supported by intermolecular hydrogen bonds. Each helix is surrounded by four neighboring helices that are composed of molecules of the opposite chirality. The helices form the walls of empty channels that are 5–6 Å wide. As has been found for some gossypol crystal forms, the open-channel structure of dianhydrogossypol might be useful for scavenging or carrying small molecules. Additional NMR studies confirm that dianhydrogossypol can be converted directly to gossypol lactol ethers in the presence of anhydrous alcohols.     

Synthesis,Crystal Structure,Electrochemical and Catalytic Properties of Hybrid Polyoxomolybdate Clusters-Based Terbium Complex

The inorganic–organic compound based on polyoxomolybdate [Tb(C₂H₆SO)₈][PMo₁₂ O₄₀]·2C₂H₆SO·½H₂O (I) has been isolated and structurally characterized by single-crystal X-ray molecular structure, IR spectra, thermogravimetric analysis and cyclic voltammetry measurements. The catalytic activities of (I) were also tested. The title compound crystallizes in monoclinic crystal system with C2/c space group. In the crystal, the polyoxidometalate anions are arranged in chains parallel to the [010] direction. The complex cations are located between these layers and linked to the neighbouring anions via weak C–H?O hydrogen bonding interactions leading to the formation of three dimensional network structure. Their catalytic activity toward organic dye is quite sizeable since the target removal is about 68% in the presence of the system POM-Tb/H₂O₂ after 120 min.     

荧光材料钴配合物的合成、晶体结构及荧光传感

以5-氨基间苯二甲酸为配体,采用溶剂热法构筑了一个新型的[Co(C_8H_5NO_4)(H_2O)]_n·2H_2O配合物。通过IR、元素分析以及X-射线单晶衍射表征产物的结构。该配合物的中心离子CoII分别与来自四个不同配体的四个羧酸氧原子、一个氨基氮原子和一个水分子上的氧原子配位,形成了六配位CoO_5N的八面体构型。对配合物的荧光性质及荧光传感性能进行了研究,结果表明不同金属离子对配合物荧光强度有不同程度的影响,该配合物可作为荧光传感材料选择性的检测Mn~(2+)。     

镉苯并咪唑二乙酸配合物的合成、晶体结构和热性能研究

1,3-苯并咪唑二乙酸与镉离子的反应,采用溶液法得到结构新颖的配合物:{[Cd3(η2-L-μ2-η2)2(4,4'-bipy)2(SO4)2(H2O)4]·5H2O}n。通过元素分析、红外光谱、热稳定性对配合物进行了初步表征,且通过单晶X-ray衍射对其晶体结构进行了测定。     

3-氨基吡嗪-2-羧酸镍配合物的合成与结构

以3-氨基吡嗪-2-羧酸(3-Hapzac)为配体合成了一个镍的配合物[Ni(3-apzac)_2(H_2O)_2],并利用元素分析、IR以及X射线单晶衍射等手段对配合物进行了表征。在配合物中,配位的水分子、羧基和与氨基都参与形成了氢键,通过强的氢键相互作用使配合物形成了三维超分子网络结构。     

4,4'-Azpy和叠氮桥联铜配合物的合成、结构和磁性

用扩散法合成了一种以4,4'-偶氮联吡啶(Azpy)为第二桥联配体的新叠氮铜二维配合物[Cu(azpy)(N_3)_2]n。对配合物进行了X-射线单晶衍射结构分析、红外光谱表征及磁性性质研究。结果表明,在配合物中,铜离子之间通过EE叠氮桥联和4,4'-Azopyridine(azpy)桥联形成了一个二维层状结构,并具有4-连接(44.62)拓扑结构。对磁性数据进行分析,得出该配合物中EE-叠氮桥联的Cu(Ⅱ)离子间存在反铁磁性耦合,而配合物在低温时出现了铁磁性耦合可能是由自旋倾斜造成的弱自发磁化作用引起的。     

工业化硫酸亚铁湿法制备氧化铁红并回收硫酸铵

探讨了利用硫酸亚铁合成高品质氧化铁红的生产工艺。论述了影响氧化铁红品质的诸多因素。     

含吡咯亚胺铜配合物的合成、表征及晶体结构

合成了一种新型含吡咯亚胺铜配合物,用元素分析、红外光谱及X射线单晶衍射对其进行了表征。结构解析表明,每个铜配合物分子含有两个吡咯亚胺配体,每个配体用两个氮原子与中心金属铜离子螯合,每个铜离子均采取平面四边形构型与配体中的四个氮原子配位。     

The Crystal and Molecular Structure of Kinamycin C p-Bromobenzoate

The molecular structure of kinamycin C has been determined by means of an X-ray study of its p-bromobenzoate derivative, C₃₁H₂₃N₂O₁₁Br. The crystals are monoclinic, P2₁, with four molecules of the derivative and four molecules of benzene in a unit cell of dimensions: a = 18.404 ± 0.005, b = 21.299 ± 0.004, c = 9.049 ± 0.001 Å, and β = 90.07 ± 0.03°. Reflection intensities were measured visually from equi-inclination Weissenberg photographs taken with Cu Ka radiation. The structure was solved by the heavy-atom method, and was refined by the block-diagonal-matrix least-squares method using anisotropic temperature factors for all the atoms. The final R factor is 8.9%. The stereostructures of the two crystallographically independent molecules are almost identical. The skeleton of the molecule is made up of four fused rings: two of these form a 1,4-naphthoquinone system and the rest are a pyrrole and a cyclohexene ring. A cyano group is bonded to the nitrogen atom of the pyrrole ring, which is rather unusual in an antibiotic.     

以二吡啶胺为配体的新型钴配合物的合成及结构

以2,2’-二吡啶胺(Hdpa)和对氨基苯甲酸钠(PABA为4-氨基苯甲酸阴离子)为原料,和氯化钴反应合成了一种新型的钴配合物[Co(Hdpa)2(PABA)]Cl(CH3OH),并通过扩散法得到了该配合物的单晶。通过单晶衍射、元素分析、红外光谱、质谱(ESI)对该配合物进行了结构表征。晶体结构表明:该配合物为阴离子-阳离子型化合物。     

吡唑-3-甲酸钴的合成、晶体结构及其与牛血清白蛋白的相互作用

利用吡唑-3-甲酸为配体,通过溶液法与氯化钴反应合成出一种钴的配合物,用X射线单晶衍射仪对其进行表征。结果显示,该配合物为单斜晶系,空间群为P21/c,a=0.509 94(2)nm,b=1.139 55(5)nm,c=0.936 80(4)nm,β=95.925(5)°。钴与两个配体分子的N、O原子和水分子的氧原子配位,形成八面体结构。利用紫外-可见吸收光谱与荧光光谱研究它与牛血清白蛋白(BSA)的相互作用。结果表明,该配合物与BSA形成稳定的复合物,荧光猝灭属于静态猝灭,猝灭速率常数kq为3.54×1012L/(mol·s),结合常数K=7.06×105L/mol,结合位点n=1.259 5。     

一种以咪唑衍生物为配体的卡宾银配合物的合成及晶体结构

以咪唑衍生物和氧化银为原料,二氯甲烷为溶剂,常温下反应生成配合物[Ag(DIM)2]BF4,并对合成物的晶体结构进行了研究。X-射线单晶解析结果表明:该晶体属于单斜晶系,空间群C_2/c,a=14.010(18),b=8.303(11),c=14.936(20),α=90.00°,β=93.910(4)°,γ=90.00°,V=1639(4)3,Z=4。     

二硝酰胺钾的合成、晶体结构及性能

以N-脒基脲二硝酰胺盐(GUDN)和氢氧化钾为原料合成了二硝酰胺钾(KDN),用元素分析、傅里叶红外光谱对其结构进行了表征。培养了KDN的单晶,并通过X射线单晶衍射仪测定了其晶体结构。采用差示扫描量热分析仪(DSC)研究了KDN的热分解行为,并测试了其感度。结果表明,KDN晶体属于单斜晶系,P2(1)/n空间群,晶胞参数为:a=0.661 0(11)nm,b=0.927 2(15)nm,c=0.719 4(12)nm,β=97.568(3)°,V=0.437 1(12)nm~3;Z=4;Dc=2.236g/cm~3;F(000)=288。KDN的熔点为128℃,撞击感度大于50cm,摩擦感度为0,静电感度为142.53mJ,感度低于RDX,是一种钝感的二硝酰胺类含能材料。     

以m-BrPhH_3 IDC为配体构筑的钴配合物的合成、晶体结构和热性能

采用溶剂热法使m-Br Ph H3IDC与Co(Ⅱ)合成了单核配合物:[Co(m-Br Ph H3IDC)2(2H2O)],采用元素分析、红外光谱以及单晶X-ray测试了其分子结构。进一步研究了这个配合物在空气中的热稳定性能。     

2-巯基吡啶与Cu(I)配合物的合成、晶体结构及光物理性质

利用Cu(I)前体[Cu(CH3CN)4]BF4与配体2-巯基吡啶、邻菲罗啉进行反应,合成了一种新型铜(I)配合物:{[Cu3(py2tH)6](BF4)3.H2O}n。运用X-射线单晶衍射方法确定了其晶体结构。同时,利用现代波谱方法对配合物的光物理性质进行研究。发射光谱显示在632nm处的发射峰属于金属到配体的电荷跃迁,即MLCT。     

邻苯二甲酰氨基酸的合成及晶体结构

用邻苯二甲酸酐作氨基保护剂,与6种氨基酸缩合制备了邻苯二甲酰氨基酸。重点考察了邻苯二甲酰甘氨酸的合成条件对产物收率的影响,最佳合成条件为:反应温度140℃,反应时间30 min,n(甘氨酸)∶n(邻苯二甲酸酐)=1∶1.2,收率95.6%。以同样的条件合成的另外5种邻苯二甲酰氨基酸的收率也都达到了81%以上。经解析发现,邻苯二甲酰甘氨酸一水合物的晶体结构属单斜晶系,P21/n空间群,晶胞参数:a=7.638 0(15)nm,b=13.803(3)nm,c=10.009(2)nm,β=106.67(3)°,Z=4,Dc=1.466 g.cm-3,μ=0.120 mm-1,F(000)=464。最终偏离因子R=0.060 6,wR=0.164 7。晶体结构分析表明,分子间氢键连接整个分子形成沿[010]方向的锯齿状长链,再通过π-π堆积作用形成稳定的三维立体结构。     

二苯二硒的合成和晶体结构

报道了一种新的合成工艺,采用氯化镉为催化剂,利用空气中的氧气直接氧化苯硒酚合成了二苯二硒晶体,表征了其晶体结构和红外光谱性质。晶体属于正交晶系,空间群 P21 21 21,a= 0 5646 (2) nm,b= 0 8288 (3) nm,c=2 4100(9)nm; V=1 1276(7)nm3,Dc=1 839 g·cm-3,Z=4, R=0 0259。     

以联吡啶为配体的新型钴配合物的合成、结构及性质

以2,2’-联吡啶(BIPY)和苯甲酸钠为共原料,和氯化钴反应合成了一种新型的钴配合物[Co(BIPY)(C_6H_5COO)_2],并通过扩散法得到了该配合物的单晶。通过X-射线单晶衍射、元素分析、红外光谱对该配合物进行了结构表征。晶体结构表明:该分子结构中,钴配位中心分别与一个2,2’-联吡啶和两个苯甲酸配位。我们还对该配合物的热稳定性进行了研究。     

Determination of the Oxidation State of Antimony, Iron and Vanadium in Mixed Vanadium and Iron Antimonate Oxide Catalysts

Vanadium and mixed vanadium and iron antimonates with rutile-type structures have been studied by XANES at Sb L₁ edge, ⁵⁷Fe Mössbauer spectroscopy and ESR spectroscopy at 77 K. The results showed that both antimony and iron remained at their highest oxidation state, i.e. Sb^V and Fe^III, whereas vanadium was present as V^III and V^IV. Two types of V^IV species were distinguished corresponding to well-isolated vanadyl species in distorted octahedral coordination and vanadyl species in the same coordination but close to each other and in a dipole–dipole interaction. Both V^III and total V^IV concentrations decreased when the iron content increased, whereas isolated V^IV concentration increased first and then decreased, with a maximum for x = 0.2 in Fe_xV_1-xSbO₄. The observed variations in cationic composition are discussed in relation with the catalytic properties of the compounds in the ammoxidation of propane. Isolated V^IV-O moieties appeared to be the most active and selective catalytic sites.