两类四氨基酞菁的合成及其性质研究

分别由4-硝基邻苯二甲酰亚胺、3-硝基邻苯二甲酸酐和金属盐、尿素、钼酸铵在熔融状态下合成2,9,16,23-四-硝基金属酞菁、1,8,15,22-四-硝基金属酞菁,还原得到两类四氨基金属酞菁.用红外光谱、紫外-可见光谱对目标化合物进行了表征,并对金属酞菁的电导率进行了测定.结果表明:在紫外吸收光谱中,Co,Cu,Ni和Zn 4种金属对氨基取代酞菁化合物最大吸收波长的影响顺序大致相同.8种酞菁化合物的电导率随着温度的升高均有不同程度的增大.对于金属Co,Cu和Ni取代的酞菁化合物来说,1,8,15,22-四-氨基取代酞菁化合物均比2,9,16,23-四-氨基取代酞菁化合物的电导率大,而Zn则相反.     

梯形(phen)Zn-O-MoO2晶体的水热合成与表征

利用水热方法合成梯形(phen)Zn—O—MoO2晶体,并用X射线衍射仪对其结构进行了表征.结果表明,(phen)Zn—O—MoO2属单斜晶系:空间群为P2/m;a=0.881 64(17)nm,b=0.643 96(14)nm,c=1.065 9(6)nm,α=γ=90°,β=100.79(3)°,V=0.594 4(4)nm3,Z=2.Zn原子为三角双锥构型,Mo原子为四面体构型,(phen)Zn—O—MoO2为折叠梯形链状结构.     

混合钼钒多金属氧酸盐的水热合成、结构表征及磁性研究

通过水热方法合成了一种混合钼钒多金属氧酸盐[Cu(phen)_2]_4{HPMo_8~Ⅵ V_6~ⅣO_(42)[Cu(phen)]_2}·2H_2O.采用X射线单晶衍射、元素分析、红外光谱对其进行了表征,同时对其磁学性质进行了研究.结果表明:标题化合物包含高度还原的二帽假Keggin结构的多氧阴离子支撑2个过渡金属配合物,即铜配合物阳离子[Cu(phen)_2]~+和结晶水;该化合物呈铁磁性相互作用.     

组氨酸的Keggin结构杂多金属氧酸盐的合成及性质研究

首次合成了组氨酸的Ｋｅｇｇｉｎ结构（ＸＭ１２Ｏ４０＾ｎ－,Ｘ＝Ｐ,Ｓｉ,Ｍ＝Ｗ,Ｍｏ）３种杂多金属氧酸盐化合物,用元素分析、ＩＲ、ＵＶ、ＴＧ－ＤＴＡ等方法对标事物进行了表征,结果表明该类化合物仍保持Ｋｅｇｇｉｎ结构、杂多酸阴离子和氨基酸靠静电作用相结合。     

Hydrothermal synthesis of pyrrhotite (Fex-1S) nanoplates and their antibacterial, cytotoxic activity study

The aim of this study was to synthesize and characterize Fe_(x-1)S 2D-nanostructures with pyrrhotite phase,as well as to explore their biological(antibacterial and cytotoxic)properties,namely the expression of reactive oxygen species(ROS)in the exposure of cells and bacteria.Based on hydrothermal synthesis,the characterization of asprepared 2D-nanostructures was performed by XRD,SEM,EDS,and TEM,in which the single-crystalline pyrrhotite phased Fe_(x-1)S nanoplate morphology was observed.The antibacterial activities of Fe_(x-1)S nanoplates against human pathogenic strains such as Staphylococcus aureus,Escherichia coli,and Enterococcus faecalis were tested.Minimum inhibitory concentration(MIC)and minimum bactericidal concentration(MBC)were determined following the broth microdilution method.Cytotoxicity and expression of intracellular ROS of pyrrhotite nanoplates on Human Gingival Fibroblast(HGF),Human Pulp Cells(HPC)and Human Osteoblast(HBC)were calculated.Cell viability was determined by the MTT method.All experiments were performed of three independent experiments and data were analyzed by Kruskal-Wallis and Mann-Whitney tests,also Pearson′s Correlation was performed.The nanoplates exhibited good bactericidal effect.All types of cells tested showed slight cytotoxicity.It was found that intracellular ROS is produced when cells and bacteria tested are exposed to pyrrhotite nanoplates in presence of both air and peroxide hydrogen.ROS production levels were higher in the bacteria than the cells exposed to these nanoplates.     

水热合成金属硫化物的浮选行为及微观性质分析

石灰中和沉淀法处理重金属废水中会产生大量的中和渣,采用化学试剂模拟中和渣,利用元素硫的歧化反应,在水热条件下将模拟渣中的氢氧化物转变成硫化物,进而,可将产生的硫化矿利用常规浮选工艺加以回收。采用X线衍射(XRD)、激光粒度仪和扫描电镜(SEM)对3种硫化物的微观性质进行分析。试验结果表明:硫化铜和硫化铅有较好的可浮性,回收率分别为91.00%和72.78%,而硫化锌浮选效果较差,回收率为28.31%;硫化铜和硫化铅比硫化锌的水热结晶好,粒径大,表面光滑。在水热过程中添加矿化剂NaOH能提高硫化锌的结晶度,水热温度提高使硫化锌的晶粒增大、表面光滑,改进后硫化锌的回收率提高至63.92%。     

CeO2微结构的水热合成和光学性质

以Ce(NO3)3·6H2O作为铈源、尿素作为沉淀剂、K-30型PVP作为表面活性剂,采用水热法成功制备二氧化铈微结构.采用X射线衍射仪(XRD)、热重/差热分析(TG/DTA)、傅里叶变换红外谱(FT-IR)、扫描电子显微镜(SEM)、拉曼光谱(Raman)、紫外可见近红外分光光度计(UV-Vis)和荧光分光光度计(PL)对此CeO2样品进行表征,结果表明:制备的CeO2样品具有萤石立方结构,样品中存在氧空位和Ce3+离子,样品具有较强的紫外吸收和室温光致发光性能.吸收边和拉曼峰位的移动与样品中氧空位和Ce3+离子有关.     

二维开放骨架硫酸镧的水热合成与表征

采用水热合成方法，以氧化镧、硫酸和哌嗪、水为原料得到了具有新颖结构的硫酸镧．单晶衍射结果表明该化合物是有机胺支撑的、通过镧与硫酸根配位形成的层状开放骨架结构，该化合物也用元素分析、差热-热重和红外进行了表征．结果表明结构解析能够同相应的表征较好地吻合．     

Template/surfactant free and UV light irradiation assisted fabrication of Mn-Co oxides composite nanorings: Structure and synthesis mechanism

A facile, green, cost effective, and template or surfactant free strategy via a two-step route i.e. UV irradiation followed by dissolution-growth for the controlled synthesis of Mn-Co composite nanorings at room temperature was proposed. The nanorings structures and the process were systematically studied via TEM, HRTEM, EDX and XRD. Bir-MnO_2 nanosheets first formed through the direct photolysis of KMnO_4 under UV light irradiation. This was followed by a dissolution-growth process via the dissolution of Bir-MnO_2 nanosheets by the generated H~+ from the redox reaction between the added Co(NO_3)_2 and residual KMnO_4, as well as the accompanied formation of CoOOH, and Mn-Co composite nanorings. It was found that a balance between the dissolution and growth rate was needed. Suitable pH, KMnO_4 presence and the starting nanosheets like Bir-MnO_2 were the key factors for the formation of nanorings. The obtained Mn-Co nanorings/TiO_2 showed enhanced efficiency for the catalytic oxidation of HCHO. Based on the above understandings, it is believed that the developed dissolution-growth method can be adopted for the designing and preparation of other Mn-Co composite nanostructures which can be further applied for environmental pollution remediation.     

水热法合成不同形貌的氧化锌及其性质研究

采用水热法,以硝酸锌为原料,分别以四氟硼酸钠、N-丁基吡啶六氟磷酸盐和溴化1-乙基-23,-二甲基咪唑离子液体为导向剂合成了具有次级结构的扇面状、微球状和实心双螺帽状三种形貌的氧化锌,利用XRD和SEM对其结构和形貌进行了表征,研究了其荧光特性及对甲基橙的光催化活性.发现微球状ZnO在可见光区具有远远强于其它两种形貌ZnO的荧光.不同形貌的ZnO对甲基橙的光催化活性与商品TiO2(P25)的活性差别不大,其中扇面状ZnO的活性最高,实心双螺帽状ZnO次之,微球状ZnO活性最差.     

过渡金属金刚烷甲酸配合物的合成和表征

在沸水体系中,由过渡金属醋酸盐与金刚烷甲酸（Hadam,C10H15COOH）反应,合成了6种配合物M（adam）2·nH2O（M=Mn,n=2;M=Co,n=6;M=Ni,n=3．5;M=Cu,n=1;M=Zn,n=0;M=Cd,n=0）,并用元素分析、摩尔电导、红外光谱和热分析方法对配合物进行了表征。结果表明,中心金属离子M^2＋与2个配体（adam）羧基中的4个氧原子以双齿形式发生配位,形成了分子配合物,配位数为4（其中铜有1个配位水,其配位数为5）。     

水热法合成磷酸锰及其表征

以六水硝酸锰和十二水磷酸钠为原料,酸性条件150℃水热条件下反应24 h制备出深绿色MnPO4.H2O颗粒。对产物的结构进行X-射线粉末衍射(XRD),扫描电子显微镜(SEM),荧光(FL)光谱,红外(IR)光谱等表征。X-射线粉末衍射(XRD)分析表明得到产物为纯净的底心单斜相MnPO4.H2O,显示原料中的正二价的锰离子被氧化为正三价的锰离子;通过扫描电子显微镜(SEM)可以观察到MnPO4.H2O的形貌为边长约15μm的立方体。在水热条件下,Mn(NO3)2的浓度?溶液的pH、反应时间和反应温度对最终产物物相和形貌均有影响。     

High efficiency synthesis of HKUST-1 under mild conditions with high BETsurface area and CO2 uptake capacity

This study focuses on the development of a hydrothermal method for the rapid synthesis of good quality copper benzene-1,3,5-tricarboxylate(referred to as HKUST-1)with high yield under mild preparation conditions to address the issues associated with reported methods.Different synthesis conditions and activation methods were studied to understand their influence on the properties of HKUST-1.It was found that mixing the precursors at50°C for 3 h followed by activation via methanol refluxing led to the formation of a product with the highest BET specific surface area of 1615 m~2/g and a high yield of 84.1%.The XRD and SEM data illustrated that the product was highly crystalline.The sample was also tested on its capacity in CO_2 adsorption.The results showed strong correlation between surface area of the sample and its CO_2 uptake at 1 bar and 27°C.The HKUST-1 prepared in this study demonstrated a high CO_2 uptake capacity of 4.2 mmol/g.It is therefore concluded that this novel and efficient method can be used in the rapid preparation of HKUST-1 with high surface area and CO_2 uptake capacity.     

碱式氧化铝纳米晶的水热合成及表征

利用Al2O3粉末和水之间的水热反应合成了纯相-γAlOOH纳米晶.XRD、FTIR、TEM和TG-DSC等分析测试结果表明:在180℃水热反应10~24 h所得纯相-γAlOOH的形貌从开始的小方块状逐渐转变为薄片状;在200℃水热反应24h所得纯相-γAlOOH的形貌为薄片状.探讨了AlOOH纳米晶在该水热体系中的形成机理.     

L—羟脯氨酸与CuⅡ的螯合物的水热合成及表征

将Ｌ—羟脯氨酸与ＣｕＳＯ４·５Ｈ２Ｏ螯合,经水热合成,得到易溶于水,难溶于酒精的螯合物,以９５％的乙醇进行重结晶,产品经ＩＲ,ＰＨ变化,氧化物灰分分析,元素分析结果表明,生成了一种较稳定的五圆环螯合物Ｃｕ（Ｃ５Ｈ８ＮＯ３）２．     

无机-有机杂化钼磷、钒钼磷多酸化合物的合成与结构

通过对V2 O5 ,Na2 MoO4·2H2 O ,HF ,Ni(NO3) 2 ·6H2 O ,H3PO4和吡啶体系水热反应的研究 ,合成并表征了无机 -有机杂多酸化合物 [C5 H6 N] 3[C5 H5 N][PMo12 O40 ] ( 1 ) ,[C5 H6 N] 4[PVMo11O40 ] ( 2 )和 [C5 H6 N] 4[HPV2 Mo10 O40 ] ( 3 ) .化合物( 1 )属单斜晶系 ,C/ 2c空间群 ,a =2 .1 867( 6)nm ,b =1 .3 978( 4)nm ,c =1 .663 3( 3 )nm ,β =1 0 5.73 ( 1 0 )°,V =4 .893nm3,R =0 .0 60 4 ,Z =4 ;化合物 ( 2 )属单斜晶系 ,C/ 2c空间群 ,a =2 .1 858( 4)nm ,b =1 .3 971 ( 3 )nm ,c =1 .663 5( 3 )nm ,β =1 0 5.83 ( 3 )°,V =4 .8873 ( 1 7)nm3,Z =4 ,R =0 .0 4 63 ;化合物 ( 3 )属单斜晶系 ,P2 1n空间群 ,a =1 .1 1 2 2 ( 2 )nm ,b =1 .94 1 2 ( 3 )nm ,c=1 .2 4 84 ( 3 )nm ,β =99.89( 3 )°,V =2 .6565( 9)nm3,Z =2 ,R =0 .0 690 .     

NiS纳米晶的水热合成及表征

在低温水热条件下,以NiCl2.6H2O、Na2S2O3、硫脲为反应物,制备了金属硫族化合物NiS纳米晶.用X射线粉末衍射(XRD)、透射电镜(TEM)分别对NiS纳米晶的结构及形貌进行了表征分析.结果表明,所得样品为六方晶系的NiS纳米晶;同时采用不同硫源及表面活性剂聚乙烯吡咯烷酮(PVP)可以获得不同形貌的纳米晶.     

十六烷氧基偶氮苯-喹啉化合物合成、表征及性能

以间苯二甲酸为原料,经多步反应合成了1种新型烷氧基偶氮苯-喹啉化合物（E）5-[8-（十六烷氧基）喹啉-5-偶氮]-1,3-苯二甲酸二乙酯,通过IR、UV-Vis和1 H NMR对其结构进行了表征.利用吸收光谱和发射光谱研究了目标化合物的反-顺异构化和发光性能.目标化合物（2.0×10^-5 mol/L的DMF溶液）在365nm紫外光照射下,398nm处的偶氮苯-喹啉结构K带π-π＊跃迁吸收峰及267nm处芳香环的B带π-π＊跃迁吸收峰逐渐减弱,光照7min后达到光稳态.目标化合物（2.0×10^-5 mol/L的DMF溶液）以312nm光激发下,在418nm处发射蓝紫色荧光.     

三乙醇胺-12-钼磷酸电荷转移盐的合成与性质研究

以 1 2 -钼磷酸和三乙醇胺为原料合成了一种新型电荷转移盐 [C6H10 O3 N]3 PMo12 O4 0 ·2H2 O .用C、H、N元素分析 ,ICP ,TG -DTA ,X射线衍射 ,IR、UV光谱对该化合物进行了表征 .结果表明 :1 2 -钼磷酸与三乙醇胺形成电荷转移盐后 ,其阴离子的Keggin结构基本不变 ,但其特征振动峰的位置发生了一定的位移 .还对该电荷转移盐的氧化还原性质及导电性等进行了讨论 .     

烷氧基偶氮苯-喹啉化合物的合成、表征及性能

以间苯二甲酸为原料,经多步反应合成了两种新型烷氧基偶氮苯-喹啉化合物5-[8-(丁氧基)喹啉-5-偶氮]-1,3-苯二甲酸二乙酯(5a)和5-[8-(辛氧基)喹啉-5-偶氮]-1,3-苯二甲酸二乙酯(5b),通过IR、UV-Vis、1 H NMR和MS等对其结构和性能进行了表征.利用吸收光谱和发射光谱研究了目标化合物的反-顺异构化和发光性能.目标化合物5a和5b(2.0×10-5 mol/L的DMF溶液),在365nm紫外光照射下,400nm处的偶氮苯-喹啉结构K带π-π*跃迁吸收峰及267nm处芳香环的B带π-π*跃迁吸收峰逐渐减弱,光照6min后达到光稳态.目标化合物5a和5b(2.0×10-5 mol/L的DMF溶液)均以311nm光激发,分别在420,418nm处发射蓝紫色荧光.