[NEt~4][Mn(salophen)(H~2O)~2]~2[Fe(CN)~6]·H~2O· CH~3OH超分子化合物的 合成和结构

室温下将[NEt~4]~3[Fe(CN)~6]和[Mn(salophen)(H~2O)(CH~3OH)]ClO~4反应,得到了超分子化合物[NEt~4][Mn(salophen)(H~2O)~2]~2[Fe(CN)~6]·H~2O·CH~3OH(salophenH~2=双水杨醛缩邻苯二胺),并对其进行了晶体结构测定。结果表明,该晶体属三斜晶系,空间群P1,晶胞参数a=1.2150(4)nm,b=1.4834(6)nm,c=1.6625(6)nm,α=81.896(7)°,β=76.980(8)°,γ=81.120(6)°,V=2.872(2)nm^3,Z=2,D~c=1.388g·cm^-^3。晶体的各部分间以氢键连接成网状超分子体系。     

[Mn3O(O2CC6H5)6(C3H4N2)3]·C6H5CO2·0.5H2O的 合成、晶体结构及磁性质

Mn(O2CMe)2·4H2O、咪唑、苯甲酸和N(n-Bu)4MnO4在无水乙醇溶剂中反应,制备得到锰的三核μ3-O桥联配位化合物[Mn3O(O2CC6H5)6(C3H4N2)3]·C6H5CO2·0.5H2O.该配位化合物的X射线单晶衍射表明,其属于单斜晶系,空间群P21/C,晶胞参数：a=1.52832(19)nm,b=1.9722(2)nm,c=2.1023(3)nm,β=92.597(3)°,Z=4.变温磁化率(5～280K)研究表明,该配位化合物中3个锰离子在低温下存在弱的反铁磁性耦合,交换积分J=-2.34cm^-1。     

配合物[Mn(bipy)3](ClO4)2的晶体结构和热分析研究

The complex [Mn(bipy)₃]·(ClO₄)₂ was synthesied and characterized by X-ray diffraction. X-ray diffraction result for the single crystal showed that the crystal belongs to triclinic, space group P1, a=0.8123(2),b=1.1024(2), c=1.8646(4)nm,α=102.30(3)°,β=91.00(3)°,γ=99.69(3)°,V=1.6056(6)nm³,Z=2,D_c=1.494g·cm^-3. The thermal decomposition of [Mn(bipy)₃](ClO₄)₂ occurred in a three steps pattern. The reaction mechanism of the first step decomposition was deduced as n(1-α)[-ln(1-α)](n-1)/n with the activation energy of 130kJ·mol^-1.     

顺酐常压催化加氢制γ-丁内酯

顺丁烯二酸酐;顺酐常压催化加氢制γ-丁内酯     

咪唑配位的夹心型杂多化合物Na_9[{Na(H_2O)}_3{Co(C_3H_4N_2)}_3(BiW_9O_(33))_2]·33H_2O的合成，结构和磁性质研究

在pH=7.5的水溶液中，咪唑与Na_2WO_4,Bi(NO_3)_3及Co(NO_3)_2反应，得到 了咪唑配位的新型杂多钨酸盐Na_9[{Na(H_2O)}_3{Co(C_3H_4N_2)}_3(BiW_9O_(33) )_2]·33H_2O，用X射线单晶衍射法及元素分析确定了其结构，晶胞参数为：空间 群P3，a=1.3904(4)nm, b=1.3904(4)nm, c=3.3169(13)nm, γ=120 °,V=5.553(3) nm~3, Z=2, R_1=0.0361，wR_2=0.0507(I>2σ)。杂多阴离子[{Na(H_2O)_3}{Co (C_3H_4N_2)}_3(BiW_9O_(33))_2]~(9-)为夹心式结构，两个三空缺Keggin离子α- B-BiW_9O_(33)~(9-)夹层中的中心离子为交替排列的三个Na(H_2O)~+和三个Co (C_3H_4N_2)~(2+)，中心离子钴的配位数为5，该杂多阴离子具有C_(3v)对称性。 对标题化合物进行了磁性质表征，拟合结果为J=6.90cm~(-1),g=2.10,θ=0.25K， 表明该化合物中的Co(II)三核簇存在着铁磁偶合。     

纳米图案化高分子凝胶的制备

A new method was proposed to prepare binary composite colloidal crystal hydrogels by interlocking the as-prepared polystyrene/sulfonated polystyrene core/shell colloidal crystal hydrogel with a second responsive gel. The shell thickness thus the core size were synchronously controlled by altering the sulfonation time and temperature. The proper monomers were radically polymerized forming the second gel within the first gel network. The composition and structure were confirmed. Nanopatterued hydrogel including porous bulk hydrogels and surface patterned hydrogels were derived by properly treating the binary composite hydrogels. Specially, some typical patterns such as arrays of “nano-bowls” ,arrays of “nano-ribbons” and “nano-mask” were achieved by changing the treatment method such as by immersion in the solvent, after solvent evaporation from the sample surface during high rate rotation. This work provides a method to prepare nanopatterued hydrogels.     

原子吸收光谱法测定莲子和莲子心中7种金属元素含量

利用火焰原子吸收光谱法测定6种不同产地的湘莲莲子和莲子心中7种金属元素含量. 莲子和莲子心样品经粉碎干燥后, 用硝酸-高氯酸混合液进行消解处理,采用火焰原子吸收光谱法测定样品中Cr、Cu、Zn、Fe、Mn、Pb、Cd的含量. 莲子和莲子心中富含微量元素Fe、Mn、Zn、Cu、Cr,有害金属元素Pb和Cd未检出. 各元素的加标回收率为98.58%~101.53%,RSD在0.78%~1.89%之间. 方法快速、简便、灵敏,结果准确可靠,为莲子和莲子心中金属元素含量测定提供了一种可靠的方法.     

季铵盐双子表面活性剂的合成及其杀菌性能研究

以N,N,N',N'-四甲基乙二胺和溴代烷烃为原料合成了系列对称型季铵盐双子表面活性剂n-2-n(n=8,10,12,14),其结构经1H NMR表征.研究了n-2-n对油田污水中常见的硫酸盐还原菌(SRB),铁细菌(FB)和腐生菌(TGB)的杀菌性能.结果表明:与传统杀菌剂1227相比,n-2-n对SRB,FB和TG...