[Ni(dien)2]2[Mn(NCS)6]·H2O的合成、晶体结构

The crystal of [Ni(dien)₂]₂[Mn(NCS)₆]·H₂O was synthesized and the structure of its single crystal was determined by X-ray diffraction. The crystal is monoclinic system, space group P2₁/c with a=16.544(3),b=15.137(2), c=17.334(3)?, β=99.90(1)°, V=4276.3(12)?³, Z=4, D_c=1.479g·cm^-3, M_r=951.55, F(000)=1998, μ=1.489mm^-1, R=0.0399, R_w=0.0958. IR was also determined.     

K-Pb-Tl-O复合氧化物的合成和电子结构的XPS研究

用熔盐阳极电沉积法合成了导电的复合氧化物K-Pb-Tl-O晶体.这些晶体具有纳米尺寸层状结构.用XPS对其进行了表征,并与相关的化合物进行了比较.实验表明,氧化物中的Pb和Tl都以高价态的单一价态存在,但电子结合能比相应的非导电低价化合物的低.该文用原子外弛豫效应解释了复合氧化物中的Pb和Tl的结合能的反常现象.讨论了它们的价电子结构与导电性的关系.     

锆氧杂环络合物合成方法探索

邻甲氧基苯基锂和 6,6-二甲基富烯 (或 6,6-二乙基富烯 )反应得配体锂盐 ( Cp′ Li) ,Cp′ Li直接和 Cp Zr Cl3· DME反应生成 2个新的锆络合物 Cp′ Cp Zr Cl2 。 BBr3和 Li Br分别用来使 Cp′ Cp Zr Cl2 环化 ,发现在相同条件下 BBr3比 Li Br3更有效。Cp′ Cp Zr Cl2 通过和 BBr3反应得到 2个新的锆氧杂环络合物。 4个新的锆络合物经元素分析、1 H NMR和 MS确证     

Determination of volatile components in peptic powder by gas chromatography-mass spectrometry and chemometric resolution

Gas chromatography-mass spectrometry (GC-MS) coupled with chemometric resolution upon two-dimensional data was proposed as a method for the analysis of volatile components in a traditional Chinese medicinal preparation peptic powder which contains Rhizoma Atractylodis, Pericarpium Citri Reticulatae, Cortex Magnoliae Officinalis and Radix Glycyrrhizae. Ninety-three components were separated and 65 of them were qualitatively and quantitatively analyzed which represented about 90.28% of the total content. With the help of chemometric resolution, the data were resolved into a pure chromatogram and a mass spectrum of each chemical component. The accuracy of qualitative and quantitative results was greatly improved by using the two-dimensional comprehensive information of chromatograms and mass spectra. The example showed that chemometric resolution could greatly enhance separation ability. This makes it possible to analyze complicated practical systems like traditional Chinese medicinal preparations with the help of coupled instruments and chemometric resolution methods.     

尼龙66/蒙脱土复合材料结晶行为的研究

在密炼机中采用熔融共混法制备蒙脱土重量分数为 2 5 %、4 5 %的尼龙 6 6 /蒙脱土复合材料 .通过DSC法对非等温结晶行为及在 2 2 8～ 2 4 0℃范围内的等温结晶行为进行研究 ,并与纯尼龙 6 6进行比较 .从其等温和非等温结晶行为的研究表明 ,蒙脱土起成核剂的作用 ,它的填入使尼龙 6 6结晶速率提高 ,但填料与基体间的相互作用使其链段运动困难 ,结晶活化能提高 ;在研究的填料含量变化范围内 ,结晶行为变化不大 ,并且找到该复合材料在 2 2 8～ 2 34℃范围结晶对温度的不敏感区 ;对非等温结晶过程分析 ,刘结平 莫志深方程是适用的 ,而Ozawa方程则是不适用的 .     

通道离子替换磷灰石固溶体比较晶体化学XRD研究

采用单相共沉淀法和隋性气体保护下的固相反应法制备了不同通道离子替换固溶体磷灰石[X₁-X₂AP]。利用XRD对通道离子替换磷灰石固溶体进行了比较晶体化学研究,结果表明:晶胞参数随通道离子半径的增大,a₀增大,c₀反而减小,且OH-ClAP和F-OHAP变化呈线性关系,符合Vegard定律,而F-ClAP在富F^-端的变化不呈线性关系;由于[PO₄]四面体沿[101]方向的滑移,c₀随a₀的变化而变化,且c₀^-2与a₀^-2呈线性关系[c₀^-2=-a₀^-2+3.2348]。     

Syntheses and characterizations of three-dimensional channel-like polymeric lanthanide complexes constructed by 1,2,4,5-benzenetetracarboxylic acid

The hydrothermal reaction of YbCl(3) small middle dot6H(2)O with 1,2,4,5-benzenetetracarboxylic dianhydride resulted in [[Yb((b)btec)(1/4)((d)btec)(3/6)(H(2)O)(2)](4).6H(2)O](n)() (1) (H(4)btec = 1,2,4,5-benzenetetracarboxylic acid), and the solvothermal reaction of Er(NO(3))(3) small middle dot6H(2)O or TbCl(3).6H(2)O with 1,2,4,5-benzenetetracarboxylic dianhydride in H(2)O/acetic acid gave rise to [[Er(2)((c)btec)(2/4)((e)btec)(2/4)((f)btec)(2/4)(H(2)O)(4)].4H(2)O](n)() (2) and [[Tb(H(2)btec)(2/4)((f)btec)(3/6)(H(2)O)].2H(2)O](n)() (3), respectively. Complex 1 crystallizes in monoclinic space group C2/m with a = 20.8119(5) A, b = 17.6174(1) A, c = 5.7252(2) A, beta = 92.324(1) degrees, and Z = 1. 1 possesses a three-dimensional framework consisting of eight-coordinate ytterbium centers and two kinds of channels along the c axis. Complex 2 crystallizes in triclinic space group P with a = 9.6739(5) A, b = 11.0039(5) A, c = 11.5523 A, alpha = 104.8330(10) degrees, beta = 91.0000(10) degrees, gamma = 114.2570(10) degrees, and Z = 2. 2 has a three-dimensional framework comprising both eight- and nine-coordinate erbium centers and channels along the a axis. Complex 3 crystallizes in monoclinic space group P2(1)/n with a = 10.7246(12) A, b = 7.1693(9) A, c = 17.158(2) A, beta = 97.109(2) degrees, and Z = 4. 3 shows a three-dimensional framework containing nine-coordinate terbium centers and channels along the b axis. Uncoordinated water molecules occupy the channels in the three complexes. TGA and XRPD were determined for the three complexes, and the results illustrate that the framework of 1 is retained upon removal of uncoordinated and coordinated water molecules.     

新型高吸水聚合物凝胶型屏蔽暂堵剂MTC-1的合成及性能

以丙烯酸（AA）、丙烯酰胺（AM）、2-丙烯酰胺基-2-甲基丙磺酸（AMPS）为原料，蒙脱土（MMT）为改性剂，过硫酸钾和无水亚硫酸氢钠为氧化还原引发体系，六亚甲基四胺（C₆H₁₂N₄）为交联剂，采用水溶液聚合法合成了一种新型高吸水聚合物凝胶型屏蔽暂堵剂（MTC 1），其结构经IR表征。在最优合成条件（AM/AMPS/AA=11/7/1, m/m/m，引发剂加量0.6 wt%，于45 ℃反应2.5 h）下，MTC-1的最大吸水倍率为1006倍。岩心流动实验结果表明：MTC-1的堵水性能较高，封堵效率达到83.72%。     

三氟化硼引发四氢呋喃聚合的研究——以环氧氯丙烷为促进剂

<正> 四氢呋喃(THF)通过正离子开环聚合而制得的聚丁二醇(PTMG)是生产嵌段聚醚聚氨酯及嵌段聚醚聚酯弹性材料的重要原料。目前制备PTMG所采用的引发剂都是强酸型的,如高氯酸、氟磺酸或发烟硫酸等,对设备腐蚀严重。用酸性较弱的三氟化硼引发聚合在文献上也有一些研究报道,但尚难以采用,其主要困难在于实际应用的     

地锦草总黄酮最佳提取分离工艺的研究

采用四因素三水平的正交实验方法,对地锦草总黄酮的最佳提取工艺进行了探索.采用乙酸乙酯萃取、酸碱沉淀、铅盐沉淀3种方法,对其最佳分离工艺进行了探索.正交实验结果表明:温浸法中四因素对地锦草黄酮的影响顺序为乙醇浓度>样液比>提取温度>提取时间.通过实验得到了地锦草总黄酮的最佳提取工艺:以10倍体积的50%的乙醇水溶液在80℃浸提1 h.地锦草总黄酮的最佳分离方法为酸碱沉淀法.这些数据为中药地锦草的开发和应用提供了科学依据.