杂原子Pb同晶取代Si－ZSM－12中的部分Si及其鉴定

杂原子Ｐｂ同晶取代Ｓｉ－ＺＳＭ－１２中的部分Ｓｉ及其鉴定赵修松，王清遐，李宏愿（中国科学院大连化学物理研究所，大连１１６０２３）关键词Ｐｈ－ＺＳＭ－１２，合成，表征ＺＳＭ－１２属丝光沸石类，具有一维线性非交叉孔道（０．５７×０．６１ｎｍ）［１，２］，...     

乙基二苯甲酰甲烷的合成及表征

乙基二苯甲酰甲烷是一种光吸收性能良好的化合物。该法以苯甲酸乙酯和苯乙酮为起始原料,经克莱森缩合生成二苯甲酰甲烷,再与溴乙烷进行烷基化反应,最后生成乙基二苯甲酰甲烷,并对合成产物进行结构分析及紫外光吸收性能表征。     

新型含金属元素二胺的合成与表征

本文分别用液相法和固相法合成了一系列含不同金属元素的二胺,并通过红外光谱,~1HNMR、~(13)CNMR,紫外光谱,电化学分析及元素分析对其进行表征,还通过DSC和TG对其热性能进行了研究,结果发现这些二胺具有良好的耐热性,是合成一些耐热高聚物的优良原料.     

平朔气煤的煤岩显微组分结构研究

用显微光度计、扫描电子显微镜(SEM)、傅立叶变换红外光谱(FTIR)、X射线衍射光谱(XRD)和X光电子能谱(XPS)等测试手段研究了平朔气煤的等密度梯度离心分离(DGC)显微组分富集物的结构。结果表明,镜质组和稳定组结构相似,含氧基团基本相同,但丝质组结构则不同,它含有较多的羧基和羰基。根据实验结果讨论了三种显微组分的大分子结构,认为它们是由许多结构相似而又不相同的结构单元所构成。镜质组和稳定组的单元核心主要为脂环、缩聚芳环,环数为5—6个;丝质组单元核心主要为缩聚芳环,环数为7—8个,环缩合程度最高,芳香层片在空间排列规则,相互定向程度大。     

Synthesis, Characterization and Thermal Decomposition Mechanism of Cetyltrimethyl Ammonium Tetrathiotungstate

The synthesis, characterization and thermal decomposition mechanism of cetyltrimethyl ammonium tetrathiotungstate （CTriMATT） were studied herein. The as-synthesized CTriMATT was characterized by Elemental analysis, X-ray diffraction （XRD）, Fourier transform infrared （FT-IR）, Ultraviolet visible （UV-Vis） spectra. The results showed that the as-synthesized CTriMATT had high purity and good crystallinity. The introduction of alkyl groups induced a shift of the stretching vibration band of W-S bond to lower wavenumber, while it had no influence on the position of WS4^2-. Thermogravimetric analysis （TG）, differential thermal analysis （DTA） and in situ XRD characterizations revealed that CTriMATT began to decompose at 423 K in nitrogen and was converted to WS2 eventually. In addition, the decomposition product of CTriMATT at 673 K in nitrogen was characterized by N2 adsorption （BET） and scanning electron microscopy （SEM）. The results demonstrated that WS2 with higher specific surface area, and pore volume could be obtained from the thermal decomposition of CTriMATT in nitrogen.     

来曲唑的合成、表征及晶体研究

合成了抗癌药物4,4′-(1H-1,2,4-三唑-1-亚甲基)-双-甲苯基氰,测定了其IR, NMR和单晶结构,晶体C17H11N5属单斜晶系,空间群P21/n,晶胞参数:a=0.70300(14) nm, b=1.6170(3) nm, c=1.3360(3) nm, β=104.80(3)°, Z=4.结构解析最终一致性因子R1=0.0897.分子间通过氢键和范德华力形成超分子结构.     

离聚体的结构表征——Ⅴ.含氟离聚体中离子微区稳定性的研究

本文用DSC方法研究了羟酸型含氟离聚体中不同金属离子种类、可离子化基团含量、配位结构单元构型及离子微区大小对离聚体中离子微区稳定性的影响。实验表明:离聚体中金属离子配位能力愈强,羟酸含量愈高,离子微区尺寸愈大,则相应离聚体中离子微区稳定性愈大。铅高聚体>锌离聚体>钙离聚体>钠离聚体。     

导电性聚西佛碱的研究：Ⅰ含硫聚西佛碱的合成,性能及表征

采用对氯苯甲醛和联苯二胺为原料,合成了4,4′-二氯代苄叉联苯胺,发现该化合物具有热致液晶性。利用所合成的二氯代化合物与硫化钠在醋酸锂催化下缩取得得到了含硫聚西佛碱探讨了高分子量含硫聚西佛碱的合成方法。测出该含硫聚西佛碱具有3.4×10~(-11)S/cm本征导电率。使用红外光谱、元素分析等方法表征了所合成的聚合物。     

Supercritical fluid chromatography of industrial paraffins and waxes

Summary The application of capillary SFC for SIMDIST investigations of paraffins and waxes is reported. Pressure, density and temperature of the mobile phase are optimized to obtain high chromatographic resolution of complex mixtures of industrial products. Isothermal linear pressure programming and asymptotic pressure and density programming are used in the range from 15 to 35 MPa in the isothermic mode above 100°C. SFC chromatograms of natural and synthetic paraffins, microcrystalline wax and candle wax are compared. The retention behaviour of paraffin mixtures and waxes has been investigated on methyl/phenyl and biphenyl capillary columns. The polarity of the stationary phases influences the absolute retention time more than it influences the chromatographic resolution.     

Thermal characterization of social vespid silk

In this paper we try to establish a link between the microclimate in the wasp nest and the structure and thermal stability of vespid silk. We suggest that there are at least two types of water that is absorbed by the silk of Oriental hornets, namely, surface water and intrinsic structural water. The release of both types of water was found to be reversible. The enthalpy values of the endothermic peaks associated with the release of water from different silk samples do not differ substantially and are in the range of 106 to 130 J g^-1 for the Vespa orientalis male larvae silk (sample #1), Paravespula germanica (yellowjacket) worker larvae silk (#3) and Vespa orientalis nest envelope(#4). For the Vespa orientalis worker larvae silk (sample #2), however, it is twice as large (228 J g^-1). This is in agreement with the increased total amount of absorbed water. The silk studied has a fibrilar structure with interconnecting surfaces overlying entire regions. It is assumed that the initial water loss stems from water evaporation from the coat of the fibers - a daily occurrence in the hornets' nest. Heating to above 70°C may result in structural changes in the silk core. This revised version was published online in July 2006 with corrections to the Cover Date.