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21.
SHEN Yu-Feng WANG Qing-Hai ZHU Dao-Qian ZHOU Liang-Mo Dalian Institute of Chemical Physics Chinese Academy of Sciences Dalian Liaoning China 《中国化学》1994,12(2):129-137
The study on retention behavior in supercritical fluid chromatography (SFC) is necessary to understand the mechanism of the various interactions in SFC. The retention of SFC in carboxylic acid methyl ester/polymethylsiloxane/CO2 system was studied systematically and the retention behavior of this kind of compounds under various typical operation conditions was described using the method of an alternative unified theory of chromatographic retention. The results illustrated that expression: Ink.= a + b/T + cp + dp/T + ep2/T can be used to describe quantitatively the retention behavior of carboxylic acid methyl ester/polymethylsiloxane/CO2 system in the ranges of reduced density from 0.549 to 1.411. It was also found that the entropy of solute in stationary phase is dependent on the density of supercritical fluid (SF) under typical operating conditions of SFC. 相似文献
22.
Xing Chen Wenguang Zhao Feng Wang Jie Xu .Dalian National Laboratory for Clean Energy State 《天然气化学杂志》2012,(5):481-487
Preparation of dispersed transition metal oxides catalyst with low oxidation state still remains a challenging task in heterogeneous catalysis.In this study,vanadium oxides supported on zeolite SBA-15 have been prepared under hydrothermal condition using V 2 O 5 and oxalic acid as sources of vanadium and reductant,respectively.The structures of samples,especially the oxidation state of vanadium,and the surface distribution of vanadium oxide species,have been thoroughly characterized using various techniques,including N 2-physisorption,X-ray diffraction(XRD),transmission electron microscopy(TEM),X-ray photoelectron spectroscopy(XPS),UV-visible spectra(UV-Vis) and UV-visible-near infrared spectra(UV-Vis-NIR).It is found that the majority of supported vanadium was in the form of vanadium(IV) oxide species with the low valence of vanadium.By adjusting hydrothermal treatment time,the surface distribution of vanadium(IV) oxide species can be tuned from vanadium(IV) oxide cluster to crystallites.These materials have been tested in the hydroxylation of benzene to phenol in liquid-phase with molecular oxygen in the absence of reductant.The catalyst exhibits high selectivity for phenol(61%) at benzene conversion of 4.6%,which is a relatively good result in comparison with other studies employing molecular oxygen as the oxidant. 相似文献
23.
LI Cun-man XIAO Yuan-sheng XUE Xing-ya FENG Jia-tao ZHANG Xiu-li LIANG Xin-miao . Dalian Institute of Chemical Physics Chinese Academy of Sciences Dalian P. R. China . Hebei Research Centre of Analysis Testing Hebei University of Science Technology Shijiazhuang 《高等学校化学研究》2011,(3):392-396
An efficient preparative method was successfully developed for isolation and purification of unstable components from medicinal plant extracts, using a combined method of preparative high performance liquid chro-matography(HPLC) and solid-phase extraction(SPE). The aim of this study was to obtain an effective method with high preparative efficiency and importantly to avoid the transformation of unstable compounds. The preparative HPLC system was based on an LC/MS controlled four-channel autopurification sys... 相似文献
24.
ZENG ZhenHua MA XiuFang DING WuChen & LI WeiXue State Key Laboratory of Catalysis Center for Theoretical Computational Chemistry Dalian Institute of Chemical Physics Chinese Academy of Sciences Dalian China 《中国科学:化学》2010,(2)
Combined with third generation synchrotron radiation light sources, X-ray photoelectron spectroscopy (XPS) with higher energy resolution, brilliance, enhanced surface sensitivity and photoemission cross section in real time found extensive applications in solid-gas interface chemistry. This paper reports the calculation of the core-level binding energy shifts (CLS) using the first-principles density functional theory. The interplay between the CLS calculations and XPS measurements to uncover the structures,... 相似文献
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The construction of an automated adiabatic calorimeter for heat capacity measurement ofsolids in the temperature range of 25- 90K is described in detail. The sample vessel of thecalorimeter has thin radial vanes which make no contact with its inner wall and are distrib-uted evenly, thus greatly improving the internal thermal equilibration of the vessel. Theprecision of temperature control for the adiabatic shields and electrical leads of the calori-metric system are heightened to a great extent by using the high precision ACD- 79 modeladiabatic controller specially developed by us for this purpose. Measurements of the heatcapacities of high purity α-Al_2O_3, one of the internationally-accepted standard referencematerials, agree with those of the National Bureau of Standards (NBS), USA within ±0.3%,demonstrating the reliability of this apparatus. 相似文献
27.
本文报导了傅里哀变换红外发射光谱法研究多相氧化物催化剂的实验装置的建立及实验条件的考察。设计加工了一个温度范围宽,可在各种气氛和真空条件下原位研究氧化物催化剂的红外发射池。以MoO_3为例,考察了样品厚度,测试温度对发射光谱的影响。当样品量小于1mm·cm~(-2)时,随样品量增加,谱峰强度线性增加,但峰形不发生变化。当样品量高于1mg.cm~(-2)时,随样品量增加,谱图严重畸变。随样品温度升高,谱峰强度近似线性增加。并用该方法研究了MoO_3在还原和再氧化过程中表面氧物种的变化。结果表明桥式MO?O?Mo物种比端基Mo=O物种较易还原,再氧化时,Mo=O物种比Mo?O?Mo物种优先形成。 相似文献
28.
Xiao Chi Ma Bao Jing Zhang Sha Deng Shan Shan Huang Ke Xin Liu Jing Ming Jia 《中国化学快报》2009,20(3):317-319
A new ent-labdane diterpenoid lactone with a new natural product was isolated from Andrographis paniculata. Their structures were elucidated on the basis of spectral evidences including 2D NMR. 相似文献
29.
Study on Bifunctionality of Mo/HZSM-5 Catalysts for Methane Dehydro-Aromatization under Non-oxidative Condition
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Lingling Su Yide Xu Xinhe BaoState Key Laboratory of Catalysis Dalian Institute of Chemical Physics Chinese Academy of Sciences Zhongshan Road P. O. Box Dalian ChinaManuscript received June revised July 《天然气化学杂志》2002,(Z1)
The optimum Mo/[H~+] ratio per unit cell of the active precursors in Mo/HZSM-5 catalysts for methane dehydro-aromatization, measured by 1H MAS NMR, was found to be about 1 when adjusting the acid sites by altering either the SiO2/Al2O3 ratios or the Mo loading. This implies that a concerted interaction between the Mo species and the Bronsted acid sites probably features the bifunctionality of the Mo/HZSM-5 catalyst. On the other hand, it was found that the driving force for Mo species to move into the HSZM-5 zeolite channels and the interaction between the Mo species and the Bronsted acid sites are closely and proportionably related with the amount of Bronsted acid sites per unit cell. 相似文献
30.
丙烯环氧化反应中失活钛硅分子筛的无氧脱附研究 总被引:3,自引:0,他引:3
采用无氧脱附方法对丙烯环氧化中失活的薄层钛硅分子筛(即Spent EPO-4)和环氧丙烷(PO)与丙二醇单甲醚(MME)浸渍的TS-1催化剂(即PO/TS-1和MME/TS-1)进行了研究,脱附产物由气相色谱定性分析,无氧脱附后的催化剂以丙烯环氧化为探针反应进行再生性能评价,同时在无氧条件下考察了TS-1在300℃时催化裂化PO反应.实验结果表明:PO浸渍TS-1可使其活性明显下降,PO在TS-1上不是简单的弱吸附,存在着化学强吸附和自聚.失活催化剂(Spent EPO-4和PO/TS-1)经无氧脱附后,其催化活性可显著恢复.通过对失活催化剂脱附产物的比较,推测了丙烯环氧化反应过程中钛硅分子筛失活原因. 相似文献