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1.
Novel chiral stationary phases based on peptoid combining a quinine/quinidine moiety through a C9‐position carbamate group 下载免费PDF全文
Haibo Wu Dongqiang Wang Guangjun Song Yanxiong Ke Xinmiao Liang 《Journal of separation science》2014,37(8):934-943
By connecting a quinine or quinidine moiety to the peptoid chain through the C9‐position carbamate group, we synthesized two new chiral selectors. After immobilizing them onto 3‐mercaptopropyl‐modified silica gel, two novel chiral stationary phases were prepared. With neutral, acid, and basic chiral compounds as analytes, we evaluated these two stationary phases and compared their chromatographic performance with chiral columns based on quinine tert‐butyl carbamate and the previous peptoid. From the resolution of neutral and basic analytes under normal‐phase mode, it was found that the new stationary phases exhibited much better enantioselectivity than the quinine tert‐butyl carbamate column; the peptoid moiety played an important role in enantiorecognition, which controlled the elution orders of enantiomers; the assisting role of the cinchona alkaloid moieties was observed in some separations. Under acid polar organic phase mode, it was proved that cinchona alkaloid moieties introduced excellent enantiorecognitions for chiral acid compounds; in some separations, the peptoid moiety affected enantioseparations as well. Overall, chiral moieties with specific enantioselectivity were demonstrated to improve the performance of peptoid chiral stationary phase efficiently. 相似文献
2.
吡咯烷酮酸性离子液体的合成及其对酯化反应的催化活性 总被引:19,自引:0,他引:19
合成并表征了 2-吡咯烷酮硫酸氢盐([Hnhp]HSO4)、 1-甲基-2-吡咯烷酮硫酸氢盐([Hnmp]HSO4)、 1-甲基咪唑硫酸氢盐([Hmim]HSO4)、 1-(3-磺酸基)-丙基-3-甲基咪唑硫酸氢盐([C3SO3Hmim]HSO4)和1-(3-磺酸基)-丙基-2-吡咯烷酮硫酸氢盐([C3SO3Hnhp]HSO4)等以HSO-4为阴离子的质子酸离子液体,并以乙酸和正丁醇的酯化反应考察了这些离子液体的催化活性.结果表明,当n(n-BuOH):n(MeCO2H):n([C3SO3Hnhp]HSO4)=1.2:1:0.005,反应温度为120 ℃和反应时间为 1 h 时,酯收率可达99%以上;反应结束后离子液体与酯产物可分成两相,而且该离子液体重复使用8次,催化活性没有明显下降.探讨了阳离子结构及Brnsted酸性对催化活性的影响,考察了离子液体与酯化反应相关组分的互溶性.结果表明,离子液体的分相性能对催化效果有较大的影响,离子液体的催化活性与其酸性、溶解性密切相关. 相似文献
3.
吗啡啉功能化酸性离子液体的合成、表征及其催化酯化性能 总被引:6,自引:0,他引:6
制备和表征了三种新型质子酸离子液体: 吗啡啉硫酸氢盐([Hnhm]HSO4)、4-甲基吗啡啉硫酸氢盐 ([Hnmm]HSO4)和SO3H-功能化的4-(3-磺丙基)吗啡啉硫酸氢盐([C3SO3Hnhm]HSO4). 以氯乙酸(CAA)和乙醇合成氯乙酸乙酯的酯化反应考察了它们的酸性和催化活性, 并与1-(3-磺酸基)丙基-3-甲基咪唑硫酸氢盐、1-(3-磺丙基)吡啶硫酸氢盐、1-(3-磺丙基)-2-吡咯烷酮硫酸氢盐等三种具有不同氮杂环的SO3H-功能化酸性离子液体以及浓硫酸相对照. 结果表明, 上述SO3H-功能化离子液体对酯化反应的催化性能比非SO3H-功能化的[Hnhm]HSO4和[Hnmm]HSO4都高, 等同甚至优于浓硫酸. 当反应条件为: n(EtOH)∶n(CAA)∶n([C3SO3Hnhm]HSO4)=1.3∶1∶0.2, 反应温度80 ℃, 反应时间3 h, 酯收率可达93.4%. 而且离子液体经真空干燥重复使用9次, 催化活性仍无明显下降. 以[C3SO3Hnhm]HSO4催化乙酸和不同醇的酯化反应获得较高的酯收率和选择性, 离子液体跟酯产物均能自动分相. 还考察了SO3H-功能化酸性离子液体对奥氏体316不锈钢的腐蚀性. 尽管SO3H-功能化离子液体与硫酸的酸性相近, 但对钢试样的腐蚀率不到硫酸的1/3. 相似文献
4.
Electronic absorption spectrum, photoacoustic absorption spectrum and ESR spectrum of bis(L-histidine)copper(II) dinitrate dihydrate crystal were recorded. The experimental results are discussed quantitatively with ligand field theory (LFT) and the radial wave function of non-free copper(II). Our calculations coincides well with the experimental results, and in particular, provides significant correlations between the spectra and coordination structures. The ESR spectrum gives some information about the restudy of classification for the ESR spectra of bis(amino acidato)copper(II) complexs. Additionally, the differences between crystal and frozen solution spectra due to the variance of PH are also reported for the title compound. 相似文献
5.
CPA矩阵分光光度法同时测定三种酚 总被引:4,自引:2,他引:2
在无水乙醇介质中,对乙酰胺基酚,对氨基酚、对硝基酚三者的紫外吸收光谱相互严重重叠,用一般的光度分析手段无法同时测定。本文首次采用CPA矩阵法,不经分离直接测定了上述三组分的含量,实验结果表明:当选取216、234、260、292、312nm5个波长点作为CPA矩阵程序的最佳波长点时,该法对样品中各组分的平均回收率在100.2%-103.5%之间,结果较满意,与现行分析方法相比,本方法具有简便、快速的优点。本法已用于扑热息痛合成物中三组分含量的测定。 相似文献
6.
以单分散SiO2 胶态晶体球形成的三维有序结构为模板 ,利用胶体晶模板技术合成了三维长程有序的二氧化锰大孔材料 .通过X射线粉末衍射 (XRD)和扫描电子显微镜 (SEM)对产物进行了表征 .其中XRD数据显示所得产物为纯四方相二氧化锰 .SEM结果表明 ,所合成的二氧化锰大孔材料孔大小均匀 ,空间排列高度有序 ,很好地复制了SiO2 胶态晶体球的自组装方式 .此外 ,对三维有序二氧化锰大孔材料的合成过程进行了分析 ,研究了前体填充次数对产物孔结构的完整性和有序性的影响 ,还发现产物孔径的收缩存在异常现象 . 相似文献
7.
Poly (vinyl alcohol) (PVA)–functionalized β-cyclodextrin (β-CD) polymer crosslinked by citric acid (PVA-g-CD) was synthesized, characterized and evaluated for the catalytic oxidation of cinnamaldehydes. The polymer showed good activity and selectivity to aldehydes for some structurally diverse cinnamaldehydes. The enhanced catalytic activity may be attributed to the synergistic effect of the intermolecular weak interactions between β-CD and the functional group of PVA. In addition, calcium peroxide as a solid oxidant was found to significantly affect the reaction. This catalyst can be recovered and reused for five times without a significant loss in its activity and selectivity. 相似文献
8.
Yunchuan Pu Mingang Zhao Xu Liang Shaoyu Wang Dr. Hongjian Wang Ziting Zhu Dr. Yanxiong Ren Zhiming Zhang Prof. Guangwei He Prof. Dan Zhao Prof. Zhongyi Jiang 《Angewandte Chemie (International ed. in English)》2023,62(22):e202302355
We report a covalent organic framework (COF) induced seeding strategy to fabricate metal–organic framework (MOF) membranes. Contrary to graphene oxide nuclei-depositing substrate, COF substrate has uniform pore size, high microporosity and abundant functional groups. We designed a series of charged COF nanosheets to induce the formation of ZIF-8@COF nanosheet seeds with high aspect ratio over 150, which were readily processed into a compact and uniform seed layer. The resulting ZIF-8 membranes with thickness down to 100 nm exhibit an ultrahigh C3H6/C3H8 separation performance and superior long-term stability. Our strategy is also validated by fabricating ultrathin ZIF-67 and UiO-66 membranes. 相似文献
9.
Synthesis and evaluation of a maltose‐bonded silica gel stationary phase for hydrophilic interaction chromatography and its application in Ginkgo Biloba extract separation in two‐dimensional systems 下载免费PDF全文
Qianying Sheng Kaiya Yang Yanxiong Ke Xinmiao Liang Minbo Lan 《Journal of separation science》2016,39(17):3339-3347
Maltose covalently bonded to silica was prepared by using carbonyl diimidazole as a cross‐linker and employed as a stationary phase for hydrophilic interaction liquid chromatography. The column efficiency and the effect of water content, buffer concentration, and pH value influenced on retention were investigated. The separation or enrichment selectivity was also studied with nucleosides, saccharides, amino acids, peptides, and glycopeptides. The results indicated that the stationary phase processed good separation efficiency and separation selectivity in hydrophilic interaction liquid chromatography mode. Moreover, a two‐dimensional hydrophilic interaction liquid chromatography× reversed‐phase liquid chromatography method with high orthogonality was developed to analyze the Ginkgo Biloba extract fractions. The development of this two‐dimensional chromatographic system would be an effective tool for the separation of complex samples of different polarities and contents. 相似文献
10.
Sheming Lu Yanxiong Ke Jianmin Li Shuxi Zhou Xintao Wu Wenxin Du 《Crystal Research and Technology》2003,38(11):1004-1008
Mixing the malonate (mal), 4,4′‐bipyridine, UO2(CH3COO)2 · 2H2O in different solvent condition gets two compounds (bpy)2(H2bpy)[UO2(mal)2(μ‐H2O)] · 8H2O (1) and (H2bpy)[UO2(mal)2] · 2H2O (2) . Both complexes contain seven‐coordinated pentagonal bipyramidal uranium center. Crystal 1 is mononuclear structure and crystal 2 contains dinuclear [(UO2)2(mal)2(μ2‐mal)2]4‐ subunit. Particularly, Crystal 2 forms the twodimensional supramolecular topology by hydrogen bonds. The sheet constructs from two sorts of chamber, of which the larger one has two water molecular guests. (© 2003 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim) 相似文献