首页 | 本学科首页   官方微博 | 高级检索  
文章检索
  按 检索   检索词:      
出版年份:   被引次数:   他引次数: 提示:输入*表示无穷大
  收费全文   2094篇
  免费   122篇
  国内免费   33篇
化学   1457篇
晶体学   15篇
力学   135篇
数学   344篇
物理学   298篇
  2024年   3篇
  2023年   9篇
  2022年   41篇
  2021年   76篇
  2020年   86篇
  2019年   90篇
  2018年   119篇
  2017年   102篇
  2016年   171篇
  2015年   114篇
  2014年   157篇
  2013年   257篇
  2012年   180篇
  2011年   160篇
  2010年   134篇
  2009年   120篇
  2008年   104篇
  2007年   78篇
  2006年   48篇
  2005年   39篇
  2004年   27篇
  2003年   16篇
  2002年   19篇
  2001年   12篇
  2000年   3篇
  1999年   5篇
  1998年   5篇
  1997年   6篇
  1996年   2篇
  1995年   6篇
  1994年   4篇
  1993年   8篇
  1992年   9篇
  1991年   2篇
  1990年   2篇
  1986年   3篇
  1985年   5篇
  1984年   6篇
  1983年   2篇
  1981年   2篇
  1980年   2篇
  1979年   1篇
  1977年   1篇
  1975年   1篇
  1974年   1篇
  1971年   1篇
  1970年   3篇
  1969年   1篇
  1968年   1篇
  1967年   1篇
排序方式: 共有2249条查询结果,搜索用时 46 毫秒
81.
A magnetic solid phase extraction method based on agarose coated magnetic nanoparticles)ACMNPs(coupled to a new magnetic field agitation (MFA) device was developed and investigated for the separation, preconcentration and determination of Pd(II) in aqueous solutions. For the first time, the formation of the nanoparticles and their encapsulation in agarose micro-flakes was conducted in a single step. For this purpose, preparation of the magnetic iron oxide nanoparticles was performed in an alkaline agarose solution. The sizes of Fe3O4 nanoparticles and agarose micro-flakes were 10–14 nm and 90–130 μm, respectively. The nanomagnetic agarose particles were functionalized by iminodiacetic acid and subjected to magnetic field agitation in the MFA device. The influence of different analytical parameters such as pH, ionic strength, type and volume of desorption solvent and amount of the adsorbent on the preconcentration of Pd(II) were investigated. Eight replicated analysis at the optimized conditions, resulted in a recovery of 94.1% with an RSD of 5.2% for Pd(II). The detection limit of the method (3σ) was 47 ng L−1 for the analyte. The method was successfully applied to the determination of Pd(II) in natural water samples.  相似文献   
82.
A series of β‐hydroxynitriles were efficiently synthesized from the regioselective ring opening of oxiranes by cyanide anion in the presence of silica‐bound 3‐{2‐[poly(ethylene glycol)]ethyl}‐substituted 1‐methyl‐1H‐imidazol‐3‐ium bromide (SiO2? PEG? ImBr) as a novel recoverable phase‐transfer catalyst in H2O (Scheme 1 and Table 2). The workup procedure was straightforward, and the catalyst could be reused over four times with almost no loss of catalytic activity and selectivity.  相似文献   
83.
A simple, efficient and practical procedure for the Biginelli reaction using zinc oxid (ZnO) as a novel and reusable catalyst is described under solvent-free conditions in high yields. The use of this agent is characterized by remarkable reactivity, moderate costs, low toxicity and simple work up procedures.  相似文献   
84.
Benzo[b][1,4]oxazines have been synthesized in good to excellent yields in the presence of the ionic liquid 1-butyl-3-methylimidazolium bromide [bmim]Br under relatively mild conditions without any added catalyst, The method offers the advantages of good yields and short reaction times, and the ionic liquid can be easily separated from the product and reused.  相似文献   
85.
Synthesis of some novel 1,2,4‐triazoles, 1,3,4‐oxadiazoles and 1,3,4‐thiadiazoles bearing a (R) 5‐(1‐(4‐(5‐chloro‐3‐fluoropyridin‐2‐yloxy)phenoxy)ethyl) unit, as a moiety of commercial herbicide, using their thiosemicarbazides in an alkaline, iodine and acidic media is reported, respectively. The structure of the synthesized compounds was characterized by IR, 1H, 13C NMR spectroscopic data, and elemental analyses. The herbicidal activities of synthesized compounds were evaluated against Echinochloa cruss‐galli, Avena fatua, and Sorgum halepense weeds. Compounds 7 and 12a showed potential herbicidal activity against gramineous weeds. Our results may provide some guidance for synthesis development of some novel oxa or thiadiazole and triazole‐based herbicidal lead structures.  相似文献   
86.
Under ultrasound irradiation and in the presence of H2O/Et2NH, ethyl cyanoacetate or malononitrile can combine with α-methylene carbonyl compounds and elemental sulfur to efficiently yield 2-aminothiophene derivatives within a few minutes. Products are easily obtained by simple filtration because of their spontaneous precipitation in the reaction mixtures.  相似文献   
87.
4-Aminoperoxybenzoic acid supported on silica gel was found to be a versatile and efficient oxidant for the oxidation of ketones to esters.  相似文献   
88.
Four‐component reaction of aminodiazines (2‐aminopyrimidine and 2‐aminopyrazine), glyoxal, formaldehyde, and methanol yields trans‐4,5‐dimetoxy‐1,3‐bis(2‐pyrimidinyl)imidazolidine (5a) and trans‐4,5‐dimetoxy‐1,3‐bis(2‐pyrazinyl)imidazolidine (5b), respectively. Changing methanol to acetonitrile leads to the formation of the corresponding 1,3‐bis(2‐pyrimidinyl) and‐1,3‐bis(2‐pyrazinyl)‐ derivatives of trans‐4,5‐dihydroxyimidazolidine (6). Details of the proposed mechanism are discussed.  相似文献   
89.
The sodium salts of the conjugated bases of uracils undergo highly chemoselective O4-monoalkylation when treated with various alkyl halides in dry DMF, while the use of methyl iodide results in N1+N3-dimethylation. Theoretical evaluations of the chemo- and regioselectivity along with X-ray crystallographic data are presented.  相似文献   
90.
Three diamine monomers with different derivatives of imidazole heterocyclic ring and meta-linked aryl ethers were synthesized and used in polycodensation reaction with various commercial dianhydrides for preparation of a series of novel poly(ether-imide) (PEI)s. The polycodensation reactions were carried out by using conventional method and in a green medium of ionic liquid (IL) without using NMP-pyridine-acetic anhydride. The PEIs were obtained in good yields (80% 96%) with moderate viscosity (0.48 0.66 dL/g) in a shorter reaction time (10 h) in IL as compared with the conventional method (36 h). All of the polymers were amorphous in nature, showed excellent solubility in amide-type polar aprotic solvents with ability to form tough and flexible films, and excellent thermal stability with Tgs in the range of 212 340 ℃ and 10% weight loss temperature (T10) up to 570℃ in N 2 and 528 ℃ in air.  相似文献   
设为首页 | 免责声明 | 关于勤云 | 加入收藏

Copyright©北京勤云科技发展有限公司  京ICP备09084417号