相转移催化氧化合成苯甲酸

苯甲酸一般由甲苯氧化而成 ,工业上采用液相空气氧化生产苯甲酸[1 ] 。ＫＭｎＯ4氧化甲苯制备苯甲酸的方法是在实验室中最常见的一种方法[2 ] ,该法的优点是反应条件温和 ,操作简便 ;其缺点是反应时间长 ,产率低 (低于 40 % ) [3] 。为了提高ＫＭｎＯ4氧化法的产率 ,本文采用十六烷基三丁基溴化磷 (ＨＤＴＢＰ)和苄基三乙基氯化铵(ＢＴＥＡ)作相转移催化剂氧化甲苯制备苯甲酸 ,具有时间短 ,收率高等优点。同时又考虑到ＨＤＴＢＰ的催化效果虽然好 ,但价格昂贵 ,因此本文采用价廉易得的苄基三乙基氯化铵 (ＢＴＥＡ)作相转移催化剂氧化甲苯制…     

Effect of La_2O_3/γAl_2O_3 Catalyst on the Activation of CH_4 and CO_2 to C_02 Hydrocarbons under Non-equilibrium Plasma

The oxidative coupling of methane (OCM) to C2 hydrocarbons using carbon dioxide as oxidant is an attractive process from environmental point of view. Only a few research papers reported for it1-3. In general, the yield of C2 hydrocarbons was about 6%. This indicated that the method of catalytic activation was unfavorable to the reaction. It is necessary for us to find a new method in order to activate reaction and improve C2 hydrocarbon yield. Non-equilibrium plasma is a cold plasma in…     

嘧啶基苯硫甲基磺酰脲化合物的合成及除草活性

４，６－二氯－２－嘧啶基苯硫甲基磺酰脲与甲醇钠反应，合成了１５个 见文献报道的标题化合物。它们的结构经ＩＲ，＾１ＨＮＭＲ，ＭＳ，元素分析证实。其中一类化合物具有较强除草活性。     

Synthesis of Tetra—Schiff Base Macrocyclic Compound Containing Benzo—12—crown—4

Tetra-Schiff base macrocyclic compound containing benzo-12-crown-4 was synthesized via condensation of 2,6-diformyl-4-methyl-phenol with 4′，5′-diaminobenzo-12-C-4 promoted by proton. The compound was characterized by MS,IR ^1HNMR spectroscopy and elemental analysis.     

气相色谱-负化学源质谱联用法测定菊酯类农药

通过固相萃取-气相色谱-负化学离子源质谱技术建立了11种拟除虫菊酯类农药残留的检测方法，并应用于茶叶农残检测。样品经乙酸乙酯提取后，用串联的活性炭和中性氧化铝固相萃取柱选择性地富集茶叶中待测组分，再由气相色谱-负化学离子源质谱分时段选择离子监测技术进行测定。方法简单快速，一次进样就能得到11种菊酯残留结果；准确度和精密度高，在0．016μg／kg、0．032μg／kg和0．064μg／kg3个添加水平下的回收率在70％～110％之间，CV≤7．4％；选择性好，消除了色素和其它杂质干扰；灵敏度高，检出限低，除了氯菊酯为10μg／kg外，其它菊酯检出限都在μg/∥kg级，七氟菊酯则达到了0．02μg／kg。     

苯并[b]萘并[2'''',3'''':5,6][1,4]二噻英并[2,3-i]噻蒽-5,7,9,14,16,18-六酮的合成及其三阶非线性光学性能

以1,4-萘醌为原料,合成了含硫的醌构稠杂环化合物苯并[b]萘并[2',3':5,6][1,4]二噻英并[2,3-i]噻蒽-5,7,9,14,16,18-六酮(4),其结构经1H NMR和IR确证.采用波长为800 nm,脉宽为80 fs的Ti:Sapphire飞秒激光,运用双光束简并四波混频法测定了4的三阶非线性光学性能,结果表明,4的三阶非线性光学极化率χ(3),非线性折射率n2,分子二阶超极化率γ和响应时间分别为2.89×10-13 esu, 5.31×10-12 esu, 3.14×10-31 esu和101 fs.并分析了4的分子结构对其三阶非线性光学性能的影响.     

电热蒸发进样—等离子体原子发射光谱中钒和钛的蒸发机理研究

自1974年Nixon报道钽丝电热蒸发作为ICP-AES进样技术以来,这一技术已引起了人们的极大兴趣,受到越来越广泛的重视。电热蒸发(ETV)-ICP-AES是一种将蒸发和激发分步进行的联用技术。石墨是目前普遍使用的蒸发器材料。然而,在高温下某些元素和石墨材料可以发生碳化反应,形成热稳定的碳化物,使分析物蒸发不完全或根本不蒸发,从而影响分析结果的灵敏度和准确性。为了解决这一问题,我们曾提出了以聚四氟乙烯(PTFE)悬浮体为氟化剂,氟化辅助ETV-ICP-AES直接测定粉煤标样中钒和钛的新方法,其检出限     

Amphiphilic miktoarm star copolymers can self-assemble into micelle-like aggregates in nonselective solvents: a case study of polyoxometalate based miktoarm stars

It is well-known that amphiphilic star-shaped copolymers can self-assemble in selective solvents to form complicated micellar constructs as a synergistic result of both the topological constraints and relative volume fractions of the arms. Although the association phenomena of amphiphilic stars have been observed in nonselective solvents, both the structural detail and formation mechanism of these associates are not clear yet. Moreover, these experimental observations are controversial with respect to molecularly dispersed starlike copolymers in nonselective solvents as is popularly believed. To clarify these issues, we have synthesized a series of polyoxometalate-based polystyrene-poly(ethylene glycol)(PS-PEG) miktoarm star supramolecular copolymers(SEW-1–5) by coupling a Keggin-type polyoxometalate of K_4[α-SiW_(12)O_(40)] with 1,2,3-triazolium bridged block copolymers of-PS_n-b~+-PEG_mI~-(n=17, 26, 39, 57, 81; m=45) through ionic exchange reactions, respectively. TEM imaging,contact angle and ~1H NMR studies reveal that SEW-2–5 self-assemble in chloroform, THF, and toluene to create micellelike aggregates ranging from cylinder to sphere with a PS corona and a PEG core, while for SEW-1, reverse bilayers are captured with a PEG corona and a PS core. Among these aggregates, the Keggin clusters of [α-SiW_(12)O_(40)]~(4-) localize at the core-corona interfaces between PS and PEG. In terms of solvent quality, chloroform, THF, and toluene are only slightly poorer for PEG than that for PS with a relative order of chloroformTHFtoluene. These unexpected aggregates originate from the topological constraints of the chemically different arms of PS and PEG in the miktoarm stars, where the weak incompatibility between the PS and PEG arms is intensified appropriately. The presence of the reverse bilayered structures of SEW-1 is due to the magnified steric hindrance of the PEG45 arm with decreasing the molecular weight of the PS17 arm. However, to the best of our knowledge,these are the first examples clearly indicating that miktoarm star copolymers can self-assemble in common good solvents or slightly selective solvents to generate micellelike aggregates. This scenario is not only in sharp contrast to the intuitively considered behavior of unimolecular miktoarm stars in nonselective solvents, but also rather different from the conventional selfassembly behavior of amphiphilic star copolymers in selective solvents.     

Structural Characterization of Anhydroicaritin Glycosides Using ESI—FT—ICR Mass Spectrometry

Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR-MS) was used to determine the structures of anhydroicaritin glycosides by the MS/MS experiments of anhydroicaritin glycosides and their methylated derivatives,With high accuracy FT-ICR-MS provides much information about the structures of compounds ,FT-ICR-MS shows the great potential application in the structural characterization of unknown compounds.