GC-FPD测定粗苯中二硫化碳及噻吩含量

建立了气相色谱法测定粗苯中二硫化碳及噻吩含量的分析方法。将粗苯以甲醇为溶剂稀释,采用GC-9A岛津气相色谱分离,FPD检测器检测,指数法分别对粗苯中的二硫化碳、噻吩进行定性定量分析。该方法分离效果好,测定的结果具有良好的准确度和精密度,整个试样分析时间不超过6 min。     

脱苯塔采萘及脱苯工艺改进的探讨

系统分析了采用传统汽提工艺的脱苯塔不能从侧线采出合格萘油的症结所在.通过对脱苯塔的操作工况、富油加热的热源选择、洗油再生的方式等工艺和设备问题的深入剖析,针对性地提出了脱苯塔减压操作、富油采用导热油间接加热、洗油采用热贫油加热并贫油再生的一系列优化工艺和设备的具体措施,从而实现了萘油的顺利采出,并在保证采萘的前提下,进...     

Structural effects on the interactions of benzene and naphthalene sulfonates with activated carbon cloth during adsorption from aqueous solutions

Interactions of benzene and naphthalene sulfonates with activated carbon cloth (ACC) during adsorption from aqueous solutions were investigated. Systematically chosen sulfonates were sodium salt of benzene sulfonic acid (NaBS), disodium salt of 1,3-benzene disulfonic acid (Na₂BDS), sodium salt of 1-naphthalene sulfonic acid (NaNS), disodium salt of 1,5-naphthalene disulfonic acid (Na₂NDS) and trisodium salt of 1,3,(6 or 7)-naphthalene trisulfonic acid (Na₃NTS). The adsorption behaviors of these adsorbates from solutions in water and in 0.01 M H₂SO₄ onto the ACC were monitored by in-situ UV–visible spectroscopic technique. The order of rates and extents of adsorption of sulfonates were explained in terms of acidity of the medium and structural factors influencing the interactions between sulfonates and the ACC surface. Kinetic data of adsorption were treated according to pseudo first-order, pseudo second-order, Elovich and intra-particle diffusion models. The best model representing the experimental kinetic data was found to be the pseudo second-order model. Adsorption isotherms of the sulfonates onto the ACC were derived at 30 °C. Isotherm data were found to fit the Freundlich model better than the Langmuir model.     

NNOWAX色谱柱分析粗苯中萘含量方法研究及应用

通过配置标准溶液,调节色谱的进样口温度和柱箱升温速率制定合适的分析粗苯中萘含量方法,使分析粗苯中萘含量的数据更加准确。     

噻吩酰胺衍生物的合成

以丁醛为原料经2步合成中间体2-氨基-5-乙基-3-噻吩甲酸(3),中间体3与2-吡啶甲酸反应合成中间体2-(2-吡啶基)-6-乙基-4H-3,1噻吩并噁嗪-4-酮(4),中间体4与取代的胺反应得到了一系列噻吩酰胺的衍生物(5a～5g),其结构得到了1H NMR、13C NMR、IR、和MS表征。     

噻吩及其衍生物

噻吩类杂环化合物应用较多的是其衍生物,该类化合物发展在我国处在起步阶段,大多数产品尚属空白,还没有产量规模化、品种系列化的生产厂家。α-噻吩衍生物广泛应用于合成医药、农药、染料、化学试剂和高分子助剂等,重要的衍生物有噻吩-α-乙酸、α-氯甲基噻吩、α-乙酰噻吩和噻吩-α-甲醛,噻吩-α-乙酸是目前用量最大的噻吩衍生物,全球用量在1000t/a左右。β-噻吩衍生物有特殊的活性,主要用于合成医药和农药。大多数β-噻吩衍生物是以β-甲基噻吩为原料合成的,重要的衍生物有β-甲基噻吩、β-噻吩甲醛、噻吩-β-乙酸乙酯和β-溴噻吩等,β-噻吩衍生物是高附加值产品,例如β-噻吩甲醛的售价为86万元/t,2-(邻硝基苯胺基)-5-甲基-β-氰基噻吩的售价为1.2万元/kg。     

Synthesis and Characterization of Polyacetylene with Side-chain Thiophene Functionality

A new polyacetylene derivative with electroactive thiophene substituent, namely poly(2-methylbut-2-enyl thiophene-3-carboxylate) was synthesized and characterized. For this purpose, novel acetylene monomer was synthesized by the reaction of 3-thiophenecarboxylic acid with propargyl bromide and polymerized with a Rh catalyst to give the corresponding polymer. The chemical structure of the polymer was characterized to comprise the conjugated backbone and electroactive thiophene side group. UV spectral changes of the polymer with temperature were also studied. The polymer exhibited better thermal stability than the unsubstituted polyacetylenes.     

Formation and growth of dispersed carbon particles during pyrolysis of ethylene,benzene, and naphthalene in a reflected shock wave

The formation and growth rates of dispersed carbon particles were determined experimentally for pyrolysis of ethylene, benzene, and naphthalene in a reflected shock wave at temperatures of 1920–2560 K and hydrocarbon concentrations in argon of 1.8–20%. The diameter of the particles formed was estimated (30–600 Å). The maximum rate of particle formation at various temperatures [(0.7–96) · 10¹⁶ cm⁻³·sec⁻¹] and the particle growth rate (0.002–0.036 cm · sec⁻¹) were determined from results of measurements of reaction (residence) times. For pyrolysis of benzene, the activation energy of the overall process of particle formation is 410 kJ/mole, and for all hydrocarbons studied, the activation energy of the overall process of particle growth is 5–50 kJ/mole. The surface average particle diameter increases with increasing concentration of the initial hydrocarbon at a constant temperature. __________ Translated from Fizika Goreniya i Vzryva, Vol. 43, No. 4, pp. 82–89, July–August, 2007.     

噻吩及吡咯并荧蒽衍生物的合成

以苊醌作为起始原料合成化合物7,10-二苯基荧蒽并[c]噻吩和N-叔丁基7,10-二苯基荧蒽并[c]吡咯,产物通过1HNMR、13CNMR、高分辨率质谱和X-射线单晶衍射等方法进行表征。其中关键中间体7,9-二苯基-8H-环戊二烯酮通过Diels-Alder环加成形成7,10-二苯基-8,9-二(甲氧羰基)荧蒽,将其还原得到7,10-二苯基-8,9-二(羟甲基)荧蒽作为关键中间体用于进一步转化为目标化合物。噻吩化合物已通过单晶X-射线进一步完成结构测定。     

噻吩生产及市场应用

本总结了噻吩生产及应用情况．介绍了各种噻吩衍生物的制备方法及用途，对国内噻吩市场做了初步分析，并对噻吩行业的发展提出了建议。     

气相色谱法测定作业场所中的苯、甲苯、二甲苯

介绍的苯、甲苯、二甲苯热导池检测器气相色谱测定方法，具有灵敏主高、准确性好的特点。     

银离子改性Y分子筛对噻吩硫的增强吸附分离性能研究

以Y分子筛为载体,采用等容浸渍法制备了一系列负载银的燃油深度脱硫复合吸附材料。研究了Ag/Y吸附剂的制备条件及其对噻吩类硫化物吸附性能的影响;并对吸附剂进行了比表面积、X射线光电子能谱和X射线衍射分析。结果表明:浸渍液的浓度为0.1 mol/L,浸渍时间为6 h,并于100℃条件下干燥2 h后于550℃焙烧2 h,是制备Ag/Y复合吸附剂的适宜条件。     

2-乙酰噻吩的合成及应用

对2-乙酰噻吩的合成和应用进行了综述,对今后的发展提出了建议。     

Microstructures and interfaces in directionally solidified oxide–oxide eutectics

This article reviews different studies carried out on the microstructures and oxide–oxide interfaces encountered in directionally solidified eutectics. Depending on the phase diagram and preparation conditions, lamellar, fibrous or three-dimensional network microstructures can be obtained. Interfaces between refractory oxides with various structural types (corundum, fluorite, rocksalt, perovskite and garnet) are investigated. Orientation relations and interface planes are reported and general features of the structure of interfaces are discussed from high-resolution electron microscopy (HREM) studies. The accommodation of lattice mismatch at the interface is investigated by geometric phase analysis of HREM images.     

2-氯甲基噻吩合成与表征

以气体甲醛代替甲醛溶液合成了2-氯甲基噻吩.探讨了物料摩尔比、反应温度及反应时间对收率的影响.在反应温度为-5℃、反应时间为2.5 h、n(噻吩):,n(氯化氢):,n(甲醛)为1:1.4:1.3的最佳合成条件下,2-氯甲基噻吩收率为65.1%.与传统的甲醛溶液法相比,气体甲醛法具有较好的经济效益和环境效益.并用元素分析法及气-质谱联用法对产物进行了表征.     

Chemical and Electrochemical Polymerization of Thiophene Derivatives

Abstract

The synthesis and some physical properties of polymers containing the thiophene ring are described. The polymerization of 3-phenylthiophene (1), 2-phenvi-thiophene (2). 2,5-diphenylthiophene (3), 2-(2-thienyl) pyridine (4) and 3,6-bis(2-thienyl)pyridazine (5) under electrochemical and chemical conditions are reported. The monomers were prepared by the nickel or palladium catalyzed cross-coupling reactions and were electrochemically polymerized using galvanostatic conditions (platinum electrodes) or chemically polymerized by oxidation with iron trichloride. The effect of monomer concentration, electrolyte and solvent were studied. From the examined polymers only poly(3-phenylthiophene) showed significant properties, considering morphology and conductivity. The other polymers gave mainly powder or porous films with low conductivity. The thermogravimetry analysis of poly (3-phenylthiophene) showed a wide temperature range of thermal stability, only over 450°C considerable weight loss was observed. Scanning electron microscopy (SEM) of samples obtained under different conditions demonstrated the dependence of the morphology upon monomer structures, nature of the dopant and synthetic route employed.     

Extraction of Thiophene with Methyl Ether of Polyethylene Glycol 350

Theoretical Foundations of Chemical Engineering - The efficiency of polyethylene glycol methyl ether 350 (PEG ME-350) in the process of extracting thiophene from model motor fuel has been studied...     

Carbonization of naphthalene and dimethylnaphthalene

A variety of analytical techniques has been utilized to determine the chemical changes which take place during the thermal conversion of the aromatic hydrocarbons naphthalene (N) and dimethylnaphthalene (DMN), to pitch, mesophase, and coke. Aromatic polymerization was shown to play a dominant role at each stage of the coking process. Secondary reactions involving hydrogen transfer and molecular rearrangement were also apparent. Polymerization of (N) occurs largely through the loss of hydrogen while the polymerization of (DMN) involves the elimination of methyl groups. The faster rate of coking for (DMN) compared to (N) is attributed to the activating effect and facile bond cleavage of the methyl group.