胜利和孤岛减压渣油中的硫醚硫和噻吩硫的测定

用ＫＩＯ３电位滴定法测定了胜利和孤岛减压渣油及其色谱分离组分中的硫醚硫，用管式炉定硫法测总硫量，差减得到噻吩类硫的含量。对胜利和孤岛渣油及其亚组分的测定结果表明，胜利减压渣油中的硫约有３６．６％为硫醚硫，６３．４％为噻吩硫；孤岛减压渣油的相应值分别为４０．１％和５９．９％；胜利减渣的芳香分中硫醚硫含量高于其胶质中的硫醚硫含量，且相差较大；而孤岛减渣的这两个组分中的硫醚硫含量相近。硫醚硫在这两个渣油     

煤中形态硫分析及脱除能力研究

在实验室自动定硫仪上采用形态硫直接测定法，测定了７种煤样的脂肪硫、黄铁矿硫与噻吩硫的含量及它们脱除难易程度（能力），结果表明采用本实验方法测得的形态硫结果与Ｘ－射线吸收精细结构能谱（ＸＡＦＳ）所分析的结果一致。煤中形态硫在加热条件下脱除能力为：脂肪硫＞黄铁矿硫＞噻吩硫＞硫酸盐硫，而在弱碱性氧化脱硫条件下各形态硫脱除能力为：黄铁矿硫＞脂肪硫＞噻吩硫＞硫酸盐硫。     

焦炭中硫的空间分布规律研究

采用炼焦混合煤模拟工业焦化过程，研究了焦炭中硫的空间分布规律。结果表明，焦炭柱同一高度的有机硫、无机硫的质量分数从中心到边缘逐渐升高；相同取样位置处裂纹表面的有机硫、无机硫比对应内部位置硫的质量分数高；对于炭化室直径为230mm的模拟实验，有机硫增加约0.035%，无机硫增加约0.08%。XPS分析显示，有机硫与无机硫的质量分数的差异是由噻吩硫及金属硫化物的质量分数不同造成的。二维相似模拟实验进一步证实焦炭柱中硫的质量分数从中心沿径向到边缘逐渐升高。     

红外碳硫测定仪测定铁矿石中硫

采用红外碳硫仪对铁矿石中硫进行测定，通过对助熔剂各类、助熔剂的加入量，助熔剂的比例，称样量、试样加入顺序等条件进行试验，选择了测定铁矿石中硫的最佳条件，此法的测定范围为0．01％－4．0％。     

醌—硫硫聚合物的合成及电化学性能的研究

聚有机二硫化物的电化学性质，受到与它共聚的有机基团的影响。为此，我们以对苯二甲醚为原料经氯甲基化，硝酸氧化，与二硫化钠缩合制得了醌－硫硫共聚物，并用循环伏安法研究了该种共聚物的电化学性质，讨论了有机基团对Ｓ－Ｓ－键电化学性质的影响，并组装成电池研究它的放电行为。     

ICP-AES法测定碳酸盐岩中的总硫及其硫的形态

建立了碳酸盐岩样品中总硫及其硫的形态的分析方法,采用分级萃取技术提取样品中的单质硫、硫酸盐硫和硫铁矿硫,选择波长182.0nm,用ICPAES测定不同形态的硫和总硫,用差减法得到有机硫。用此方法测试了国家一级标准和10个广元地区的碳酸盐岩样品,结果表明,碳酸盐岩中总硫的浓度较大,在0.05%~2.00%之间,碳酸盐岩中硫主要以硫酸盐硫和硫铁矿硫两种形式存在,占总硫含量的90%以上,单质硫的含量较低,低于总硫含量的1%,有机硫的含量受总硫和几种无机硫的影响误差较大。样品中各形态硫的加和值与总硫测定值和总硫参考值相符,每个样品的硫测定3次,其相对标准偏差(RSD)为0.15%~3.7%。     

煤在不同O2/CO2气氛下燃烧硫析出特性研究

研究了煤在不同氧体积分数、混有CO2气氛下燃烧硫析出特性，结果表明，煤在低氧、混有CO2气氛下燃烧，SO2和H2S析出速率曲线均呈现双峰结构，H2S析出率明显增大，硫析出时间延长；在高氧气氛下，SO2和H2S析出速率曲线均呈现单峰结构，硫析出时间缩短。煤在低氧体积分数、混有CO2气氛下燃烧能够改善煤灰自固硫能力，降低硫的最终析出率；煤在高氧体积分数、混有少量CO2气氛下燃烧与空气气氛下燃烧相比，硫的最终析出率无明显变化。     

硒氢化钠作用下硫代碳酸甲酯的脱保护反应

由硫代碳酸甲酯与硒氢化钠反应，合成了相应的硫酚或硫醇，产率〉９０％，为巯基的脱保护提供了一种有效的方法。     

稀土元素与金属硫蛋白作用的研究

稀土元素与金属硫蛋白作用的研究黄仲贤，郑起，高红英，顾伟强，刘芳（复旦大学化学系，上海，２００４３３）关键词稀土元素，金属硫蛋白，运铁蛋白金属硫蛋白（Ｍｅｔａｌｌｏｔｈｉｏｎｅｉｎ，ＭＴ）是广泛存在于动、植物体内的一类重要的重金属结合蛋白，它能结合Ｃ...     

用电化学方法氧化硫制备硫酸

粒状硫在阳极室内被电化学氧化得到硫酸。实验发现由疏转化为硫酸的量随电流密度的增加而增加，随硫床层厚度的降低而增加。用一定粒径的硫颗粒，生成的疏酸量最大。在电流密度为８４ｍＡ／ｃｍ￣２、粒径为７１０μｍ、硫床层厚度为１．１５ｍｍ时可得到硫酸的最大浓度为３５％，由硫转化为硫酸的能量消耗范围为０．５５～２．１ｋＷｈ／ｋｇ，具体数值与电流密度有关。     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.