5(6)-苯并三氮唑羧酸酯的合成

以对氨基苯甲酸为原料，经硝化、还原、闭环、酰氯化及酯化反应合成了一系列苯并三氮唑羧酸酯类化合物。     

八甲基环四硅氮烷离子开环聚合研究

以甲苯为反应溶剂、三氯化钌为催化剂,六甲基二硅氮烷锂盐为引发剂,通过对八甲基环四硅氮烷离子开环聚合合成聚硅氮烷聚合物。利用红外射线和核磁共振表征聚合物结构。实验结果表明:160℃下,八甲基环四硅氮烷在钌基催化剂和锂盐引发剂共同作用下持续反应16h,发生完全开环聚合反应。最后在理论上阐明了不同实验条件下八甲基环四硅氮烷离子开环聚合效率不同的原因。     

水下涂料的新发展

本文根据现代造船工业对涂料要具备三年有效防污寿命,叙述了防污涂料的最新技术发展。典型的毒料包括新的杀虫化合物,如有机锡、三氮杂苯和苯脲的衍生物。同时,对海洋工程的高性能材料也有叙述,包括氯化橡胶涂料、环氧聚酰胺涂料和新近研制的“控制释放”的有机聚合物。     

氧氮玻璃连接氮化硅陶瓷的研究进展

陶瓷连接技术是结构陶瓷实用化必须解决的难题之一．氧氮玻璃与氯化硅陶瓷间良好的化学相容性,保证了连接的有效性和可靠性．本文对氧氮玻璃的性能、连接机理以及结合强度的影响因素作了简要的综述．     

氮氧化物的制备、性质和应用

介绍了一氧化二氮、一氧化氮、三氧化二氮、二氧化氮、四氧化二氮、五氧化二氮的制备方法、性质和应用等     

聚二乙氧基磷腈的合成与表征

聚二乙氧基磷腈是以磷、氮原子交替排列作为主链结构的无机高分子,具有良好的成膜性,是一类有潜在应用前景的新型膜分离材料。本文研究了由三聚六氯化环磷腈进行固相聚合制备聚氯化磷腈以及由后者制备聚二乙氧基磷腈的方法,同时对产物进行了表征。     

金属材料表面改性技术—奥氏体氮碳共渗的进展

国际热处理联盟专用木语委员会已经将氮碳共渗正式定义为化学热处理(以前称为软氯化),它可用于金属零件,以形成表面氮碳富集的化合物层,并在该层下面形成富氮扩散区。铁素体氮碳共渗是在Fe-N-C三元系共析温度之下(即低于580℃)进行的,其扩散区处于铁素体状态,旨在使金属零件表面具有良好的耐磨性、抗疲劳与抗腐蚀性能。但是,普通碳钢经处理后,化合物层下面不具备明显硬化层。奥氏体氮碳共渗是在590～720℃进行的奥氏体状态处理,此时共     

四氯化锡催化聚丙烯腈关环反应机理的研究

本文用X射线光电子能谱(xps)及红外光谱对四氯化锡催化聚丙烯腈分子内氰基关环反应的机理进行了研究,通过氰基中氮原子和四氯化锡中锡原子的结合能变化及在红外光谱中观察到N→Sn配位健的形成,认为该反应是络合催化反应。      

介绍一种DDNP氮量的测定方法

用注射器气量法测定氮量虽然使DDNP氮量测定方法前进了一步,但尚有不足之处,操作条件不易掌握。我们认为用测定Pb(N_3)_2纯度的水封式气量装置,略加改动,来测定DDNP的氮量更为优越。 (一) 原理以盐酸氯化亚铜溶液分解DDNP,重氮基被破坏,生成氯化二硝基苯酚和氮气,根据产生气体的体积,计算氮量。其反应如下:     

原子转移自由基聚合法制备氮卤胺型抗菌棉织物及性能

合成了氮卤胺前驱体2-(3-(6-甲基-4-氧-1,4-二氢嘧啶-2-基)脲基)甲基丙烯酸乙酯(SCMHBMA)，通过原子转移自由基聚合(ATRP)法接枝在棉织物表面，制备出棉织物接枝SCMHBMA聚合物(Cotton-g-PSMA)，通过氯化处理得到抗菌棉织物。探究了棉织物接枝前后的元素变化、热力学性能等，并对氯化后的棉织物进行储存稳定性、洗涤耐久性和抗菌性能测试。结果表明，氯化棉织物(Cotton-g-PSMA-Cl)经过5次洗涤和60 d常规储存后，活性氯浓度(Cl⁺%)仅分别降低22%和18%，并且降低的活性有效氯可以通过简单的再氯化作用得到有效的提高。在抗菌测试中，抗菌棉织物Cotton-g-PSMA-Cl与金黄色葡萄球菌和大肠杆菌接触1 min后，基本杀灭100%菌株。合成出的氮卤胺型抗菌棉织物表现优异的抗菌性能，在长期抗菌领域具有广阔的应用前景。     

Formation of NCl3 and N2O in the reaction of NaOCl and nitrogen compounds

This paper deals with the problems that can arise when a nitrogen-containing compound, in this case ammonium chloride, is present in a solution which is to be chlorinated. The chlorination can be performed with chlorine itself, or with a compound capable of forming active chlorine, such as sodium hypochlorite. A short literature review is given concerning this subject, and the reactions of nitrogen compounds with active chlorine are discussed. The formation of nitrogen, nitrogen trichloride and dinitrogen monoxide in these systems is explained and proven in experiments. It is shown that, especially in acidic circumstances, free nitrogen trichloride can be formed which at higher temperatures is able to evaporate from the solution. The amount of nitrogen trichloride recovered exceeds 30% of the theoretical value. The nitrogen trichloride formed detonates very easily upon rapid heating, even in quantities of one gram. Upon the chlorination of acidic ammonium ion containing solutions (pH < 8) nitrogen trichloride is formed; therefore these circumstances are to be avoided. This can be done, for example, by the addition of sufficient alkali or by intensive stirring. When the formation of nitrogen trichloride cannot be avoided stringent safety measures are necessary.     

电子工业用气体三氯化硼中微量氯的比色法测定

介绍了化学比色法测定三氯化硼中微量氯的过程及消除基体干扰的方法。     

气相色谱与电感耦合等离子体质谱联用测定海产品中有机锡的研究

本文报道用气相色谱和电感耦合等离子体质谱联用法测定海产品中的有机锡。经色谱柱分离进样,用等离子体质谱仪在线耦合测定了三氯丁基锡、二丁基锡二氯化物、氯化三丁基锡,并对影响测定的各种因素进行了研究探讨。用该联用方法测定三氯丁基锡、二丁基锡二氯化物、氯化三丁基锡,可以在14分钟内分离完全。仪器检出限分别为：0．1μg／L^-1。线性范围从1．0μg／L^-1到200μg／L^-1。本实验方法应用于海产品中三氯丁基锡、二丁基锡二氯化物、氯化三丁基锡的测定,结果较为满意。     

不同晶型纳米TiO2的溶剂热合成及其光催化活性研究

采用不同的醇溶剂,以六亚甲基四胺为沉淀剂,以TICl3为前驱体,通过溶剂热的方法控制合成出纳米级的锐钛矿型、金红石型和板钛矿型的二氧化钛.通过XRD、TEM、UV-Vis光谱和XPS能谱对其进行了表征,研究了醇的种类、六亚甲基四胺的量对二氧化钛相组成及光催化性能的影响.结果发现,以甲醇为溶剂,酸性条件有利于生成锐钛矿相,碱性条件有利于生成金红石相和板钛矿相.溶剂热条件下可以得到氮掺杂的TiO2-xNx.光催化降解甲基橙活性结果表明锐钛矿和板钛矿混晶具有最好的光催化活性.     

Preparation of High-Purity Arsenic via Hydrogen Reduction of Arsenic Trichloride

The chemical equilibria involved in the hydrogen reduction of arsenic trichloride under reaction conditions of practical interest are assessed by thermodynamic modeling. Experimental data for high-purity arsenic trichloride are used to optimize the reduction conditions. The optimal residence time of the gas mixture in the reaction zone is 30–50 s. The optimal reduction temperature is 1023 K. Condensation temperatures in the range 600–650 K make it possible to minimize the percentage of amorphous arsenic. The yield of elemental arsenic is 99.99%.     

Spill behaviour using REACTPOOL. Part III. Results for accidental releases of phosphorus trichloride (PCl(3)) and oxychloride (POCl(3)) and general discussion

Phosphorus trichloride and oxychloride are aggressive materials, widely used in the process industries. On escape to the atmosphere they create toxic clouds that may cause serious damage to people and to the environment. When spilled onto the ground they create liquid pools that can boil, evaporate or even solidify. The main feature of the pool behaviour is the exothermic reaction of these chemicals with water, which is complicated and depends heavily on the amount of water available for reaction, and as result of which the pool has changing composition and properties. The purpose of this paper is to describe the dangers involved in cases of accidental releases of phosphorus trichloride and oxychloride, to report their properties, referring to toxicity data and major accidents. The spill behaviour of phosphorus trichloride and oxychloride has been incorporated into REACTPOOL [R.F. Kapias, C. Griffiths, J. Haz. Mater.]. Model results indicate that the pool behaviour is strongly affected by the amount of water available for reaction. Surface roughness and wind speed, also have a strong effect on the results. Although there are no experimental data for model validation, it is shown that REACTPOOL gives useful insights into the behaviour of such spills. The paper concludes with a discussion comparing the behaviour for several water reactive chemicals to which REACTPOOL has been applied.     

Solvothermal synthesis of visible light responsive nitrogen-doped titania nanocrystals

Nitrogen ion-doped titania nanoparticles were obtained by the homogeneous precipitation in hexamethylenetetramine-titanium trichloride mixed solution followed by heat treatment in the solution at desired temperatures. After that the sample powders obtained were calcined in air at desired temperatures. Various phases of titania such as anatase, rutile and brookite were obtained depending on the reaction condition. Crystallite size, specific surface area and color also greatly changed as 5-50 nm, 20--200 m²·g^-1 and light gray-yellow, respectively, depending on the solvent, pH, etc. The products after calcination around 400°C were yellow indicating doping with nitrogen ion. Photocatalytic activity for the oxidative decomposition of NO in air atmosphere was also evaluated by using a continuous flow system with 1 ppm NO gas, where the high pressure mercury arcs filtered using various filters were irradiated. All colored titania nanoparticles showed photocatalytic activity under visible light irradiation for the oxidative decomposition of nitrogen monoxide in air. Especially, the nanoparticles of anatase type nitrogen-doped titania obtained by the homogeneous precipitation using hexamethylenetetramine-methanol aqueous solution around 200°C showed excellent photocatalytic activity under visible light irradiation.     

Effect of Various Additives on the Yield and Molar Radioactivity of Labeled Products in Solid-Phase Isotope Exchange

A series of tritium-labeled amino acids were prepared by high-temperature solid-phase isotope exchange in the presence of various additives, namely, of 4-dimethylaminopyridine and rhodium trichloride. These agents strongly affect the degree of isotope exchange. 4-Dimethylaminopyridine provides successful labeling of high-melting compounds; it presumably increases the probability of the reaction of active tritium species with the substrate. The positive effect of rhodium salts may be due to an increase in the thermal stability of amino acids, i.e., in the presence of rhodium trichloride the same yield can be attained at higher temperatures. Therefore, despite modification of the catalyst occurring when rhodium trichloride is reduced, the molar radioactivity of the labeled product appears to be higher than without rhodium salts. Thus, in the presence of rhodium salts, the decrease in the yield of labeled amino acids with increasing temperature is less pronounced than the increase in the molar radioactivity of these substrates, which allows preparation of highly labeled products in reasonable yields.     

Liquid-vapor equilibria in the AsCl3-HCl-H2O system

The liquid-vapor equilibria in the AsCl₃-HCl-H₂O system have been studied by a flow method at high hydrogen chloride concentrations (above 20 wt %) over the entire arsenic trichloride solubility range at temperatures from 25 to 105°C and a pressure of 1.013 MPa. The composition effects on the parameters of the liquid-vapor equilibria have been assessed, and the conditions for the most effective recovery of arsenic trichloride from hydrochloric acid solutions by distillation were established.     

Preparation of Trichloride and Tetrachloride of Molybdenum

Molybdenum trichloride was successfully prepared in quantity by the reduction of molybdenum pentachloride with hydrogen. The most satisfactory yields were obtained with a 4 to 5 mole excess of hydrogen at pressures of 100 psi or higher and at a temperature of 125°C.Molybdenum tetrachloride was prepared by direct reaction of molybdenum trichloride with molybdenum pentachloride in a sealed tube or steel bomb maintained at 250° C. X-ray patterns of the various chlorides were obtained.