苯与溴反应的实验装置改进

1问题的提出现行高二化学课本(人教版)中苯与溴反应的演示实验笔者发现存在以下问题:(1)实验时由于溴易挥发,有剧毒,造成严重的环境污染,影响了师生健康。(2)反应不易控制。由于反应物和催化剂一次加入,反应比较剧烈,不易控制反应速率。(3)产品不易检验。生成的气体中混有一定量的溴蒸气,造成对HBr检验的干扰。鉴于此,笔者从师生身体健康和教学效果出发,对本实验装置进行了改进。2实验用品2mL液溴,4mL苯,CCl4液体,AgNO3溶液,10%NaOH溶液,提拉式铁丝网,脱脂棉,20×200mm、18×180mm具支试管各1支,U型管,试管,橡皮塞等。3实验装置1苯和…     

苯跟溴取代反应实验的改进

按照现行高中化学课本第二册(人教版)介绍的方法去做演示实验时,常存在如下问题:(1)实验仪器容积大,药品用量多,反应剧烈难以控制;(2)装置不密闭,不能避免苯、澳和嗅化氢蒸气对空气的污染;(3)锥形瓶上玻璃导管易下垂而插入蒸馏水中,有碍实验正常进行。现将我的改进方法介绍如下。     

利用注射器巧做苯的溴代反应实验

苯的溴代反应是苯的重要化学性质之一。笔者利用一次性注射器,设计出了全封闭式的“苯的溴代反应”实验装置。     

苯与溴取代反应的实验改进

人教版《化学2》中苯的溴代反应实验[1],人们已做了不少探究改进,但仍然存在一些不足[2~8]:(1)用磁铁吸引铁粉的改进方法不仅操作不方便,而且难以保证把铁屑全部吸住,稍有不慎操作就会失败;(2)装置中用直玻璃导管不利于苯和Br2蒸气的充分冷凝回流;(3)向反应后的混合物中直接注入NaOH溶液,除去未反应的Br2来观察溴苯的真实     

溴苯制取实验的绿色化设计

液溴与苯在铁粉催化下的反应非常剧烈,反应容器的温度很高,常规条件下即使使用洗气瓶也仍然有大量溴蒸气以及苯蒸气溢出;另外,由于苯和液溴都易挥发,而试剂的取用以及产物的分离操作都是在敞口条件下进行的,也会不可避免地造成苯与溴的挥发泄漏,污染十分严重。因此,中学化学教师基本上都不做该演示实验了。笔者对此实验重新进行了绿色化设计,利用一次性注射器、输液器、粉针瓶和普通小药瓶做实验仪器,实现了实验过程的全封闭操作,解决了污染问题,收到了很好的效果。     

间二氟苯溴化反应产物的气相色谱-质谱分析

采用气相色谱-质谱(GC/MS)法对间二氟苯溴化反应产物的组成与结构进行了分析,并对间二氟苯溴化反应的选择性及反应条件进行了初步探讨。结果表明:间二氟苯的溴化反应具有较强的选择性,其主要反应产物为1-溴-2,4-二氟苯,副产物为1-溴-2,6-二氟苯、1-溴-3,5二氟苯及二溴代间二氟苯等溴化物。该反应的反应条件对产物组成有较大影响。     

苯不能使溴水和溴的四氯化碳溶液褪色吗

正苯不跟Br2水、Br2的CCl4溶液起反应,苯不能使Br2水、Br2的CCl4溶液褪色的结论,笔者长期信以为真。事实究竟怎样呢?1苯不跟溴水反应(不能使溴水褪色)的由来就笔者50多年执教中学化学的阅历和回忆,苯不能跟溴水起反应(苯不能使溴水褪色),这早已是学界的定论。下面按文献出版的先后年序,并     

测定乙醇分子结构演示实验的研究

关于测定乙醇分子结构的实验,笔者按全日制普通高级中学教科书《化学》[1]所述实验装置和步骤进行实验,总未能得到预期的结果,经过反复实验观察,发现该实验装置存在以下问题:(1)由于分液漏斗上没有“mL”值刻度标尺,因而从分液(滴液)漏斗往烧瓶中滴入无水乙醇时,无法直接准确测量滴入无水乙醇的体积;并且,在滴入无水乙醇时,常因乙醇跟钠激烈反应,瞬间产生大量氢气,压强突然猛增,大量氢气和乙醇气体从玻璃旋塞液流孔经乙醇层外逸,致使实验失败。(2)氢气的体积由测量乙醇跟钠反应产生的氢气从广口瓶里压入量筒中水的体积(包括由广口瓶到量筒…     

甲酸氧化反应动力学反应装置的改进

进行甲酸氧化反应动力学实验时,需要在反应前用去离子水清洗反应装置内壁。由于原反应装置（图1）存在缺陷,反应装置口使用橡皮塞,反应装置底部无活塞,每次换液时,需取出橡皮塞,倒出废液,洗净后再放回,操作不方便,而且容易损坏反应装置。在实验时,要将配制好的液体（水、溴、溴试剂、盐酸）加入到反应装置内,恒温并等待Br^-生成;但由于橡皮塞孔径较大,在加入甲酸之前,易有液体从橡皮塞孔径挥发,使液体浓度发生改变,影响实验结果。     

新的二苯并环状溴鎓盐的合成及性质研究

以4,4'-二取代联苯(或4,4'-二取代二苯甲烷)为原料合成了几种新的3,7-二取代二苯并环状溴(鎓)盐.对几种溴(鎓)盐与KBH₄及与NaN₃的反应进行了研究.结果表明,前一反应主产物为2-溴-4,4'-二取代联苯(或2-溴-4,4'-二取代二苯甲烷),后一反应的主产物为2-叠氮基-2'-溴-4,4'-二取代联苯(20a-20d).通过20a-20d的热反应合成几种新的多取代咔唑(21a-21d).     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。