自粘结低硅铝X型沸石的结构、吸附和N2/O2分离比

用原位合成方法直接将高岭土转化为所需形状的低硅Ｘ型沸石（ＰＬＳＸ）,经Ｘ衍射,＾２９Ｓｉ＾２７ＡｌＭＡＳＮＭＲ谱证实ＰＬＳＸ的结构硅铝比接近１,它含ＬＳＸ的组成为４０．４０％,含４Ａ的组成为１７．９２％,其余为无定形硅、铝氧化物、ＬＳＸ的骨架硅铝比接近１,是骨架负电荷分离最是均匀的Ｘ型沸石,２９３Ｋ时静态法测定和推算ＬＳＸ的饱和吸附水达３９．８０ｗｔ％,ＬＳＸ的组成为Ｎａ９６－ｘＫｘ（Ａｌ９６Ｓｉ     

洗涤剂用沸石的钙离子交换性能的研究

作为洗涤剂助剂,沸石的主要作用是通过离子交换降低水中的钙镁离子浓度、软化洗涤用水以提高洗涤剂中的表面活性剂的洗涤效率。因此,沸石对钙镁离子交换容量的大小和交换速率的快慢是评价洗涤用沸石的重要质量指标［１,２］。目前,使用最多的沸石类助剂为ＮａＡ沸石。为了弥补ＮａＡ型沸石镁离子交换能力的不足,先后又出现了Ａ、Ｘ型沸石混合使用［３］、高铝Ｘ型沸石(ＭＡＸ)［４～５］和高铝Ｐ型沸石(ＭＡＰ)等技术［１,２］。ＭＡＸ型和ＭＡＰ型沸石与ＮａＡ型沸石一样具有最小的硅铝比(ＳｉＯ２／Ａｌ２Ｏ３＝２)。因此,这三种沸石的…     

阴离子X~-(F~-、Cl~-、Br~-)对中孔分子筛MCM-41合成与性质的影响

在凝胶体系ＮａＸ（Ｆ、Ｃｌ、Ｂｒ）Ｎａ２ＯＡｌ２Ｏ３ＳｉＯ２ＣＴＡＢ（十六烷基三甲基溴化铵）Ｈ２Ｏ中，研究了水热合成中孔ＭＣＭ４１的合成条件。实验证明，在３９８Ｋ下晶化８～１６ｄ，ＮａＸ／ＳｉＯ２介于０．０１～０．０５时，均可合成出ＭＣＭ４１分子筛；ＮａＦ的加入，可以加快ＭＣＭ４１分子筛的晶化速度；ＮａＢｒ的加入，对形成ＭＣＭ４１分子筛有阻碍作用。采用ＸＲＤ、ＳＥＭ、ＴＧＤＴＡ和Ｎ２吸附对合成样品加以表征，证明合成样品具有介孔分子筛特性。     

新型洗涤剂用沸石MAP的合成及其性能表征

在ＳｉＯ_２－Ａｌ_２Ｏ_３－Ｎａ_２Ｏ－Ｈ_２Ｏ体系中,采用加入晶种的方法水热合成出新型洗涤剂用沸石－ＭＡＰ。其硅铝比（Ｓｉ／Ａｌ）在 １．０７－１．１３之间,平均晶粒直径小于０．４μｍ,钙离子交换容量为２９０～３１３ ｍｇＣａＣＯ_３／ｇ（干沸石）,非离子表面活性剂的吸附量在 ８３～ １００ｇ ｏｉｌ／１００ｇ（沸石）之间。本文着重考察了影响合成 ＭＡＰ沸石的因素,确定了ＭＡＰ沸石会成的最佳范围,并对其物理化学性质进行了表征。     

氟氯有机化合物对HZSM-5分子筛改性过程中氟和氯的作用

利用ＸＲＤ，ＭＡＳ，ＮＭＲ，ＩＲ和ＸＰＳ等手段研究了ＣＦ４－ｎＣｌｎ改性的ＨＺＳＭ－５分子筛的体相和表面结构的变化。结果表明，改性过程中Ｆ和Ｃｌ均能使ＨＺＳＭ－５脱铝和脱硅。Ｃｌ可以使沸石骨架ＳｉＯ２／Ａｌ２Ｏ３升高，而Ｆ除使沸石骨架脱铝外，还会极化其晶格。Ｆ比Ｃｌ更容易在沸石表面富集。Ｆ和Ｃｌ是通过取代Ｏ或ＯＨ与沸石表面Ｓｉ或Ａｌ作用的。改性后的沸石表面有数种含氟表面物种存在。     

杂原子B—ZSM—35沸石的干法合成,表征及CO＋H2反应性能的研究

首次利用吸附态模板剂在Ｎａ２Ｏ－ＳｉＯ２－Ｂ２Ｏ３－ＤＥＡ干粉体系中合成了杂原子Ｂ－ＳＺＭ－３５沸石，ＸＲＤ，ＳＥＭ，ＩＲ，及ＣＯ加氢反应研究了其物理化学特性。结果表明，Ｂ原子同晶取代Ａｌ原子进入ＺＳＭ－３５沸石骨加。     

彩玻管十二种元素的XRF分析

本文应用ＸＲＦ测试彩色玻璃显象管成分中１２种元素：Ｓｉ、Ａｌ、Ｎａ、Ｋ、Ｂａ、Ｔｉ、Ｆｅ、Ｐｂ、Ｍｎ、Ｓｂ、Ｃｏ、Ｎｉ。对各元素进行了基体校正，消除了共存元素的影响因素，所得测试值与化学值比较，得到满意结果。     

模板剂对ZSM—35沸石合成及其物化性能的影响

本文分析了乙二胺和正丁胺为模板剂，在水热体系Ｎａ２Ｏ－ＳｉＯ２－Ａｌ２Ｏ３－Ｈ２Ｏ中合成了ＺＳＭ－３５沸石，并利用ＸＲＤ，ＳＥＭ，ＩＲ及ＣＯ加氢反应手段考察了其物理化学特性。结果表明，模板剂对ＺＳＭ－３５沸石的合成，结构，形貌，红外振动，稳定性及催化性能有显著的影响作用。     

电感耦合等离子体光谱和质谱法分析贻贝标准物质

采用电感耦合等离子体光谱和质谱法分析了贻贝标准物质,光谱法测定Ｋ、Ｎａ、Ｃａ、Ｍｇ、Ｐ、Ａｌ、Ｆｅ、Ｚｎ、Ｍｎ和Ｓｒ,质谱法测定Ａｓ、Ｂ、Ｃｄ、Ｃｏ、Ｃｒ、ＣｕＧａ、Ｇｅ、Ｍｎ、Ｍｏ、Ｎｉ、Ｐｂ、Ｓｅ、Ｓｒ、Ｕ和Ｖ。在优化的工作条件下,测定了来自基体元素Ｋ、Ｎａ、Ｃａ、Ｐ、Ｃｌ的Ｃ的多原子离子＾３９Ｋ＾１６Ｏ、＾３９Ｋ２、＾４０Ａｒ＾２３Ｎａ、＾４３Ｃａ＾１６Ｏ、＾４２Ｃａ＾１６Ｏ、＾３１Ｐ＾１６     

Study on Infrared Spectra and Chemical Bonding of the Cluster Anion ［Cl_2FeS_2MoS_2Cu（PPh_3）_2］~－

ＳｔｕｄｙｏｎＩｎｆｒａｒｅｄＳｐｅｃｔｒａａｎｄＣｈｅｍｉｃａｌＢｏｎｄｉｎｇｏｆｔｈｅＣｌｕｓｔｅｒＡｎｉｏｎ［Ｃｌ_２ＦｅＳ_２ＭｏＳ_２Ｃｕ（ＰＰｈ_３）_２］~－ＫｏｎｇＸｉａｎ－Ｌｉｎｇ；ＣｈｅｎＺｈｉ－Ｄａ；ＳｈｅｎｇＴｉａｎ－Ｌｕ；ＷｕＸｉ...     

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。     

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。     

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.     

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。