常压催化加氢合成邻氨基苯酚的研究

用硅溶胶改性的漆原镍催化剂，在常压液相催化条件下，氢化邻硝基苯酚制备邻氨基苯酚的反应过程，可分为诱导期、恒速吸氢阶段、吸氢衰减期３个反应阶段．恒速吸氢阶段的吸氢速率为５×１０２ｍｏｌ／（ｋｇ·ｍｉｎ）且与体系的温度无关，诱导期随温度的增加而变短，吸氢衰减期的长短随溶剂量的变化而变化．实验结果表明，邻氨基苯酚的收率在９５％左右．     

CoNiZ系列合金的结构和马氏体相变性质

利用X射线衍射研究了CoNiZ(Z=Si,Sb,Sn,Ga等)合金在不同热处理条件下的相组成.当Z元素为Sn,Sb时,材料是完全的B2结构;但Z为Si时,材料变成面心立方的γ相.形成B2还是γ相由电子浓度和原子尺寸效应两种因素共同决定.而CoNiGa的研究结果表明,在合金中除了形成B2结构的同时还容易形成γ相,常表现出两相共存的特性.对材料进行不同方式的热处理可以使合金中两相的含量有所消长,γ相含量的多少对CoNiGa合金的马氏体相变有很大的影响.分析指出,两相共存及其所带来的物性变化是CoNiGa铁磁性形状记忆合金非常有利用价值的物理性质.     

用于双光子激发荧光寿命显微成像的高重复频率皮秒扫描相机

建立了一台基于新研制的高重复频率皮秒扫描相机的双光子激发荧光寿命显微成像系统,重点介绍所研制的高重复频率皮秒扫描相机。为了在高时间分辨力的同时扩大时间测量范围,实现大面积两维空间高时间分辨取样测量,从而提高采样速率和更有效地发挥扫描相机的作用,设计和研制了一种大面积、高时间分辨力扫描变像管和一种重复频率高达1MHz的斜坡电压扫描电路。基于上述关键部件所研制的扫描相机具有重复频率高、扫描速度可调、时间分辨力高、工作面积大、非线性低、触发晃动小等优点。用钛宝石飞秒激光器作为激光脉冲源,通过脉冲提取器将76MHz的高重复频率降低为1MHz,采用可调延时器和标准具对扫描相机的时间分辨力、扫描速度和非线性进行标定。该系统的时间分辨力达到6.5ps,非线性为2.60%,可测量的时间范围从十几皮秒到几十纳秒。测量了若丹明6G和香豆素314两种标准荧光染料的荧光寿命,取得了与参考文献一致的实验结果。     

A copper‐based reverse atom‐transfer radical polymerization process for the living radical polymerization of polyacrylonitrile

The reverse atom‐transfer radical polymerization (RATRP) technique using CuCl₂/2,2′‐bipyridine (bipy) complex as a catalyst was applied to the living radical polymerization of acrylonitrile (AN). A hexasubstituted ethane thermal iniferter, diethyl 2,3‐dicyano‐2,3‐diphenylsuccinate (DCDPS), was firstly used as the initiator in this copper‐based RATRP initiation system. A CuCl₂ to bipy ratio of 0.5 not only gives the best control of molecular weight and its distribution, but also provides rather rapid reaction rate. The rate of polymerization increases with increasing the polymerization temperature, and the apparent activation energy was calculated to be 57.4 kJ mol^?1. Because the polymers obtained were end‐functionalized by chlorine atoms, they were used as macroinitiators to proceed the chain extension polymerization in the presence of CuCl/bipy catalyst system via a conventional ATRP process. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 226–231, 2006     

Synthesis of polyacrylonitrile via reverse atom transfer radical polymerization catalyzed by FeCl3/isophthalic acid

FeCl₃ coordinated by isophthalic acid was first used as a catalyst in the azobisisobutyronitrile‐initiated reverse atom transfer radical polymerization of acrylonitrile. N,N‐Dimethylformamide was used as a solvent to improve the solubility of the ligand. An FeCl₃‐to‐isophthalic acid ratio of 0.5 not only gave the best control of the molecular weight and its distribution but also provided rather a rapid reaction rate. The effects of different solvents on the polymerization of acrylonitrile were also investigated. The rate of the polymerization in N,N‐dimethylformamide was faster than that in propylene carbonate and toluene. The molecular weight of polyacrylonitrile agreed reasonably well with the theoretical molecular weight in N,N‐dimethylformamide. The rate of polymerization increased with increasing polymerization temperature, and the apparent activation energy was calculated to be 59.9 kJ mol^?1. Reverse atom transfer radical polymerization was first used to successfully synthesize acrylonitrile polymers with a molecular weight higher than 80,000 and a narrow polydispersity as low as 1.22. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 44: 219–225, 2006     

低密度聚乙烯光引发交联机理——Ⅱ.BNB自旋捕捉ESR研究

在光引发剂二苯甲酮(BP)存在下,紫外光辐照低密度聚乙烯(LDPE)所形成的自由基中间体已被自旋捕捉剂2,4,6-三特丁基亚硝基苯(BNB)所捕捉,其自旋加合物自由基已为电子自旋共振(ESR)所特征。现已检测和鉴定到二种自旋加合物:一种是叔碳自由基;另一种是仲碳自由基。它们分别是由BP的激发三重态从LDPE链的支化点和亚甲基团上夺氢所形成的自由基中间体同自旋捕捉剂BNB反应生成的。上述的证据表明:LDPE的光引发交联点主要发生在叔碳和仲碳原子上,且H-型交联点占主导地位。     

液相色谱法测定地质样品中的芳香化合物

发展了用液相色谱法检测地质样品中芳香化合物的方法。对观察到的色谱峰进行了定性分析，了该法对油气地球化学勘探的意义。     

结构参数X的计算方法及与分子总键能和生成焓的关系

本文借助于电负性I和有效主量子数n_i^*定义了有效价电子数Z_i′。由Z_i′、 n^*_i及成键电子数mi定义的原子结构参数δ_i和分子结构参数X被计算。发现A_mB_n型分子的X相似文献   

正交试验法优化CS汽化吸附条件

通过正交试验设计,优化了影响西埃斯(CS)标准样品管制备的参数:汽化温度、采样流速、采样时间。结果表明,CS标准样品管的最佳吸附条件为汽化吸附温度:260℃,采样N2流速:330mL/min,采样时间:15min。在15~1500ng范围内,色谱峰面积与进样量有良好的线性关系,线性相关系数为0.9995,检出限为6.0ng。     

壳聚糖衍生物的制备及其吸附性能

壳聚糖衍生物的制备及其吸附性能曲荣君，马千里，郑秀丽，孙言志（烟台师范学院化学系烟台２６４０２５）关键词壳聚精衍生物，制备，吸附壳聚糖（ＣＴＳ）是重金瞩离子的吸附剂￣［１，２］，由于壳聚精分子中的－ＮＨ＿２在ｐＨ较低的水溶液易形成而使ＣＴＳ溶于水，造...