A2BA2型两亲性液晶嵌段共聚物的合成与表征

利用原子转移自由基聚合(ATRP)技术合成A2BA2型两亲性液晶嵌段共聚物.聚乙二醇与2,2-二氯乙酰氯反应生成结构对称的多官能团大分子引发剂,引发偶氮苯单体6-[4-(4-乙氧基苯基偶氮)酚氧基]己基甲基丙烯酸酯(AZO6Et)的ATRP反应.利用凝胶色谱(GPC)与核磁共振氢谱(1H NMR)表征了产物的分子量与结构组成,利用示差扫描量热法(DSC)与偏光显微镜(POM)对聚合物的液晶性进行了表征.该液晶嵌段共聚物在光信息储存、光开关与分子器件等领域具有潜在应用.     

具有液晶相的四烷氧基苯并菲-1,4-二醌的合成

研究合成了 6,7,10,11-四戊氧基苯并菲-1,4-二醌和 6,7,10,11-四庚氧基苯并菲-1,4- 二醌两个新化合物,经核磁氢谱和碳谱、质谱、IR 及元素分析等测定,对其结构进行了表征。该类化合物在紫外可见光区 250～630 nm 的范围有光吸收。采用偏光显微镜和示差扫描量热仪对其性能进行了研究,结果表明,该材料具有液晶性。此外,本文对该类化合物的合成方法也进行了改进,利用亚硝酸钠/三氟乙酸/二氯甲烷体系替代了常用的硝酸铈铵/四氢呋喃/水体系,反应时间可从原来的 2 h 缩短至 15 min,并在室温下完成;在合成中间体 1,2-二甲氧基-6,7,10,11-四烷氧基苯并菲时,采用二氯甲烷作为溶剂,将三氯化铁与 3,3＇,4,4＇-四烷氧基联苯的摩尔比从 8∶ 1 提高到 10∶1,反应时间可从原来的 5 h 缩短至 2 h。     

Salamo型三核钴(Ⅱ)配合物的合成、晶体结构及荧光性质研究

合成了一个新的Salamo型双肟配体2,2~′-[乙二氧双(氮次甲基)]二萘酚(H_2L)及其三核钴(Ⅱ)配合物[Co_3(L)_2Cl_2],通过元素分析、红外光谱、紫外-可见吸收光谱、荧光光谱和X-射线单晶衍射法等对配合物进行了表征.结果表明:在钴(Ⅱ)配合物中,Co1形成了五配位的扭曲四方锥构型;Co2形成了六配位的八面体几何构型.该配合物通过分子间的氢键作用形成了二维和三维的超分子结构.Hirshfeld表面分析证明了分子内短程作用对配合物稳定性的贡献.钴(Ⅱ)原子配位后,配合物的荧光强度有所减弱.实验数据有助于进一步开展Salamo型配合物的光学性质的研究.     

加合物C29H25N5O6S的合成及晶体结构研究

介绍了有机加合物N-(2-硝基苯基)-2-苯乙酰胺并N-乙氧羰基-N’-o-硝基苯乙酰基硫脲的合成及结构研究,其分子式为C29H25N5O6S,分子量为571.60.采用溶剂挥发培养出了0.30mm×0.26mm×0.24mm尺寸的加合物单晶,该加合物通过FT-IR、1 HNMR和X-射线单晶衍射分析方法进行了表征.该化合物属于单斜晶系,P21/c空间群,晶胞参数:a=12.796 5(11),b=13.502(3),c=11.261(3),α=90°,β=102.329°(3),γ=90°,Z=4,V=2 726.6(10)3,D=1.329mg/m3,F(000)=1 192,GOF=1.035.结构由直接法解出,最终偏离因子为R1=0.080 6,wR2=0.135 6.X-射线单晶衍射分析显示,晶体中分子主要通过分子间N-H…O氢键(N1-H1A…O4键长为3.005,键角为170.23°)和C-S键(C23-S1键长为3.847)相互连接,在晶体中形成了一维链状结构.对该加合物的合成及其分子的微观晶体结构进行了研究.     

纯六方相钛酸锌粉体制备和表征

采用溶胶-凝胶法,用Ti(OC4H9)4、Zn(NO3)2·6H2O、无水乙醇、冰醋酸等原料,利用直接升温和保温-升温两种方法合成超细的六方相ZnTiO3粉体.利用TG-DSC、XRD、SEM等测试分析手段对凝胶的热分解、相转变以及粉体结构形貌进行了表征.实验结果表明:ZnTiO3凝胶的热分析中,前躯体的热重变化主要分为三个阶段,其中DSC曲线在770～820℃和850～930℃间有多个小的吸热放热峰出现,对应于复杂的相变.在粉体制备过程中,先于700℃保温3 h再850℃加热5 h的处理,可以获得单一的六方相ZnTiO3粉体.     

纯六方相钛酸锌粉体制备和表征

采用溶胶-凝胶法,用Ti（OC4H9）4、Zn（NO3）2.6H2O、无水乙醇、冰醋酸等原料,利用直接升温和保温-升温两种方法合成超细的六方相ZnTiO3粉体.利用TG-DSC、XRD、SEM等测试分析手段对凝胶的热分解、相转变以及粉体结构形貌进行了表征.实验结果表明：ZnTiO3凝胶的热分析中,前躯体的热重变化主要分为三个阶段,其中DSC曲线在770820℃和850930℃间有多个小的吸热放热峰出现,对应于复杂的相变.在粉体制备过程中,先于700℃保温3 h再850℃加热5 h的处理,可以获得单一的六方相Zn-TiO3粉体.     

阔叶材纸浆纤维素制备胆甾型液晶的研究

以阔叶材纸浆板为原料,研究硫酸水解条件下纤维素微晶悬浮液制备的实验条件,以及纤维素胆甾型液晶织态结构的形成、影响因素及其机理.设计两组实验,通过光学显微镜研究了温度变化对水解后纤维素微晶粒径分布的影响;通过FTIR表征水解前后纤维素微晶表面官能团的变化;通过偏光显微镜确定纤维素胆甾型液晶织构形成的临界浓度.结果表明:在...     

Preparing and studying of phase change energy storage materials

The thermal energy storage phase change material used for building has been prepared with a few of fatty acids based on the principle of binary low eutectic point. The thermal behaviors such as phase transition temperature and enthalpy of compound energy storage material are researched through differential scanning calorimeter (DSC) and scanning electron microscope (SEM). The results show that the thermal energy storage phase change composite material can be used in the wall panels well as its higher latent heat.     

高分辨率双频激光回馈的位移测量方法

在分析双频激光回馈测量原理的基础上,提出了一种基于双频激光回馈原理的高精度位移测量方法,研究了双频激光回馈的基本现象并给出了理论依据,进一步在回馈光学系统基础上,对两路正交的光回馈条纹,利用电路进行细分处理：即5细分和4倍频电路相结合,细分产生的计数脉冲最后送入单片机进行计算及显示．采用可编程逻辑器件FPGA和单片机设计信号处理电路,利用FPGA实现4倍频细分,利用电阻链细分实现5细分．全部电路通过逻辑、时序仿真,验证了本方法的可行性．目前此系统可满足高精度位移测量的要求．     

Quantitative phase analysis of the calcium silicate slag as the residue of extracting alumina from high-alumina fly ash

Calcium silicate slag is the residue of process of pre-desilication alkali lime sintering applied in the high-alumina fly ash to extract the alumina. The quantitative phase analysis (QPA) of the calcium silicate slag has been performed by the Rietveld method based on the powder X-ray diffraction (XRD) with the aid of noncommercial software GSAS-EXPGUI. A known weight of crystalline internal standard (10% CaF₂) was added to the calcium silicate slag to calculate the fraction of amorphous phase and other crystalline phases on an absolute basis. Besides, the calcium silicate slag was characterized by X-ray fluorescence (XRF) and thermo gravimetric (TG) differential scanning calorimetry (DSC) to test the QPA results and investigate its other characters. Finally, the results show that the amorphous fraction is 17.5% (hereinafter, the percentages refer to the mass fraction), and the major crystalline phases detected in the calcium silicate slag consist of 23.5% Beta-Ca2SiO₄, 10.0% bredigite, 10.3% Ca₃Al₂O₆ (C₃A) and 21.6% CaCO₃.     

双偶氮生色开链冠醚的合成

以水杨醛、对硝基(氯、甲氧基)苯胺、乙二胺、二乙烯基三胺为原料，经过先偶联后桥连的方法，合成了2类双偶氮生色开链冠醚，其结构特征是氮杂链作桥链，酚羟基作端基，对位取代的苯偶氮基作为生色基团，形成新的双偶氮化合物5和6的结构经元素分析，红外光谱和质谱得到确定．     

EFFECT OF La-RICH RE ON THE STRUCTURE AND PROPERTIES OF B319 ALLOY IN LOST FOAM CASTING

IntroductionLost foam casting( LFC) process is a newtechnology that is different from the conventionalempty mould cavity casting completely.This tech-nology is an important orientation of casting tech-nology,and is called as casting technology for to-morrow.At present,the studies on LFC are fo-cused on casting techniques mainly[1～ 5] .There islittle information on the structure and mechanicalproperties of B31 9in LFC process.Now for alu-minum alloy in LFC process,the main problemsare se…     

Analysis of ganciclovir and its related substances using high performance liquid chromatography and liquid chromatography-mass spectrometry methods

Objective High performance liquid chromatography (HPLC) and liquid chromatography-mass spectrometry (LC/MS) methods were developed for the determination of ganciclovir and its related substances. Methods A Hypersil ODS2 column (4.6mm×250mm, 5μm) was used with a mobile phase of 0.02M potassium 1.0mL/min, and UV detector set at 254nm was used for monitoring the eluents. Results The method was simple, rapid, selective and capable of separating all related substances at trace level with a detection limit of 0.04μg/mL. It has been validated with respect to accuracy, precision, linearity, and limits of detection and quantification. The linearity range was 10.2-153.0μg/mL with r=0.9998. The percentage recoveries ranged from 96.7% to 101.6%, and RSD was 1.24%-1.96% (n=5). Conclusion The method was found to be suitable not only for monitoring the reactions during the process development but also for quality control of ganciclovir. For identification of related substances, LC/MS was used. The mainly related substances of ganciclovir active pharmaceutical ingredients (API) were determined as guanine, (1, 3-dioxolan-4-yl) methyl acetate, and diacetyl guanine.     

考虑损耗时拉曼放大泵浦光的偏振效应

利用高非线性和较大吸收损耗的光子晶体光纤制作光纤拉曼放大器,是当前的一种趋势,这导致泵浦光非线性旋转效应明显增强．本文在考虑吸收损耗条件下,研究了泵浦光的非线性旋转问题,首次得出了连续光条件下的解析解．结果表明,输入线偏振光与圆偏振光都不会产生非线性旋转,只有椭圆偏振光才有非线性旋转．旋转是绕着邦加球的纬线进行,s3保持不变．随着吸收损耗的增加,有效长度变小,相对的旋转速度变慢．这表明,如果光纤对于泵浦光的吸收越强,越有利于拉曼放大．