足球状CdS微米球的合成与发光性能的初步研究

应用化学水浴沉淀法,合成了具有特殊形貌的由纳米颗粒组成的Cds微米球,通过改变反应温度实现了对产物尺寸的控制．XRD测试结果表明生成产物为结晶良好的六角结构CdS,PL谱测试说明了产物有较好的光致发光性能．利用TEM,SAED,FEG-SEM和紫外吸收谱分析等测试手段对其结构和形成机理进行了研究．     

离子液体中微波合成纳米结构的Bi2S3和Bi19Br3S27

在不同咪唑基离子液体中, 利用微波辅助法快速合成了不同形貌的Bi2S3纳米粒子和Bi19Br3S27纳米棒. 利用XRD, TEM和SEM对合成产物进行了结构和形貌的表征. 实验结果表明离子液体在合成过程中对产物的相结构和形貌发挥了重要的作用. 实验中还进一步考察了不同实验条件对产物形貌的影响. 对实验的合成机理进行了初步探讨. 对不同形貌和纳米结构的Bi2S3和Bi19Br3S27进行了UV-Vis光谱分析.     

GaN纳米带、纳米环和Z字结构纳米线在金属镓颗粒上的原位生长及其发光性质

在1050℃氨气和氢气混合气氛中加热金属镓,在镓颗粒表面原位生长出了GaN纳米带、纳米环和Z字结构纳米线．利用激光拉曼光谱仪、扫描电子显微镜和透射电子显微镜对产物进行了表征,结果表明,所得不同形貌GaN纳米结构均为单晶六方纤锌矿结构,纳米带宽度在20～300nm,长达30gm;纳米环直径在5-8gm;Z字结构纳米线的直径约为160nm．研究了反应温度和时间对产物形貌和结构的影响,提出了不同形貌GaN纳米结构的可能形成机理．从GaN纳米结构的发光光谱中观察到了发光峰位于361nm强的紫外光发光和456nm弱的蓝光发光,这两种发光分别起源于GaN宽带隙带边的激子发射和浅的给体向深的局域受体的跃迁．     

纳米MnO2：水热法制备及盐对晶型和形貌的影响

在水热条件下,向反应体系中加入简单的无机盐,利用KMnO4和MnCl2反应生成不同晶型/形貌的一维MnO2纳米材料.用X-射线衍射(XRD)、场发射扫描电镜(FESEM)、透射电镜(TEM)、高分辨透射电镜(HRTEM)以及选区电子衍射(SAED)等对产物进行了结构和形貌的表征.结果显示,加入的简单无机盐不仅影响产物的晶型,同时也对产物的形貌也起到了控制作用.     

前处理时间对Co_3O_4形貌及光催化性能的影响

以Co Cl2、Na2CO3为原料,以油酸钠(SOA)为表面活性剂,采用水热-热分解法合成了纯相尖晶石结构的Co3O4粉体。利用TG-DTA、XRD和SEM等手段跟踪反应过程,研究了不同水热时间对产物形貌和结构的影响,并根据实验结果分析了可能的反应机理及结构对光催化性能的影响。实验结果表明:制备前驱体的水热时间是影响产物形貌的关键因素,并且终产物的结构形貌很大程度上决定了其光催化性能。     

表面活性剂种类对纳米氧化锌形貌的影响

利用简单的水热法,以Zn(Ac)2.2H2O为锌源,通过调整表面活性剂的种类及碱源,制备了一系列不同形貌的纳米结构氧化锌;利用场发射扫描电子显微镜和X射线粉末衍射仪分析了产物的形貌和晶体结构,并探讨了多种表面活性剂和醋酸钠碱源对氧化锌纳米结构的影响.结果表明,以NaOH作为碱源时,在不添加任何表面活性剂的情况下,产物的形貌结构与氢氧化钠的加入量有关,当n(Zn2+)∶n(OH-)为1∶2.5、1∶10及1∶20时,分别得到片状、棒状及海胆状纳米结构的氧化锌;产物均为六方相氧化锌.     

氧化亚铜微/纳米结构的形貌可控制备及光催化和防污性能

利用简便易行的液相法,采用葡萄糖为还原剂,通过调整加料方式、反应温度、NaOH用量等条件,实现具有{110}截面八面体、八面体和短足形等形貌的Cu2O微/纳米结构的可控制备,运用透射电子显微镜、扫描电子显微镜、紫外可见分光光度计等对产物进行组成、结构、形貌和光响应的表征,对Cu2O的形貌结构和生长机理进行研究。对比和优化了具有不同形貌的Cu2O微/纳米结构对甲基橙染料的光催化性能。将不同形貌的微/纳米Cu2O作为防污剂复配的自抛光防污涂料,涂层磨蚀率、接触角与实海挂板实验证明该涂料具有良好的防污性能。     

回流法可控合成BiPO4纳米棒及其光催化性能

采用回流法合成了BiPO₄纳米棒光催化剂, 探讨了反应时间、反应物比例、pH值和反应物浓度对BiPO₄晶相结构和形貌尺寸的影响, 利用粉末X射线衍射(XRD)、透射电镜(TEM)、比表面积分析(BET)和紫外-可见漫反射光谱(UV-Vis DRS)等对产物进行了表征, 以亚甲基蓝(MB)为探针研究了其光催化活性. 反应时间和反应物浓度对产物的形貌尺寸影响较大, 反应物比例和pH值对产物晶相结构和形貌尺寸均有较大的影响, 进一步影响BiPO₄光催化剂的活性. 调控各种因素后可合成出具有单斜相独居石/六方相混晶结构的高紫外光活性BiPO₄纳米棒光催化剂.     

N2流量对GaN的形貌及光学和电学性能的影响

采用化学气相沉积法(CVD)在Si(100)衬底上以Ni为催化剂,金属Ga和NH3为原料合成了GaN微纳米结构,并研究了N2流量对产物GaN的形貌及光学和电学性能的影响。利用场发射扫描电子显微镜(SEM)、透射电镜(TEM)、X射线衍射仪(XRD)、Xray能谱仪(EDS)、光致发光谱(PL)和霍尔效应测试仪(HMS-3000)等测试手段对样品的形貌、结构、成分、光学和电学性能进行了分析。结果表明,随着N2流量的增加,产物GaN的形貌发生了由微米棒到蠕虫状线再到光滑纳米线的转变;生成的GaN均为六方纤锌矿结构;样品均表现出383 nm的近带边紫外发射峰和470 nm左右的蓝光发射峰;所有样品均为p型;并对产物GaN的形貌转变机理进行了分析。     

氧化铜纳米片的水热合成与表征

利用水热法一步制备了形貌均一的氧化铜纳米片,借助场发射扫描电子显微镜、X射线粉末衍射仪和透射电子显微镜分析了产物的形貌和晶体结构;并研究了反应物浓度及表面活性剂等因素对氧化铜纳米结构的影响.结果表明,以氢氧化钠作为碱源时,在不添加任何表面活性剂的情况下,随着氢氧化钠浓度的升高,纳米片的尺寸减小、厚度增大;此外,通过添加不同的表面活性剂可以得到不同形貌的氧化铜纳米结构.     

1-肼基-2,3-二氮杂萘盐酸盐的合成新方法

研究了l-肼基-2,3-二氮杂萘盐酸盐的合成新方法.以相对廉价易得的邻苯二甲酸酐为起始原料,依次通过还原、溴代、环合、取代、酸化等反应步骤得到目标产物1-肼基-2,3-二氮杂萘盐酸盐.研究表明该方法具有原料便宜易得、收率高、产物易分离纯化、后处理操作简单、总成本低等优点.     

Green polymer chemistry: new methods of polymer synthesis using renewable starting materials

The present article reviews the recent results reported mainly from our group on “green polymer chemistry”. Characteristic important aspects of green polymer chemistry include herein, typically (1) using renewable resources as starting materials for polymer production, and (2) employing green method for the polymer synthesis. As renewable starting materials, the following materials were employed; lactic acid, itaconic anhydride, renewable plant oils, and cardanol. Polymer production using these materials contributes to mitigate the carbon dioxide emission because of their “carbon neutral” nature. As green method, lipase enzyme was mainly used for polymerization catalyst, since lipase is a natural benign catalyst, showing a specific catalysis as well as recyclable character. Polymer synthesis from these materials and the catalyst provided various value-added functional polymers, demonstrating good examples of green polymer chemistry.

     

以粉煤灰为原料合成Eu3+掺杂的铝硅酸钠发光材料

以粉煤灰为原料,采用固相法合成了Eu3+掺杂的铝硅酸钠发光材料。利用粉末X射线衍射仪(XRD)、扫描电子显微镜(SEM)、热分析技术(TG-DSC)、荧光光谱仪(PL)等对合成的样品进行表征,并与以分析纯的SiO2和Al2O3为原料得到的样品进行比较。结果表明:由不同的起始原料制备的NaAlSiO4:Eu3+均具有六方相结构;两种样品的形貌均不太规则,由许多小的球形颗粒和块状团聚体组成;由不同原料得到样品的TG-DSC曲线的变化趋势大致相同;在254及395 nm的紫外光激发下,均表现出Eu3+的特征发射。该研究为提高粉煤灰综合利用率、促进资源循环利用、减少其对环境的污染提供了一种新的思路。     

Synthesis of Calcium Phosphates by Gas-Solid Reaction of CaO-P 2 O 5

Calcium phosphates are useful materials in fertilizer, dentifrice, biomaterials, etc., and have been popularly synthesized by a wet method, a hydrothermal method, a flux method, and a solid-state reaction method. However, there has been no report on synthesis by chemical vapor deposition (CVD) method or gas-phase reaction. In the present study, calcium phosphates were synthesized by gas-solid reaction of CaO solid and P 2 O 5 gas. The CaO/P 2 O 5 ratio of starting materials was changed from 5.06 to 0.64, and the reaction was carried out at 400-1100;C. These calcium phosphates were investigated using X-ray diffractometry (XRD) and scanning electron microscope (SEM). By gas-solid reaction of CaO-P 2 O 5 , g -MET only was synthesized at 400-500;C, g -MET, HA, and g -PYR at 600-700;C, and g -MET, HA, g -PYR, and g -TCP above 800;C. Synthesized calcium phosphates were independent on the CaO/P 2 O 5 ratio of starting materials but dependent on the reaction temperature.     

Separation and Quantification of Key Starting Materials of Irbesartan Using Liquid Chromatography–Mass Spectrometry as a Separation and Identification Tool

Abstract

A liquid chromatography–mass spectrometry (LC-MS) method was developed and validated for determining the levels of 4-methyl-2-cyano biphenyl and 4-bromomethyl-2-cyano biphenyl, which are key starting materials of an antihypertensive drug substance, irbesartan. An active pharmaceutical ingredient of irbesartan was synthesized by using these two starting materials for its therapeutic use. We have explicated the LC-MS method to separate and quantify these two compounds in irbesartan at nanogram levels. The method was capable of separating irbesartan and its starting materials, which were monitored for their absence in the finished product of irbesartan. The separation was carried out at 40°C on a 150- × 4.6-mm cyano column by using the mobile phase containing 60 volumes of water adjusted to pH 3.2 with formic acid and 40 volumes of acetonitrile. The detection wavelength was 220 nm. The MS involved an electrospray ionization (ESI) probe and ion-trap analyzer and was validated with respect to its specificity, accuracy, and precision.     

Efficient access to azaindoles and indoles

[Structure: see text] An expedient, catalytic method for the synthesis of diverse azaindoles and indoles, starting from readily available and inexpensive starting materials, is described. Conditions were developed for effective reductive alkylation of electron-deficient o-chloroarylamines, substrates previously viewed as poor partners in this reaction. The derived N-alkylated o-chloroarylamines were elaborated to N-alkylazaindoles and N-alkylindoles via a novel one-pot process comprising copper-free Sonogashira alkynylation and a base-mediated indolization reaction.     

吲哚衍生物合成与应用的研究进展

综述了以苯胺衍生物(或硝基苯衍生物)为原料合成吲哚衍生物的方法和吲哚衍生物的应用。吲哚类化合物的合成方法主要有：Fischer合成法,苯胺衍生物合成法,硝基衍生物合成法和Nenitzescu合成法等。吲哚衍生物在制药、染料和香料等领域有重要应用。参考文献105篇。     

新型多取代3-烯基吲哚的合成

开发了一种以吲哚为起始原料,合成具有多个反应位点的多取代3-烯基吲哚的新方法,合成了9个目标化合物,其中8个为新化合物,其结构经¹H NMR, ¹³C NMR和HR-MS(ESI)表征。     

Study of hydrothermally synthesized LiFePO4 with different morphology

Monodispersed LiFePO₄ particles with different morphology have been successfully obtained through hydrothermal method using same starting materials. The morphology of the as-synthesized LiFePO₄ particles were dependent on feeding sequence of starting materials. Different dissolution rate of solid phase in precursor prepared by reversing feeding sequence lead to different morphology. The half-cell using as-obtained LiFePO₄ with different morphology were assembled to investigate electrochemical performance. The results show that LiFePO₄ with nanorods morphology displays a higher initial discharge capacity and excellent cycle retention than the sample with microplates morphology.

     

草酸处理对丙烷氨氧化催化剂Sb-V-O结构和催化性能的影响

以不同量的草酸处理钒的起始原料,采用共沉淀法制备了VSb3混合氧化物催化剂,运用N2低温吸附、X射线衍射、X射线光电子能谱和H2程序升温还原等方法对催化剂进行了表征,并考察了其在丙烷氨氧化反应中的催化性能.结果表明,草酸的处理可使所得样品中V处于较低的价态,从而有利于活性相SbVO4的生成.当草酸/V(摩尔比)为3时,所制VSb3混合氧化物中存在较多的活性相SbVO4,且其表面具有适量Sb和V的分布,使催化剂具有良好的氧化/还原性能平衡,因而在丙烷氨氧化反应中表现出更高的活性和丙烯腈选择性.