ZnS纳米球的水热法制备及其光催化性能研究

在表面活性剂十六烷基三甲基溴化铵(CTAB)的辅助下,以乙酸锌为锌源,硫脲(NH2)2CS为硫源,使用水热法通过改变反应时间,成功制备了不同粒径的ZnS球状颗粒。利用X射线衍射(XRD)、扫描电子显微镜(SEM)、X-射线能谱,高分辨透射电子显微镜(HRTEM))、紫外可见分光光谱和光致发光谱(PL)等测试手段对样品的晶体结构、形貌、光学性质进行了分析。通过对不同粒径的ZnS纳米颗粒对亚甲基蓝的光催化降解的催化活性进行了评估。实验结果表明:在表面活性剂CTAB的作用下,随着反应时间的增加,生成的ZnS晶核生长成纳米颗粒,然后ZnS纳米颗粒将进一步发生团聚从而形成平均粒径超过500nm的ZnS纳米球,但制备的ZnS产物的晶体结构均为立方纤锌矿结构。随着ZnS粒径的增加,样品的紫外吸收峰从418nm逐渐蓝移到362nm,而PL发射峰位的峰强随着粒径的增大而增强。光催化结果显示,反应12h制备的ZnS纳米球的光催化性能最佳。     

ZnS纳米球的水热法制备及其光催化性能研究

在表面活性剂十六烷基三甲基溴化铵(CTAB)的辅助下,以乙酸锌为锌源,硫脲(NH₂)₂CS为硫源,使用水热法通过改变反应时间,成功制备了不同粒径的ZnS球状颗粒.利用X射线衍射(XRD)、扫描电子显微镜(SEM)、X射线能谱,高分辨透射电子显微镜(HRTEM))、紫外可见分光光谱和光致发光谱(PL)等测试手段对样品的晶体结构、形貌、光学性质进行了分析.通过对不同粒径的ZnS纳米颗粒对亚甲基蓝的光催化降解的催化活性进行了评估.实验结果表明:在表面活性剂CTAB的作用下,随着反应时间的增加,生成的ZnS晶核生长成纳米颗粒,然后ZnS纳米颗粒将进一步发生团聚从而形成平均粒径超过500nm的ZnS纳米球,但制备的ZnS产物的晶体结构均为立方纤锌矿结构.随着ZnS粒径的增加,样品的紫外吸收峰从418nm逐渐蓝移到362nm,而PL发射峰位的峰强随着粒径的增大而增强.光催化结果显示,反应12h制备的ZnS纳米球的光催化性能最佳.     

荧光光谱法研究纳米硫化锌与牛血清白蛋白的相互作用

采用水相法合成了ZnS纳米颗粒,通过XRD及TEM技术对纳米ZnS进行了表征,结果表明纳米ZnS的粒径约为7～8 nm.利用荧光光谱考察了纳米ZnS与牛血清白蛋白(BSA)的相互作用,结果显示,两者的相互作用可导致BSA内源荧光猝灭,推测其猝灭机理为静态猝灭,结合常数Ka=1.73×105 L·mol-1,结合位点数n...     

Mn2+掺杂对低温生长ZnS的形貌及光致发光性能的影响

以Zn粉和S粉为原料,Au纳米颗粒为催化剂,采用低温(450℃)化学气相沉积法(CVD),在Si(100)衬底上制备了未掺杂和Mn2+掺杂的ZnS微纳米结构.利用X射线衍射仪(XRD)、能量弥散X射线谱(EDS)、场发射扫描电子显微镜(SEM)和光致发光光谱(PL)等测试手段对样品的结构、成分、形貌和发光性能进行了分析.结果表明,所得ZnS样品均为六方纤锌矿结构,未掺杂的ZnS为微纳米球,在波长为450和463 nm处有2个发光强度较大的蓝光峰;Mn2+掺杂ZnS为纳米线,在波长479和587 nm处分别有1个微弱的蓝光峰和1个强度相对较大的红光峰.此外,还对ZnS微纳米结构的形成过程进行了探讨,并提出了可能的形成机理.     

大麦醇溶蛋白负载白藜芦醇自组装纳米颗粒及其性质研究

采用液-液分散法自组装大麦醇溶蛋白纳米颗粒,重点考察了溶剂(异丙醇)浓度、大麦醇溶蛋白浓度、溶液p H值及离子强度等因素对自组装纳米颗粒粒径和Zeta电位的影响。结果表明:在选择溶剂(异丙醇)浓度为55%,蛋白质浓度为66 mg/m L,分散液p H值为7.0,离子强度为0时,自组装出粒径为(70.0±1.8)nm,Zeta电位9 m V的大麦醇溶蛋白纳米颗粒。在此基础上,进一步制备了白藜芦醇-大麦醇溶蛋白复合纳米颗粒,考察了芯材比对复合纳米颗粒粒径、包封率及载药率的影响,结果表明,当芯材比为1∶5时,自组装复合纳米颗粒的粒径为(135.3±2.5)nm,Zeta电位为(18.91±0.02)m V,包封率为90.4%,载药率为18.8%。扫描电子显微镜结果表明,大麦醇溶蛋白纳米颗粒以及白藜芦醇-大麦醇溶蛋白复合纳米颗粒均为表面光滑的球形颗粒;傅立叶变换红外光谱结果表明,复合纳米颗粒中白藜芦醇与大麦醇溶蛋白之间还存在较强的氢键与静电相互作用。     

极稀溶液体系中自组装合成纳米介孔氧化硅及其铝修饰材料

在极稀溶液中, 通过改变反应溶剂去离子水的量或原料中铝源的量, 可控合成了不同粒径(20~70 nm)、形貌和孔道结构的纳米介孔氧化硅颗粒和纳米介孔铝掺杂氧化硅材料. 这种材料具有高比表面积(BET比表面积1000 m²/g)和较大的孔容(1.1~1.8 cm³/g). 反应物浓度降低或反应物中添加铝源后, 介孔材料的有序性下降, 粒径减小, 孔容增大, 并产生大量的间隙孔. 通过小角X射线衍射(SAXRD)、透射电镜和氮气吸附-脱附实验表征了样品.     

纳米Pb(II)-没食子酸配合物的合成及其燃烧催化性能

采用液相分散沉淀法制备了纳米 Pb(II)-没食子酸配合物粉体. 用热重分析(TG)、X 射线衍射仪(XRD)、透射电镜(TEM)、核磁共振仪(1H NMR)、红外光谱仪(IR)、激光散射粒径分析仪和元素分析仪对样品的物相、形貌、粒径和组成进行了表征. 研究了没食子酸的浓度和分散剂用量对产物的粒子大小的影响. 并测试了产物对推进剂燃烧的催化作用. 结果表明: 产物的平均粒径约为 30 nm. 没食子酸的浓度降低和分散剂用量增加均使产物的粒子减小. 产物能明显改善推进剂的燃烧性能, 使推进剂的燃速提高 88%, 压强指数降低了 70%.     

纳米颗粒跟踪分析仪用于二氧化钛纳米颗粒分散及检测

以纳米颗粒跟踪分析仪为检测手段,建立了二氧化钛(TiO2)纳米颗粒分散和检测的方法,考察了分散剂种类、超声方式、超声时间、超声温度、分散试剂浓度、pH值对TiO2分散的影响,以及本分散方法对于一般商品TiO2的通用性.采用NTA测定粒径和颗粒数量浓度,对检测过程中稀释试剂浓度、稀释倍数等检测条件进行了优化,颗粒数量浓度...     

一种新型季胺盐壳聚糖纳米载药体系的制备与性能

在制备壳聚糖衍生物N,N,N-三甲基壳聚糖盐酸盐(TMC)的基础上,通过将两种性质相反的电解质溶液进行共混,制备了一种新型的 TMC/CMC(羧甲基壳聚糖)纳米载药颗粒体系.用激光散射仪和透射电镜表征了空白颗粒和载药颗粒的粒径、粒径分布、Zeta 电位和形态结构.栽药体系纳米颗粒的粒径在 200～600 nm 范围,表面可带正或负电荷,且 Zeta 电位具有可调性.研究表明:牛血清蛋白(BSA)的包封率与起始的 TMC、BSA 浓度相关;纳米载药颗粒对 BSA 的释放表现为,先爆释而后缓释并可保持 40 h 以上的释放.     

纳米Pb(II)-没食子酸配合物的合成及其燃烧催化性能

采用液相分散沉淀法制备了纳米Pb(II)-没食子酸配合物粉体. 用热重分析(TG)、X射线衍射仪(XRD)、透射电镜(TEM)、核磁共振仪(¹H NMR)、红外光谱仪(IR)、激光散射粒径分析仪和元素分析仪对样品的物相、形貌、粒径和组成进行了表征. 研究了没食子酸的浓度和分散剂用量对产物的粒子大小的影响. 并测试了产物对推进剂燃烧的催化作用. 结果表明: 产物的平均粒径约为30 nm. 没食子酸的浓度降低和分散剂用量增加均使产物的粒子减小. 产物能明显改善推进剂的燃烧性能, 使推进剂的燃速提高88%, 压强指数降低了70%.     

二氧化碳和丙烯直接合成甲基丙烯酸的NiPMo/TiO2催化剂的研究

用溶胶-凝胶法以磷钼酸(MPA)的镍盐溶液水解钛酸四丁酯制备了NiPMo/TiO2催化剂.使用ICP、 XRD、 TG-DTA、 IR、 TPD-MS和微反应技术研究了催化剂的化学组成、热稳定性、化学吸附性质和催化反应性能.杂多钼酸盐与TiO2通过O2-在TiO2表面发生了键合.在623 K下,杂多阴离子仍保持原有的Keggin结构.CO2在Lewis酸位Ni(Ⅱ)和Lewis碱位Ni-O-Mo的桥氧协同作用下生成CO2卧式吸附态Ni(Ⅱ)←O-(CO)←(O--Ni).丙烯有多种吸附态在催化剂上吸附.在563 K、 1 MPa和空速1500 h-1的反应条件下,丙烯的摩尔转化率为3.2%,产物MAA选择性为95%.     

Synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives

Different approaches for the synthesis of 1-benzyloxypyrazin-2(1H)-one derivatives from simple amino acids have been investigated. A library of 33 precursors for the preparation of N-hydroxy pyrazinones was obtained in moderate to good yields.     

Toward new camptothecins. Part 6: Synthesis of crucial ketones and their use in Friedländer reaction

In the context of the preparation of camptothecin and luotonin A analogs, the synthesis of some key keto-precursors and their use in Friedländer condensation are described. This paper also focuses on the stability of these keto intermediates and emphasizes the major differences between indolizinones and pyrroloquinazolinones series. Noteworthy is also the report of some original structures isolated as by-products of some experiments.     

CoFe2O4自形成磁性液体场致结构化对磁化的影响

The Langevin paramagnetic theory can’t describe the relation between magnetization of ferrofluids and applied magnetic field. The structuralization of ferrofluids, which is considered the main influence factor of the magnetization, is regarded. The part of magnetization works is deposited when the structure is forming. This action influences the magnetization of ferrofluids directly or indirectly. On the base of the “compressing” model, the Langevin function that usually describes the magnetization of ferrofluid is modified, and a well-fitted curve is obtained. An equation of the relation between the equivalent volume fraction after being “compressed” and the intensity of magnetic field is discovered, which approximately describes the process of magnetization. The relation between the approximate initial susceptibility and the volume fraction can be obtained from modified formula.     

Highly regioselective Buchwald–Hartwig amination at C-2 of 2,4-dichloropyridine enabling a novel approach to 2,4-bisanilinopyridine (BAPyd) libraries

The highly regioselective Buchwald–Hartwig amination at C-2 of the cheap and readily accessible reagent, 2,4-dichloropyridine with a range of anilines and heterocyclic amines is described. This new methodology is robust and provides a facile access to 4-chloro-N-phenylpyridin-2-amines on 0.25 mol scale. These intermediates undergo a further Buchwald–Hartwig amination at higher temperature to enable rapid exploration of the chemical space at C-4 and to provide a library of 2,4-bisaminopyridines.     

KMnO4-mediated oxidative CN bond cleavage of tertiary amines: Synthesis of amides and sulfonamides

KMnO₄-mediated oxidative CN bond cleavage of tertiary amines producing secondary amine was introduced, which was trapped by electrophiles (acyl chloride and sulfonyl chloride) to form amides and sulfonamides. The reaction could take place at mild condition, tolerating a wide range of function groups and affording products in moderate to excellent yields.     

Chemistry of heterocyclic compounds at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences, over 50 years (Review)

The review contains a concise historical account and information on the most significant researches undertaken by the staff at the A. E. Favorsky Irkutsk Institute of Chemistry, Siberian Branch of the Russian Academy of Sciences on the Chemistry of Heterocyclic Compounds. Dedicated to Academician of the Russian Academy of Sciences B. A. Trofimov on his 70th jubilee. Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 10, pp. 1443–1502, October, 2008.     

A general and convenient synthesis of 4-(tosylmethyl)semicarbazones and their use in amidoalkylation of hydrogen,heteroatom, and carbon nucleophiles

A general synthesis of previously unknown semicarbazone-based α-amidoalkylating reagents, 4-(tosylmethyl)semicarbazones, has been developed. The synthesis involved three-component condensation of semicarbazones of aliphatic or aromatic aldehydes with the same or other aldehydes and p-toluenesulfinic acid. The scope and limitations of this reaction were investigated. The compounds obtained were demonstrated to be an efficient α-(4-semicarbazono)alkylating agents. They were reacted with H- (sodium borohydride), O- (sodium methylate), S- (sodium phenylthiolate), N- (pyrrolidine, sodium succinimide), P- (trialkyl phosphites), and C-nucleophiles (sodium diethyl malonate) to give the corresponding products of the tosyl group substitution, 4-substituted semicarbazones, including analogues of nitrofurazone. Among the prepared compounds tested in vitro for antibacterial and antifungal activity, three nitrofuryl-containing semicarbazones exhibited high biological activities with minimum inhibitory concentration (MIC) values of 8–32 μg/mL.     

Sulfur-directed metal-free and regiospecific methyl C(sp3)–H imidation of thioanisoles

Regiospecific and direct imidation of the methyl C(sp³)–H bond of thioanisoles is realized under mild and metal-free conditions with N-fluorobis(benzenesulfonyl)imide as an oxidant and nitrogen source. Proposed mechanism suggests that thionium ion intermediates and a Pummerer-type reaction are involved. The imidation has advantages such as high step-economy, excellent functionality tolerance, and regiospecificity, giving structurally diverse imidation products.     

Synthesis of novel chiral bidentate hydroxyalkyl-N-heterocyclic carbene ligands and their application in palladium-catalyzed Mizoroki–Heck couplings and asymmetric addition of diethylzinc to benzaldehyde

A small library of new chiral bidentate hydroxyalkyl-imidazolium salts 1 is conveniently synthesized on multi-gram scale from inexpensive and commercially available chiral pool amino acids. The corresponding carbenes, generated by deprotonation of imidazolium salts 1, in combination with palladium(II) chloride were tested in the Mizoroki–Heck coupling reaction. The most significant results in terms of yields and reactivities were achieved with low catalyst loading. The catalytic activities of these imidazolium salts were also investigated in the asymmetric addition of diethylzinc to benzaldehyde. The use of MgO nanoparticles as an additive in conjunction with these ligands played a crucial role in increasing the efficiency of these reactions.