含吡啶基取代多苯基芳基有机硅化合物的合成

2,4,5-三苯基、3-吡啶基环戊二烯酮(4),分别与烯丙基三乙氧基硅烷及乙烯基三乙氧基硅烷发生Diels-Alder反应,生成2,4,5-三苯基3-吡啶基苄基三乙氧基硅烷(5)、2,4,5-三苯基3-吡啶基苯基三乙氧基硅烷(6)、1,3,4-三苯基2-吡啶基苯(7)和1,3,4-三苯基2-吡啶基二环[2.2.1]-2-烯-7-酮(8)。它们的产率分别为75％、41％、10％和10％。     

含吡啶基取代多苯基芳基有机硅化合物的合成

2,4,5-三苯基,3-吡啶基环戊二烯酮(4), 分别与烯丙基三乙氧基硅烷及乙烯基三乙氧基硅烷发生Diels-Alder反应, 生成2,4,5-三苯基 3-吡啶基苄基三乙氧基硅烷(5),2,4,5-三苯基 3-吡啶基苯基三乙氧基硅烷(6),1,3,4-三苯基 2-吡啶基苯(7)和1,3,4-三苯基 2-吡啶基二环[2.2.1]-2-烯-7-酮(8). 它们的产率分别为75%, 41%, 10%和10%.     

直接法制备三乙氧基硅烷催化剂的研究进展

综述了直接法合成三乙氧基硅烷的研究进展,着重对直接法的反应机理和催化剂组分的筛选进行了分析讨论.同时介绍了以三乙氧基硅烷为原料,合成烯丙基三乙氧基硅烷、γ-(2,3-环氧丙氧)丙基三乙氧基硅烷、苯乙基三乙氧基硅烷、五乙氧基二硅烷等衍生物的工艺,提出了催化剂制备过程中存在的问题及研究方向.     

聚γ-(β-氰乙基)胺丙基硅氧烷铂配合物的合成与催化性能

γ-氨丙基三乙氧基硅烷与丙烯腈反应，得到γ-(β-氰乙基)胺丙基三乙氧基硅烷。后者用气相法二氧化硅固载，再与氯亚铂酸钾反应，合成了聚γ-(β-氰乙基)胺丙基硅氧烷铂配合物。研究了它对不饱和烃与三乙氧基硅烷的硅氢加成反应的催化特性。     

五甲基-2-噻吩基二硅烷的光解反应

本文研究了五甲基-2-噻吩基二硅烷的光解反应, 反应以环乙烷为溶剂, 乙醇作为捕捉剂, 主要产物是二甲基-2-噻吩基硅烷, 三甲基-2-噻吩硅烷, 三甲基乙氧基硅烷和二甲基乙氧基硅烷。     

γ—（乙二胺基）丙基三乙氧基硅烷的合成

γ-(乙二胺基)丙基三乙氧基硅烷是一种新型的偶联剂和交联剂。其合成方法可首先通过γ-氯丙基三氯硅烷与无水乙醇发生醇解反     

3-己酰基硫代-1-丙基三乙氧基硅烷的合成及其在SSBR/SiO_2复合体系中偶联效果研究

以γ-巯丙基三乙氧基硅烷与己酰氯为单体,在N2保护与低温下合成偶联剂3-己酰基硫代-1-丙基三乙氧基硅烷(HXT),将HXT与双-(3-乙氧基硅基丙基)二硫化物(TESPD)分别添加于溶液聚合丁苯橡胶(SSBR)/SiO2混炼胶复合体系中.采用流变学方法表征复合体系的动态粘弹行为,发现HXT可改善填料和基体的相互作用,有效阻止SiO2粒子在加工过程中的团聚.与TESPD相比较,含HXT体系具有较高“Payne效应”临界应变值.     

聚γ-(2-噻唑脲基)丙基倍半硅氧烷配合物的合成及磁性能

以2-氨基噻唑和异氰酸酯丙基三乙氧基硅烷为原料,合成了γ-(2-噻唑脲基)丙基三乙氧基硅烷(TUPTES),并采用溶胶-凝胶工艺制备了其过渡金属配合物(PTUPTES-Cu,PTUPTES-Ni).用红外光谱、核磁共振谱、扫描电镜和能谱等分析手段进行了表征.磁性测试结果表明,两种配合物在低温下都是较好的软铁磁体,其居里-外斯温度分别为119和75 K.     

(4S)-4-羧基杂氮硅三环的合成

利用L-N,N-双(β-羟乙基)丝氨酸及L-N,N-双(β-羟乙基)苏氨酸与三乙氧基硅烷或氯烷基三乙氧基硅烷反应合成了具有手性的(4S)-4-羧基杂氮硅三环(1～5),并运用IR、~1HNMR、EI-MS等手段表征了结构。证据显示存在着贯穿笼状结构的N→Si配键。     

高分子膜湿度传感器的制备

近年来对高分子电解质湿敏材料的研制十分活跃,本文报道以聚γ-氨丙基三乙氧基硅烷季铵化合物的湿敏材料及其元件性能。 试剂 γ-氨丙基三乙氧基硅烷(盖县化工厂),使用前蒸馏,折光指数n_D~(20)为1.4190;碘甲烷、十六烷基三甲基溴化铵、甲苯、无水乙醇皆为分析纯。     

Detail review on chemical,physical and green synthesis,classification, characterizations and applications of nanoparticles

ABSTRACT

Nanotechnology is an emerging field of science. The base of nanotechnology is nanoparticles. The size of nanoparticles ranges from 1 to 100?nm. The nanoparticles are classified into different classes such as inorganic nanoparticles, organic nanoparticles, ceramic nanoparticles and carbon base nanoparticles. The inorganic nanoparticles are further classified into metal nanoparticles and metal oxide nanoparticles.similarly carbon base nanoparticles classified into Fullerene, Carbon nanotubes, Graphene, Carbon nanofiber and carbon black Nanoparticles are also classified on the basis of dimension such as one dimension nanoparticles, two-dimension nanoparticles and three-dimension nanoparticles. The nanoparticles are synthesized by using two approaches like top-down approach and bottom-up approach. In this review chemical, physical and green synthesis of nanoparticles is reported. The synthesized nanoparticles are synthesized using different qualitative and quantitative techniques. The Qualitative techniques include Fourier Transform Infrared Spectroscopy (FT-IR), UV-Vis spectrophotometry, Scanning electron microscope (SEM), X.ray diffraction (XRD) and Atomic Force Microscopy (AFM). The Quantitative techniques include Transmission Electron Microscopy (TEM), Annular Dark-Field Imaging (HAADF) and Intracranial pressure (ICP). The nanoparticles have different application which is reported in this review.     

Effects of surface coordination chemistry on the magnetic properties of MnFe(2)O(4) spinel ferrite nanoparticles

To understand the influence of surface interactions upon the magnetic properties of magnetic nanoparticles, the surface of manganese ferrite, MnFe(2)O(4), nanoparticles have been systematically modified with a series of para-substituted benzoic acid ligands (HOOC-C(6)H(4)-R; R = H, CH(3), Cl, NO(2), OH) and substituted benzene ligands (Y-C(6)H(5), Y = COOH, SH, NH(2), OH, SO(3)H). The coercivity of magnetic nanoparticles decreases up to almost 50% upon the coordination of the ligands on the nanoparticle surface, whereas the saturation magnetization has increased. The percentage coercivity decrease of the modified nanoparticles with respect to the native nanoparticles strongly correlates with the crystal field splitting energy (CFSE) Delta evoked by the coordination ligands. The ligand inducing largest CFSE results in the strongest effect on the coercivity of magnetic nanoparticles. The change in magnetic properties of nanoparticles also correlates with the specific coordinating functional group bound onto the nanoparticle surface. The correlations suggest the decrease in spin-orbital couplings and surface anisotropy of magnetic nanoparticles due to the surface coordination. Such surface effects clearly show the dependence on the size of nanoparticles.     

醇热解法合成超顺磁性氧化铁纳米粒子及其性能

以甲氧基聚乙二醇同时作为溶剂、还原剂及修饰剂,在高温下分解乙酰丙酮铁,制备了纳米Fe3O4粒子,采用透射电子显微镜和X射线衍射分析表征材料的形貌和相组成,傅里叶变换红外光谱仪表征材料的表面修饰物,超导量子干涉仪测试合成的纳米粒子的磁性能,纳米粒度与zeta电势分析仪测试磁性纳米粒子在水中的zeta电势。 结果表明,纳米Fe3O4粒子的大小为（10.1±1.6） nm,粒度均一,单分散性好,在300 K下具有超顺磁性,饱和磁化强度为45 A·m2/kg。 红外结果表明,-COO-共价结合在粒子表面。 zeta电势为-25 mV。 其在水中的稳定性与以三甘醇为反应介质、高温分解法制备的纳米Fe3O4粒子作比较,表现出长时间（60 d以上）的良好分散性。 静电作用及空间位阻效应是其高稳定分散性的原因。     

Enhanced photocatalytic degradation of C.I. Basic Violet 2 using TiO2-SiO2 composite nanoparticles

In this report, TiO(2) -SiO(2) composite nanoparticles were prepared by the thermal hydrolysis method using titanium tetrachloride and tetraethylorthosilicate as TiO(2) and SiO(2) precursors, respectively. The prepared nanoparticles were characterized by X-ray powder diffraction (XRD), Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), nitrogen adsorption/desorption and UV-Vis diffuse reflectance spectroscopy (DRS). The results indicated that, in comparison with pure TiO(2), TiO(2)-SiO(2) composite nanoparticles had a higher thermal stability, which prevents phase transformation from anatase to rutile. In addition, the TiO(2)-SiO(2) nanoparticles had a higher specific surface area, larger pore volume, greater band gap energy and smaller crystallite size. Thus, the surface area of TiO(2)-40% SiO(2) composite nanoparticles was about 17 times higher than that of pure TiO(2) nanoparticles. The photocatalytic activity of TiO(2)-SiO(2) composite nanoparticles in the photodegradation of C.I. Basic Violet 2 was investigated. The photodegradation rate of Basic Violet 2 using TiO(2)-40% SiO(2) nanoparticles calcined at 600°C was much faster than that using pure TiO(2) and Degussa P25 TiO(2) by 10.9 and 4.3 times, respectively. The higher photoactivity of the TiO(2)-SiO(2) composite nanoparticles was attributed to their higher surface area, larger pore volume, greater band-gap energy and smaller crystallite size compared with pure TiO(2).     

Preparation and application of polystyrene‐grafted ZnO nanoparticles

The precursor of ZnO was prepared by precipitation and ZnO nanoparticles were obtained by calcination afterwards. Poly(styrene) (PSt) was grafted onto the ZnO nanoparticles in a non‐aqueous suspension to reduce the aggregation among nanoparticles and to improve the compatibility between nanoparticles and the organic matter. The obtained samples were characterized by X‐ray powder diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared spectroscopy (FT‐IR), zeta potential measurement, lipophilic degree (LD) test, photocatalytic experiments, sedimentation test, and contact angle measurement. The LD of composite particles after a high‐temperature treatment was stable. The photoluminescence of PSt‐grafted ZnO nanoparticles was observed by naked eyes and was recorded using a digital camera. The ZnO nanoparticles were used to reinforce poly(vinylidene fluoride) (PVDF) films and the mechanical and electric properties of the films were also measured. Copyright © 2007 John Wiley & Sons, Ltd.     

憎水性三金属纳米粒子的合成、表征及磁性

以磺基琥珀酸二辛酯钠盐(AOT)为表面活性剂,采用反胶束法合成了憎水性CoFe/Au纳米粒子, 利用配体交换、水洗等去除AOT并使纳米粒子分级.采用紫外-可见光谱(UV-Vis)、透射电镜(TEM)、X射线衍射(XRD)、X射线电子能量散射(EDX)及等离子发射光谱 (ICP)等对产物进行了表征,通过超导量子干涉仪(SQIUD)研究了纳米粒子的磁性质.结果表明,反胶束法合成的CoFe/Au三金属纳米粒子具有较好的单分散性和稳定性,平均粒径约为4 nm.当外磁场强度为1.5×10⁴ A/m时,阻塞温度T_b为65 K,温度高于T_b时纳米粒子显示出超顺磁性,低于T_b时呈铁磁性,在5 K时其矫顽力(Hc)达4.67×10⁴ A/m.     

Size-dependent interaction of silica nanoparticles with different surfactants in aqueous solution

The size-dependent interaction of anionic silica nanoparticles with ionic (anionic and cationic) and nonionic surfactants has been studied using small-angle neutron scattering (SANS). The surfactants used are anionic sodium dodecyl sulfate (SDS), cationic dodecyltrimethyl ammonium bromide (DTAB), and nonionic decaoxyethylene n-dodecylether (C(12)E(10)). The measurements have been carried out for three different sizes of silica nanoparticles (8, 16, and 26 nm) at fixed concentrations (1 wt % each) of nanoparticles and surfactants. It is found that irrespective of the size of the nanoparticles there is no significant interaction evolved between like-charged nanoparticles and the SDS micelles leading to any structural changes. However, the strong attraction of oppositely charged DTAB micelles with silica nanoparticles results in the aggregation of nanoparticles. The number of micelles mediating the nanoparticle aggregation increases with the size of the nanoparticle. The aggregates are characterized by fractal structure where the fractal dimension is found to be constant (D ≈ 2.3) independent of the size of the nanoparticles and consistent with diffusion-limited-aggregation-type fractal morphology in these systems. In the case of nonionic surfactant C(12)E(10), micelles interact with the individual silica nanoparticles. The number of adsorbed micelles per nanoparticle increases drastically whereas the percentage of adsorbed micelles on nanoparticles decreases with the increase in the size of the nanoparticles.     

Preparation of Silver Nanoparticles through Alcohol Reduction with Organoalkoxysilanes

Silver nanoparticles of narrow size distribution were prepared through the chemical reduction in an alcohol solution with several organoalkoxysilanes. In this system, organoalkoxysilanes served as a stabilizer, protecting silver nanoparticles from aggregation. The changes in size and morphology of colloidal silver nanoparticles were investigated with the addition of organoalkoxysilanes such as 3-aminopropyltriethoxysilane (APS), methyltriethoxysilane (MTS), phenyltrimethoxysilane (PTS), vinyltriethoxysilane (VTS), and 3-glycidoxypropyltrimethoxysilane (GPS) as stabilizers. The organic functional groups of organoalkoxysilanes interact with silver ions and clusters, which stabilize silver nanoparticles in the system. The silver nanoparticles obtained were characterized with transmission electron microscopy (TEM), UV-vis spectroscopy, etc.     

Preparation of surface plasmon resonance biosensor based on magnetic core/shell Fe3O4/SiO2 and Fe3O4/Ag/SiO2 nanoparticles

In this paper, surface plasmon resonance biosensors based on magnetic core/shell Fe(3)O(4)/SiO(2) and Fe(3)O(4)/Ag/SiO(2) nanoparticles were developed for immunoassay. With Fe(3)O(4) and Fe(3)O(4)/Ag nanoparticles being used as seeding materials, Fe(3)O(4)/SiO(2) and Fe(3)O(4)/Ag/SiO(2) nanoparticles were formed by hydrolysis of tetraethyl orthosilicate. The aldehyde group functionalized magnetic nanoparticles provide organic functionality for bioconjugation. The products were characterized by scanning electronic microscopy (SEM), transmission electronic microscopy (TEM), FTIR and UV-vis absorption spectrometry. The magnetic nanoparticles possess the unique superparamagnetism property, exceptional optical properties and good compatibilities, and could be used as immobilization matrix for goat anti-rabbit IgG. The magnetic nanoparticles can be easily immobilized on the surface of SPR biosensor chip by a magnetic pillar. The effects of Fe(3)O(4)/SiO(2) and Fe(3)O(4)/Ag/SiO(2) nanoparticles on the sensitivity of SPR biosensors were also investigated. As a result, the SPR biosensors based on Fe(3)O(4)/SiO(2) nanoparticles and Fe(3)O(4)/Ag/SiO(2) nanoparticles exhibit a response for rabbit IgG in the concentration range of 1.25-20.00 μg ml(-1) and 0.30-20.00 μg ml(-1), respectively.     

Alkyl-terminated crystalline Ge nanoparticles prepared from NaGe: Synthesis, functionalization and optical properties

High purity NaGe was directly prepared by a low-temperature reaction of NaH and Ge. The product was characterized by powder X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray (EDX) spectroscopy. This material is a useful starting reagent for the preparation of Ge nanoparticles. Hydrogen-terminated germanium (Ge) nanoparticles were prepared by reaction of NaGe with NH₄Br. These Ge nanoparticles could be prepared as amorphous or crystalline nanoparticles in quantitative yields and with a narrow size distribution. The nanoparticles were functionalized via thermally initiated hydrogermylation with 1-eicosyne, CH₃(CH₂)₁₇C≡CH to produce alkyl-terminated Ge nanoparticles. The modified Ge nanoparticles were characterized by powder XRD, transmission electron microscopy (TEM), Fourier transform infrared (FT-IR) and Raman spectroscopy, and photoluminescence (PL) spectroscopy. The alkyl-functionalized Ge nanoparticles can be expected to have promising applications in many technological and biological areas.