微波辅助4-十二烷氧基苄胺保护的憎水性纳米金原位还原合成

利用新型表面活性剂4-十二烷氧基苄胺(C₁₂OBA)构成的C₁₂OBA/正庚烷/正丁醇/HAuCl₄/NaOH(aq.) W/O型微乳液作为微反应器, 通过微波辐射加热的正丁醇原位还原法制备了C₁₂OBA包裹的憎水性金纳米粒子, 并通过紫外可见光谱(UV-vis)、透射电镜(TEM)、X射线衍射(XRD)、红外光谱(FT-IR)和接触角(CA)等分别进行了表征和分析. 结果显示, C₁₂OBA既可参与形成稳定的W/O型微乳液, 又可作为金粒子的良好保护剂. 微乳液内核中碱度的增加能增强位于膜相的正丁醇分子的还原能力. 在固定氯金酸用量时, C₁₂OBA/金的物质的量比增加有利于获得小尺寸、高单分散性的憎水性纳米金颗粒, 而体系的极性增加则导致金粒子的尺寸增大、单分散性下降. 通过本实验方法可方便快速地合成尺寸约为5 nm的具有高度单分散的憎水性金纳米粒子.     

4-(4-甲基苯氧基)苄胺的合成

甲基苯氧基苄胺;农药;4-(4-甲基苯氧基)苄胺的合成     

新型双链表面活性剂DDOBA的合成与高单分散性憎水纳米金的制备

自行设计合成了新颖的苄胺型双链表面活性剂3,4-双十二烷氧基苄胺(DDOBA). 利用DDOBA/正丁醇/正庚烷/甲酸/HAuCl₄·4H₂O自发形成的水/油(W/O)型微乳液作为微反应器, 通过微波辐射下的甲酸还原法成功制备了DDOBA保护的憎水性金纳米粒子, 并通过紫外-可见(UV-Vis)光谱、透射电镜(TEM)、高分辨透射电镜(HR-TEM)和X射线衍射(XRD)等方法进行了表征和分析. 结果显示, DDOBA既可参与形成稳定的W/O型(油包水型)微乳液, 又可作为金纳米粒子的良好保护剂. 在合适的微乳液体系组成范围内, 用本实验方法可以获得高单分散性的憎水性金纳米粒子, 并能在空气/水界面上自动形成大面积短程有序的纳米金二维自组装膜.     

反相微乳液化学剪裁制备明胶-γ-Fe2O3纳米复合微粒

复合纳米微粒;反相微乳液化学剪裁制备明胶-γ-Fe2O3纳米复合微粒     

4-烷氧基苯甲醛-4-氨基安替比林希夫碱的合成及抑菌活性

报道了4-氨基安替比林与4-烷氧基苯甲醛缩合反应生成希夫碱的合成和抑菌活性,分子结构由1HNMR、IR和元素分析表征;抑菌活性测定结果表明,化合物(5a,5d,5e,5f,5g)对金黄色葡萄球菌、大肠杆菌、枯草杆菌、黑霉菌、青霉菌(抑菌环直径15.3 ～ 21.70 mm)均有较好的抑菌活性,其中化合物(5f)对黑霉菌(抑菌环直径26.20 mm)有优良的抑菌活性.     

金纳米粒子的微波法合成及在蛋白质检测中的应用

通过对微波反应器中氯金酸和柠檬酸钠混合物进行直接加热,快速、一步合成了金纳米粒子.通过调节反应初始混合物中氯金酸与柠檬酸钠的比例,可获得不同粒径窄分散的金纳米粒子.进一步将所合成的金纳米粒子功能化,考察了其在蛋白质检测中的应用.     

金纳米微粒共振光散射光谱探针测定维生素B4-水溶性腺嘌呤的研究

建立了一种以金纳米微粒为探针共振光散射(RLS)法测定维生素B4的新方法.在弱酸性介质中(pH 4.2),金纳米微粒在635 nm有一最大共振散射峰.加入微量维生素B4后,金纳米微粒与维生素B4通过静电引力结合.形成了粒径较大的聚集体,导致RLS强度显著增强.研究了体系的共振光散射光谱特征和反应适宜条件,探讨了共振光散射增强的机理.结果表明,维生素B4质量浓度在0.1～5.0μg/mL 时与散射强度(△I)呈线性关系,检出限(3σ)为12.0 ng/mL,相对标准偏差(RSD)为2.2%.该方法已用于片剂中维生素B4的测定.     

镧-镍复合氧化物纳米微粒的固相合成及其催化性能

The La-Ni complex oxide catalyst was prepared by solid state reactions under microwave. The structure and reducibility of the catalyst were characterized by using TG-DTA, XRD, TEM and TPR methods. At the same time the catalytic activity of oxidative dehydrogenation of ethylbenzene to styrene with carbon dioxide over the complex oxide nanoparticle was investigated.The Results show that the product is K2NiF4 nanoparticles,and the size is 13nm.The complex oxide sample had high activity for the oxidative dehydrogenation of ethylbenzene to styrene.     

金纳米粒子的合成、特性及其在生物医学检测中的应用研究进展

近年来,纳米技术越来越广泛的应用到各个领域,金纳米粒子因其具有许多优良的物理、化学及生物学性质而引起了人们特别的关注。本文综述了金纳米粒子几种经典的合成方法,以及基于金纳米粒子独特的理化性质在病原体、核酸蛋白质检测方面的最新研究进展。     

ZnWO4纳米微粒高效催化合成5-苯基-1H-四氮唑

约10 nm大小的ZnWO4纳米微粒通过简单的溶剂热方法成功合成出来,将其应用于催化苯甲腈[3+2]环加成合成5-苯基-1H-四氮唑的反应。结果表明,0.2 mmol的ZnWO4纳米微粒110℃催化反应10 h,合成产物的产率达到81%;非晶态、纳米棒ZnWO4作为催化剂的产率分别为43%和65%。显然,催化剂用量少,反应时间短,反应条件温和,催化效率高。这或许归因于ZnWO4纳米微粒的小尺寸和高分散性,导致其比表面积大,活性位点多。ZnWO4纳米微粒表面的不饱和W原子与腈基作用,活化了腈基从而加速了反应的进行。     

反相微乳液中憎水性纳米金的原位还原法合成

利用十八胺(C18NH2)/正丁醇/正庚烷/HAuCl4(aq)W/O型微乳液体系,在常温的碱促进条件下由正丁醇原位还原氯金酸合成了具有高度单分散的憎水性金纳米粒子。由C18NH2稳定的金纳米颗粒运用紫外可见光谱(UV-vis)、透射电镜(TEM)和X射线衍射(XRD)等分别进行了表征和分析,并探讨了微乳液体系各组分对形成金纳米粒子形貌、尺寸和单分散性的影响。结果显示,随十八胺/氯金酸摩尔比的增加,金粒子的尺寸逐渐减小而单分散性逐渐提高。在正丁醇原位慢还原氯金酸的过程中,实验所选W/O型微乳液模板和表面活性剂十八胺分子对憎水性金纳米粒子的形貌和尺寸仍具有良好的控制作用。     

憎水性金纳米粒子的制备、表征与形貌控制

在十六烷基三甲基溴化铵(CTAB)或十八胺(C18NH2)/正庚烷/乙醇/HAuCl4.4H2O W/O型微乳液体系中,利用简单的加热手段通过乙醇还原法制备了具有不同形貌和尺寸的憎水性金纳米材料。由CTAB或C18NH2稳定的金纳米颗粒运用紫外可见光谱(UV-vis)、透射电镜(TEM)和X射线衍射(XRD)等分别进行了表征和分析。用混合表面活性剂(CTAB/C18NH2)替代单一表面活性剂(CTAB)可以削弱CTAB对金纳米晶体生长的导向作用并提高粒子的单分散性。     

Microwave-assisted synthesis of corroles

The recently developed Gross's method for the synthesis of corroles has been modified and successfully applied to the preparation of new free base tris-aryl- and tris-pyrimidyl-corroles using solvent-free conditions and microwave irradiation. Compared to conventional heating, the microwave technique afforded an increase in corrole yields of ca. 30% and led to noticeably cleaner reaction mixtures. It is demonstrated that short reaction times and high temperatures are required to afford optimum yields.     

Biomimetic synthesis of gold nanoparticles and their aggregates using a polypeptide sequence

The polypeptide sequence MS14 (MHGKTQATSGTIQS) was used to explore a new method for biomimetic preparation of gold nanoparticles and their aggregates. Self‐congregation of gold nanoparticles into aggregates in MS14 aqueous solution and self‐assembly of gold crystallites onto the designed complex of MS14‐PET film [protonated poly(ethylene terephthalate)] proved the specific gold‐binding characteristic of the single‐copy peptide MS14 in vitro. In aqueous solution MS14 could recover Au(III) to Au(0), tested by means of TEM, EDX and XPS. Further research suggested that the pH of the solution and the concentration of Au(III) influenced the morphology and size of the gold nanoparticles formed. In addition, extra reducing agent, sodium citrate, was introduced into the HAuCl₄–MS14 system and uniformly dispersed nanoparticles under neutral condition were obtained. Finally, we discuss the possible mechanism of this biomimetic synthesis. Copyright © 2007 John Wiley & Sons, Ltd.     

Gamma radiation induced synthesis of gold nanoparticles in aqueous polyvinyl pyrrolidone solution and its application for hydrogen peroxide estimation

Gold nanoparticles (Au nps) have been synthesized in aqueous solution of polyvinyl pyrrolidone (PVP) by gamma radiolysis from HAuCl₄·3H₂O precursor and in presence of small concentrations of Ag⁺, 2-propanol and acetone. The effect of different experimental parameters, such as concentration of reactant, molecular weight of PVP on nanoparticle formation was studied. TEM image confirmed that spherical Au nps were formed when PVP of molecular weight 360,000 Da was used as capping agent. H₂O₂ is a reactant in the enzyme catalyzed reaction of o-phenylene diamine (o-PDA). The reaction product has a weak absorption in the yellow region of the spectrum. When this product interacts with Au nps, it leads to enhancement of the absorption peak. The nanoparticles synthesized by radiation method were used for estimation of H₂O₂. The absorbance value of this peak at λ_max was observed to change with H₂O₂ concentration, which was monitored for estimation of H₂O₂. The response is linear in the range of 2.5×10⁻⁶ mol dm⁻³ to 2×10⁻⁴ mol dm⁻³ and 1×10⁻⁷ mol dm⁻³ to 3×10⁻⁶ mol dm⁻³ H₂O₂ in two separate sets of experimental parameters with detection limit 1×10⁻⁷ mol dm⁻³.     

Synthesis and shapes of gold nanoparticles by using transition metal monosubstituted heteropolyanions as photocatalysts and stabilizers

Gold nanoparticles were prepared via a simple photoreduction technique in the presence of transition metal monosubstituted Keggin heteropolyanions (PW11M, M= Cu²⁺, Ni²⁺, Zn²⁺, Fe³⁺), in which PW11M acted as reducing agent, photocatalyst and stabilizer. The results indicated that the formation rate and morphology of the nanoparticles strongly depended on the kind of transition metal substituted in heteropolyacid and the preparation conditions, such as irradiation time and propan-2-ol amount. The photoreduction rates of PW11Zn and PW11Fe were faster than those of PW11Ni and PW11Cu. The shapes of the nanoparticles synthesized in the presence of PW11Fe and PW11Zn were nearly uniform spheres, whereas the morphologies of the nanoparticles synthesized in the presence of PW11Ni and PW11Cu were found to contain a mixture of flat triangular/hexagonal structures as well as spheres. Increases in the irradiation time and the propan-2-ol amount could make the morphology of nanoparticles uniform and shorten the formation time of the nanoparticles. __________ Translated from Chinese Journal of Applied Chemistry, 2007, 24(7) (in Chinese)