3,3′,5,5′-四甲基联苯胺与钼磷酸纳米晶分子杂化材料的合成与表征(英文)

以3,3′,5,5′-四甲基联苯胺(TMB)与Keggin结构钼磷酸H3PMo12O40杂化,合成得到新型分子杂化材料,经元素分析及IRI、CP、XRD等手段表征,确定其分子结构为(TMB)3PMo12O40,TEM显示该分子杂化材料颗粒直径在40nm~60nm,分布均匀,属球形颗粒纳米晶,UV-vis和ESR谱证明(TMB)3PMo12O40分子杂化材料为电荷转移型超分子化合物,并具有显著的光敏性和电催化活性。     

空心结构(C12H8N2)3·H3PMo12O40/WO3的制备及光催化研究

制备了杂多化合物(C12H8N2)3.H3PMo12O40和空心结构复合催化剂(C12H8N2)3.H3PMo12O40/WO3,采用等离子体原子发射光谱(ICP-AES)、元素分析(EA)、热重-差热分析(TG-DTA)、X射线衍射(XRD)、傅里叶变换红外光谱(FTIR)、扫描电镜(SEM)、能量色散X射线谱(EDS)、紫外-可见漫反射吸收光谱(UV-vis DRS)进行了表征。在高压汞灯照射下,研究了杂多化合物(C12H8N2)3.H3PMo12O40、空心WO3微球和空心复合催化剂(C12-H8N2)3.H3PMo12O40/WO3对罗丹明B水溶液的光催化降解活性,结果表明,在复合催化剂中,杂多化合物(C12-H8N2)3.H3PMo12O40和WO3具有协同作用,光催化活性比单独的杂多化合物和WO3都高。     

新型氨基化磁性树状分子纳米颗粒的制备与表征

采用化学共沉淀法,以FeC13.6H2O和FeSO4·7H2O为原料制备磁性Fe3O4纳米颗粒,采用3-氨丙基三乙氧基硅烷(APTES)、丙烯酸丁酯(BA)和无水乙二胺(EDA)对其进行修饰,制备了三代表面氨基化的磁性Fe3O4树状分子纳米颗粒,并对其进行结构表征与性能测试.结果表明:树状分子逐代修饰在磁性颗粒表面,氨基含量逐代增加,分别为0.41、0.69和0.87mmol/g; Fe3O4纳米颗粒平均尺寸在12nm左右,修饰后的三代磁性纳米颗粒的粒径逐代增加,分别为14、27和40nm左右;三代产品仍具备较高的饱和磁化强度,展现出了典型的超顺磁性.这种氨基功能化的磁性纳米粒子在细胞分选、固定化酶和靶向药物等诸多领域有着巨大应用潜力.     

{H3[PMo12O40]/Pt/PAMAM}复合膜的制备及对甲醇的电催化氧化

采用循环伏安法在玻碳电极上制备了{H3[PMo12O40]/Pt/PAMAM}复合膜,用X射线光电子能谱(XPS)、扫描电子显微镜(SEM)、电子能谱技术(EDS)、原子力显微镜(AFM)和循环伏安法(CV)研究了膜的组成、形貌及其对甲醇的电催化氧化活性。结果表明,Pt纳米粒子在PAMAM基底上分散均匀;最外层沉积H3[PMo12O40]后,与相同条件下制备的Pt/PAMAM膜相比,{H3[PMo12O40]/Pt/PAMAM}复合膜修饰电极对甲醇的氧化有更强的电催化活性。     

3,3’,5,5’-四甲基联苯-4,4’-二羟乙基醚的合成与表征

以3,3’,5,5’-四甲基联苯二酚(TMBP)和2-氯乙醇为原料两步法合成了3,3’,5,5’-四甲基联苯-4,4’-二羟乙基醚。探讨了反应物物质的量比、碱用量、催化剂及反应温度对转化率的影响。结果表明,在n(TMBP)∶n(NaOH)∶n(2-氯乙醇)=1∶3.0∶2.5,反应时间为10h,反应温度为110℃条件下,总转化率达95.9%,纯度达99.1%。并用红外、质谱以及核磁等方法对产物结构进行了表征。     

负载银簇的硅基杂化纳米颗粒制备及其SERS性能

本研究发展了一种简便的"原位还原"策略构建负载银簇的硅基杂化纳米颗粒(Ag@SHNPs)。首先利用两亲性嵌段共聚物PS₈₉-b-PAA₁₆自组装行为和3-巯基丙基三甲氧基硅烷(MPTMS)在亲水链段PAA区域的水解缩聚反应形成有机硅胶束杂化纳米结构,再利用有机硅骨架中丰富的巯基作为还原位点,原位将银盐转化为银簇,最终得到负载银簇的硅基杂化纳米颗粒,并对该杂化纳米颗粒的形貌、结构以及成分组成作了分析。通过测试材料对不同细胞系的毒性验证了其良好的生物相容性。最后以4-巯基苯甲酸(4-MBA)为探针分子,对硅基杂化颗粒基底的表面增强拉曼散射(SERS)活性进行检测。在532 nm波长的激光激发下, 4-MBA标记的硅基杂化纳米颗粒展示出明显的拉曼信号增强特性,增强因子约为10⁵。因此,该硅基杂化基底材料在SERS生物成像和高灵敏检测方面具有潜在的应用前景。     

二茂铁衍生物-钼磷酸杂化材料的合成与性质

本文采用固相反应法合成一种新型有机-无机杂化材料,乙酰二茂铁-多金属氧酸盐混合价化合物[Fe(C5H5)2COCH3]3HPMo12O40·C2H6O,用元素分析、ICP、AAS、IR、XRD、UV、TG、ESR等进行表征,确定了该化合物的组成和结构,测定其磁性和导电性.结果表明,反应过程中,乙酰二茂铁与杂多阴离子之间发生了电荷转移,杂多阴离子部分还原,生成了混合价化合物的杂化材料; 铁磁性质及导电性质测定结果表明,该材料为弱铁磁体和弱的半导体材料.     

新型多金属氧酸盐化合物的制备及其降解有机染料研究

以[Ru(2,2′-bipy)3]Cl2和H3PMo12O40为反应物,采用化学共沉淀法,制备出一种新型的配合物-多酸化合物[Ru(2,2′-bipy)3]3(PMo12O40)2。IR、TG、BET等测试结果表明,该化合物结合了有机、无机两者的优良性质,热稳定性较好,比表面积较大,达到69.675m2/g。在室温、自然光照下,100mg样品可在30min内使罗丹明B(RhB)溶液完全脱色,催化降解效率超过99%,说明该化合物具有较高的降解有机染料能力。     

壳层厚度对核-壳结构PS-SiO_2杂化颗粒压缩弹性模量的影响

基于正负电荷间的静电作用制备了具有核-壳结构的聚苯乙烯-氧化硅(PS-SiO2)杂化颗粒,通过调节正硅酸乙酯的用量对样品的SiO2壳层厚度进行控制。利用原子力显微镜(AFM)在微观尺度上测定杂化颗粒的力-位移曲线,根据Hertz接触模型和Sneddon接触模型,考查了SiO2壳层厚度对样品压缩弹性模量的影响。扫描电子显微镜(SEM)和透射电镜(TEM)结果显示,杂化颗粒中PS内核尺寸为(197±9)nm,壳层由SiO2纳米颗粒组成,在本试验范围内杂化颗粒样品的壳厚为11~16nm。在Hertz接触模型条件下,PS微球的弹性模量为(2.2±0.5)GPa,其数值略低于PS块体材料。当SiO2壳厚由11nm增至16nm时,杂化颗粒的弹性模量从(4.4±0.6)GPa增至(10.2±1.1)GPa,其数值明显低于纯SiO2,且更接近于PS内核。     

PMTES/Fe_(2)O_(3)有机-无机杂化材料的研究EI

以甲基三乙氧基硅烷 (MTES)、氯化铁为原料 ,采用溶胶 -凝胶工艺 ,制备聚甲基三乙氧基硅烷 /三氧化二铁(PMTES/Fe2 O3)有机 -元机杂化材料。研究溶胶 -凝胶体系的电化学性能 ,探索 MTES与 Fe2 O3杂化机理 ,并对该材料进行 IR、SEM、TG、DTA、XRD测试 ,结果表明 ,PMTES/Fe2 O3 杂化材料耐温性能优良 。     

Preparation and electrochemical and electrocatalytic properties of nanocomposite multilayer film based on a Keggin-type phosphomolybdate

An electrostatically self-assembled multilayer film has successfully been prepared on quartz or indium-tin-oxide substrates by alternating adsorption of a Keggin-type phosphomolybdate H3PMo12O40 (PMo12) and 1,10-diaminodecane (1,10-DAD). The formation of (PMo12/1,10-DAD), film was investigated by ultraviolet (UV) spectroscopy. The UV spectra showed that the deposition of the films was uniform and reproducible. The cyclic voltammetry on the PMo12-based multilayer film indicated that the PMo12 anions in the film undergo rapid four 2e(-)/2H+ redox processes, and electrocatalytically active towards the reduction of bromate.     

Preparation and photocatalytic activity of an electrostatically self-assembled film made of [PMo12O40](3-) and a bipolar hemicyanine cation

An electrostatically self-assembled film of PMo12/H6 has successfully been prepared on quartz substrates by alternating adsorption of [PMo12O40(3-) (PMo12) and a bipolar hemicyanine derivative of (E)-1,1'-(hexane-1,6-diyl)bis(4-(4-(dimethylamino)styryl)pyridinium) bromide (H6Br2). The UV-visible spectra showed that the film was uniformly deposited and the charge transfer between two film-forming components might occur in the film. The photocatalytic performance of the film was studied for the degradation of aqueous dye Methyl Red (MR) under UV irradiation. The degradation of MR follows Langmuir-Hinshelwood first-order kinetics.     

Optimization and comparative analysis of Cs ion intercalated H3PMO12O40 photocathode: one-step hydrothermal strategy

Journal of Materials Science: Materials in Electronics - The current study focused on fabrication of phosphomolybdic acid (H3PMo12O40) (PMA) and cesium intercalated phosphomolybdic acid...     

Interfacially synthesized PAni-PMo12 hybrid material for supercapacitor applications

The concept of interfacial polymerization is utilized for the synthesis of polyaniline-phosphomolybdate (PAni-PMo12) molecular hybrids and it is well characterized. The electrical conductivity of the synthesized hybrid materials increases with increase in PMo12 wt%. The synthesized hybrid materials are evaluated as the active electrode materials for supercapacitor application. Cyclic voltammetric studies of the hybrid-modified electrode shows broad parallelogram-shaped peak as an evidence for pseudo-capacitive behaviour. The galvanostatic charge-discharge studies enlighten that interfacially synthesized hybrid materials loaded with PMo12 show relatively enhanced specific capacitance values than PMo12 free samples.     

水热法制备BaO-Nd_2O_3-TiO_2系纳米粉体

采用水热法制备了BaO-Nd2O3-TiO2(BNT)系纳米粉体。在KOH碱性溶液中,以TiCl4,BaCl2和Nd(NO3)3为反应物,先制备出BaO-Nd2O3-TiO2(BNT)凝胶前驱体,再经低温水热处理,得到BNT系纳米粉体。产物通过XRD、IR、TEM等手段进行测试分析,结果表明:该法获得的BNT系纳米粉体为立方相结构,稀土元素掺杂均匀,产物粒径小,分散度高。讨论了BNT系纳米粉体的形成机理,发现凝胶前驱体的存在有利于BNT系纳米粉体的成功制备。     

负载磷钼杂多酸/La0.7Ca0.3Fe0.25Co0.75O3/聚吡咯的制备及光催化性能研究

采用甘氨酸-硝酸盐燃烧法成功制备了La0.7Ca0.3Fe0.25Co0.75O3钙钛矿型复合氧化物,以(NH4)2S2O8为氧化剂,运用化学氧化法合成La0.7Ca0.3Fe0.25Co0.75O3/聚吡咯薄膜,然后通过静电自组装方法制备了一种新的表面负载修饰型复合光催化剂La0.7Ca0.3Fe0.25Co0.75O3/PPy/PMO12。采用XRD、SEM、FT-IR对催化剂的物化结构进行了表征。光催化性能测试是以亚甲基蓝染料的水溶液为降解目标,结果表明,PMo12的负载修饰改进了La0.7Ca0.3-Fe0.25Co0.75O3/PPy光催化剂的催化活性。     

Surfactant-assisted synthesis of Keggin-type polyoxometalates nanorods

It was demonstrated that Keggin-type polyoxometalates nanorods (POMs-nanorods) were prepared from a solution containing a surfactant polyethylene glycol (PEG), when heteropolyanions [X(n+)M12O40](-(8-n)) (X(n+) = P5+ and Si4+; M = W and Mo) were precipitated by ammonia ion obtained by hydrolysis of urea at 373 K. In this method, PEG was used as a template and ammonia ion (NH4+) was a counterion. In an oil bath kept at 373 K without stirring, three kinds of ammonium salts of POMs, i.e., (NH4)3PW12O40, (NH4)4SiW12O40, and (NH4)3PMo12O40 nanorods were obtained. The POMs-nanorods were characterized by transmission electron microscopy (TEM), selected area electron diffraction (SAED), infrared spectra (IR), inductively coupled plasma atomic emission spectrometry (ICP-AES) and X-ray powder diffraction (XRD). TEM showed that nanorods were 0.5-1.5 microm in length, and 50-150 nm in diameter. The results of IR, ICP-AES and XRD proved the existence of Keggin structure. The formation process of POMs-nanorods, (NH4)(8-n) [X(n+)M12O40](-(8-n)) (X(n+) = P5+ and Si4+; M = W and Mo) in a H2O/PEG system was discussed.     

Hydrogen peroxide and oxygen-hydrogen oxidation of aromatic compounds in catalytic systems containing heteropoly compounds

Hydrogen peroxide and Pt activated mixture of gaseous O(2) and H(2) have been applied to oxidation of aromatic compounds in the presence of redox active heteropoly compounds in the form of acid H(4)PMo(11)VO(40) and tetrabuthylammonium (TBA) salts TBA(4)PMo(11)VO(40) and TBA(4)HPW(11)Fe(OH)O(39). Benzene, toluene and phenol were subjected to hydroxylation of the ring, which was accompanied by secondary oxidation in the reaction with hydrogen peroxide. Oxygenation of toluene was equally directed to the ring and to methyl group. The total reactivity of substrates was increased in the order of benzene相似文献