纳米TiO2/介孔ZSM-5协同过硫酸盐光催化降解硝基苯酚废水

以具有介孔结构的ZSM-5沸石分子筛负载纳米TiO2制备出性能良好的复合型催化材料.结合扫描电镜(SEM)、N2吸附-脱附等温线(BET/BJH模型)和X射线衍射进行表征,并将其协同过硫酸盐光催化降解硝基苯酚废水.结果表明:在pH为4.5,催化剂投加量为0.8g/L,,FeSO4为0.8g/L,Na2S2O8为1.6g/L,常温下反应240min,对硝基苯酚(50mg/L)去除率达到98.4%.     

过硫酸盐光催化降解硝基苯酚废水纳米TiO2/介孔ZSM-5协同

以具有介孔结构的 ZSM-5沸石分子筛负载纳米 TiO 2制备出性能良好的复合型催化材料．结合扫描电镜(SEM)、N2吸附-脱附等温线(BET/BJH 模型)和 X 射线衍射进行表征,并将其协同过硫酸盐光催化降解硝基苯酚废水．结果表明：在 pH 为4．5,催化剂投加量为0．8 g/L,,FeSO 4为0．8 g/L,Na2 S2 O 8为1．6 g/L,常温下反应240 min,对硝基苯酚(50 mg/L)去除率达到98．4％．     

用乙酰胺合成六方形貌介孔氧化硅纤维

以正硅酸乙酯(TEOS)为硅前驱体,乙酰胺(CH3CONH2)为助溶剂,十六烷基氯化吡啶(C16PyC l)为结构导向剂,在酸性溶液中合成六方形貌的介孔氧化硅纤维,经小角X射线衍射(SXRD)、扫描电子显微镜(SEM)和低温N2吸附-脱附技术等表征。结果表明:合成的样品为六角状外形的氧化硅纤维,直径约4~7μm,长度约几十微米。六角状纤维的孔道具有与MCM-41类似的六方结构;煅烧后样品的吸附数据显示出吸附-脱附等温线为典型的IV型,吸附-脱附滞后环为H2型,孔道的孔径分布较宽;BJH最可几孔径为2.96 nm和3.50 nm,表明样品具有特殊的双孔道结构;计算的BET表面积为1 060 m2.g-1。     

N 掺杂介孔 TiO2 的合成

通过简单的溶胶-凝胶方法合成了N掺杂的介孔TiO2.用X-射线粉末衍射(XRD)、扫描电子显微镜(SEM)、N2吸附、X射线光电子能谱(XPS)、紫外-可见(UV-vis)漫反射吸收光谱等手段进行了表征.X-射线粉末衍射表明,焙烧前的产物为无定形TiO2,焙烧后的产物为TiO2的锐钛矿.N2吸附-脱附等温线表明,N-20的BET表面积为76 m2/g,孔尺寸大约为10 nm,X射线光电子能谱(XPS)辅助证明有N掺入了TiO2中.紫外可见漫反射光谱(UV-vis)表明,N掺杂的介孔TiO2的吸收带边位置发生红移,吸光范围向可见光区拓宽.     

铁掺杂纳米二氧化钛介孔材料的合成、结构与性能

以TiCl4、FeCl3·6H2O和NH3·H2O等为原料,以有机大分子表面活性剂(十六烷基三甲基溴化铵)为模板和结构导向剂,采用水热法制备出铁掺杂纳米TiO2介孔材料.X射线衍射分析结果表明,产品为锐钛矿结构.透射电镜观察发现样品为球形,粒径约为10～15 nm,颗粒之间显示出无序孔道.N2吸附-脱附等温线形状为Langmuir Ⅳ型,是典型的介孔结构吸附-脱附等温线,其最可几孔径为20 nm.利用该纳米TiO2介孔材料作为光催化剂对有机染料进行了吸附和降解实验,发现介孔材料比非介孔材料对染料具有更强的吸附性和降解效果,在日光照射60 min后对藏蓝染料的降解率达到了100%.     

溶胶-凝胶法制备钒掺杂中孔氧化硅及丙烷氧化脱氢的研究

采用溶胶-凝胶法制备了钒掺杂中孔氧化硅（V-meso-SiO₂）,用N₂ 物理吸附、X射线衍射、透射电镜、拉曼光谱、紫外可见漫反射、红外光谱、程序升温脱附、程序升温还原系统研究了催化剂的物化性质并测试了其在丙烷氧化脱氢反应中的催化性能。结果表明： V-meso-SiO₂催化剂具有约600m²/g的比表面、5.0nm左右的平均孔径、类似蠕虫状的介孔孔道结构;氧化钒在材料的骨架内主要是以高度分散的孤立态的四面体钒存在,是丙烷氧化脱氢反应的活性中心位;通过优化反应温度、原料气体流速等条件,V-meso-SiO₂催化剂对于丙烷氧化脱氢反应具有较好的催化活性。     

多孔单晶CeO2空壳球的制备及其CO催化氧化性能研究

以水热法成功制备了(110)面暴露的高活性多孔单晶CeO2空壳球催化剂样品,研究了其形成过程并提出了相应的形成机理.通过X射线衍射、透射电镜及低温氮气吸附/脱附等温线对催化剂结构进行了详细的表征,结果表明:该材料具有多孔结构以及较高的比表面积(259 m2/g).该多孔单晶CeO2催化剂在CO氧化转化中显示了较好的催化性能,其催化活性远高于商业化CeO2,这主要归结于其特殊的(110)高能面的暴露以及多孔单晶结构.     

氨基官能化的扩孔MCM-41复合材料吸附捕集CO_2

制备了扩孔的介孔氧化硅MCM-41,然后以其为载体,通过化学接枝法将3-[2-(2-氨基乙基氨基)乙基氨基]丙基-三甲氧基硅烷嫁接到其介孔结构中,制备了氨基官能化的介孔氧化硅复合材料.通过N2吸附脱附实验、红外光谱、热重分析等手段对氨基官能化前后扩孔MCM-41的物理化学属性进行了表征,然后考察了复合材料对CO2的吸附捕集性能.结果表明:与单纯扩孔MCM-41相比,氨基官能化的扩孔MCM-41复合材料的比表面积、总孔容及孔径均减小;同时,所制复合材料对CO2的吸附量明显增大(两者的CO2吸附量分别为28 mg/g和76 mg/g),且在循环CO2吸附脱附实验中呈现出优异的稳定性.     

干胶-水蒸汽辅助晶化法合成多级孔ZSM-5分子筛

采用干胶-水蒸汽辅助晶化法,通过优化制备条件,合成了粒径约80 nm的表面多孔纳米球形ZSM-5.考察了结构导向剂质量分数、硅源、铝源、沉淀剂种类、晶核形成时间及老化温度对纳米ZSM-5晶体形貌的影响.采用X射线衍射(XRD)、傅里叶变换红外光谱(FT-IR)、N_2物理吸附-脱附及透射电子显微镜(TEM)等表征手段对合成的分子筛进行了表征.结果表明:结构导向剂的质量分数、铝源的类型和晶核形成时间均能明显影响分子筛晶体形貌;结构导向剂质量分数的降低有助于提高ZSM-5微孔结构的长程有序性;优化合成条件可制备出具有约介孔2 nm、比表面积357.1 m~2/g、由80 nm的晶粒堆积形成的多级孔ZSM-5分子筛材料.     

氧化硅纳米颗粒的形貌和孔结构的调控及其对药物输运性能影响

以阳离子表面活性剂十六烷基三甲基溴化铵(CTAB)和两亲性嵌段共聚物聚苯乙烯-b-聚丙烯酸(PS-b-PAA)为双模板剂,以正硅酸乙酯(TEOS)为硅源,通过精确调控模板剂与硅源之间的界面自组装行为,制备了3种多级孔氧化硅纳米颗粒,包括核壳型双介孔氧化硅纳米颗粒(CS-DMSNs)、嵌入型双介孔氧化硅纳米颗粒(E-DMSNs)及空心型介孔氧化硅纳米颗粒(H-MSNs)。利用透射和扫描电镜、氮气吸附-脱附等表征方法对多级孔氧化硅纳米颗粒形貌和孔结构进行分析,探讨其作为药物输运载体时的形貌和孔结构对载药量、释放性能及细胞存活率的影响规律。     

K2FeO4石墨化生物质多孔炭的制备及其电容性能

采用K₂FeO₄浸泡和热处理相结合的方法制备了石墨化柚子皮多孔炭(GSPC). 通过扫描电子显微镜(SEM)、比表面积分析(BET)、X射线衍射(XRD)、X射线光电子能谱(XPS)和拉曼光谱(Raman)对材料的形貌和组成进行表征. 使用循环伏安法(CV)、交流阻抗法(EIS)和恒流充放电法(GCD)研究了GSPC的电容性能. 结果表明:石墨化后材料的比表面积由75.91 m2/g增大到619.78 m2/g,孔容积由0.192 cm3/g增大到0.425 cm3/g;GSPC具有出色的双电层电容性能,在1 A/g的电流密度下,比电容达254 F/g,且具有优异的倍率性能(7 A/g的电流密度下,电容保持率为74%). 此外,GSPC电极在100 mV/s下循环10 000次的比电容没有衰减,具有优异的循环稳定性. 此研究可为开发廉价的高性能生物质炭基材料提供新思路.     

Polyaniline nanostructures tuning with oxidants in interfacial polymerization system

Three kinds of nanostructured polyanilines (PANIs) were prepared through interfacial polymerization by using ammonium persulfate (APS) as a single oxidant, and APS/FeCl3, APS/K2Cr2O7 as composite oxidants, respectively. It is observed that faster formation process and higher yield of nanostructured PANIs could be achieved in the presence of FeCl3 and K2Cr2O7. The as-prepared PANIs were characterized by field emission scanning electron microscopy, ultraviolet–visible absorption spectroscopy, Fourier transform infrared and Raman spectroscopy, X-ray diffraction analysis and electrochemical measurements including cyclic voltammetry and galvanostatic charge/discharge measurement. The influence of composite oxidants on the morphology, microstructure, and electrical and electrochemical properties of PANIs was discussed. Interestingly, when APS/K2Cr2O7 was used as the composite oxidants, PANI exhibited petal-like structure with high yield of 57.35% instead of general nanofibrous morphology formed in interfacial polymerization. Compared with those nanofibrous PANIs obtained by using APS as a single oxidant or APS/FeCl3 as composite oxidants, petal-like PANIs exhibited the largest specific capacitance (692.4 F/g at scan rate of 5 mV/s) and highest cycle stability among them. It provides a new insight into the control of PANI nanostructures with high yield and energy storage ability by simply selecting suitable composite oxidants in interfacial polymerization.     

壳聚糖/聚乙烯醇/氧氟沙星共混无纺布的制备及体外释放研究

以静电纺丝法制备了具有抗菌性能的壳聚糖/聚乙烯醇/氧氟沙星共混无纺布,测定了共混无纺布的力学性能,通过红外光谱(FT-IR) 、X-射线衍射(XRD)和扫描电子显微镜(SEM)对其结构性能进行了表征,选出了载药量较大、力学性能较好(壳聚糖/聚乙烯醇质量比为7,氧氟沙星质量分数为4%)的共混无纺布,在不同pH值的缓冲溶液中对其进行了体外药物释放实验。结果表明,所得的无纺布纤维直径均匀,平均为200nm。聚乙烯醇可以改善氧氟沙星/壳聚糖/聚乙烯醇共混无纺布的力学性能;氧氟沙星在壳聚糖/聚乙烯醇共混膜中有良好的相容性;氧氟沙星在pH为7.40的缓冲溶液中达到释放平衡时需要6h。     

Synthesis of Porous Hollow Micro spheres of BiVO_4 Based on EDTA and SDBS via Hydro thermal Method

Porous hollow microspheres of bismuth vanadate(BiVO_4) were successfully synthesized with the assistances of ethylenediamine tetraacetic(EDTA) and sodium dodecylbenzene sulfonate(SDBS) via hydrothermal method.The as-prepared BiVO_4 samples were characterized by X-ray diffraction(XRD),field-emission scanning electron microscopy(FE-SEM) and UV-vis diffuse reflectance spectra(DRS).It was found that the ratio of EDTA and SDBS had a significant impact on the crystalline structure,size and morphology of BiVO_4 photocatalyst.The crystal phase could be adjusted by changing the mass ratio of EDTA and SDBS.The photocatalytic activities of different BiVO_4 samples were investigated through the degradation of RhB in the presence of H_2O_2 under visible light irradiation.The results indicated that the photocatalytic performance of the BiVO_4 microstructures was greatly influenced by the porous structure,morphology and band gap.The BiVO_4 sample prepared with the EDTA and SDBS ratio of 2:1 and total amount of 1.5 g have shown superior photocatalytic performance for its unique morphology,good porous structure and low band gap energy.     

Ag@SiO2复合纳米微粒的制备及其抗菌性能

利用简单的一步法合成Ag@SiO2复合纳米微粒,并对其样品进行了TEM,HRTEM,XRD和UV表征.结果表明银纳米粒子成功包覆于二氧化硅微球之中,且壳层呈多孔状结构.以二倍稀释法测试了Ag@SiO2纳米颗粒对金黄色葡萄球菌、绿脓杆菌和大肠杆菌的最小抑菌质量浓度以及最小杀菌质量浓度,结果表明Ag@SiO2纳米颗粒具有良好的抗菌持久性能,并且对革兰氏阴阳两种细菌具有良好的杀菌选择性.     

Porous cobalt oxide nanowires: Notable improved gas sensing performances

The porous Co3O4 nanowires have been successfully synthesized via modified template method. A possible growth mechanism governing the formation of such 1D nanowires is proposed. The as-prepared products have been characterized by X-ray Powder Diffraction (XRD), Extended X-ray Absorption Fine-structure (EXAFS), High-resolution Transmission Electron Microscopy (HRTEM) and N2 adsorption/desorption analysis. Our systematic studies have revealed that the porous Co3O4 nanowires show excellent gas sensing performances, which demonstrate the potential application of the 1D nanostructured Co3O4 in the detection of the ethanol gas as a sensor material. The improved performances are owing to its large specific surface area and porous morphology.     

硅源加入方式对Fe3O4/SiO2核壳结构制备的影响及磁性能研究

表面包覆惰性层是解决四氧化三铁(Fe3O4)粒子团聚、易氧化、亲水性差等问题的一种有效方法,但惰性层的引入一般会导致包覆后样品磁性能下降,从而限制了Fe3O4的应用.以正硅酸乙酯(TEOS)和氨水为原料,制备了具有良好磁响应性的Fe3O4/SiO2核壳结构.样品的结构、形貌、尺寸和表面吸附官能团采用X-ray粉末衍射(XRD)、扫描电镜(SEM)、透射电镜(TEM)和红外光谱(FTIR)等测试手段进行了表征.研究发现,TEOS加入方式影响SiO2层生长过程,从而影响包覆的均匀程度.Fe3O4/SiO2核壳结构表现出顺磁性和良好的磁响应性(52emu/g).     

二氧化硅气凝胶的常压制备及其特性研究

以正硅酸乙酯为原料,先采用溶胶-凝胶法制备湿凝胶,然后浸泡在反应溶液中进行老化,再利用正己烷进行溶剂交换,三甲基氯硅烷进行表面改性,最终获得轻质多孔二氧化硅气凝胶. 进一步考察了凝胶时间随乙醇和水的不同加入量和pH值的变化,利用FTIR、XRD和SEM等方法对二氧化硅气凝胶表征. 结果表明,所制备的疏水SiO2气凝胶的密度、比表面积和孔隙率分别为77～200 kg·m-3,500～750 m2g-1和85%～95%,其颗粒尺寸为50～200 nm.     

Incorporation of Sphingosine 1-Phosphate Loaded Mesoporous Silica Nanoparticles into Poly( L-lactic acid ) Nanofibrous Scaffolds for Bone Tissue Engineering

Controlled release of the functional factors is the key to improve clinical therapeutic efficacy during the tissue repair and regeneration.The three-dimensional(3D)scaffold can provide not only physical properties such as high strength and porosity but also an optimal environment to enhance tissue regeneration.Sphingosine1-phosphate(S1P),an angiogenic factor,was loaded into mesoporous silica nanoparticles(MSNs)and then incorporated into poly(L-lactic acid)(PLLA)nanofibrous scaffold,which was fabricated by thermally induced phase separation(TIPS)method.The prepared scaffolds were examined by attenuated total reflection Fourier transform infrared spectroscopy(ATR-FTIR),scanning electron microscopy(SEM),and transmission electron microscopy(TEM)and compressive mechanical test.The ATR-FTIR result demonstrated the existence of MSNs in the PLLA nanofibrous scaffold.The SEM images showed that PLLA scaffold had regular pore channel,interconnected pores and nanofibrous structure.The addition of MSNs at appropriate content had no visible effect on the structure of scaffold.The compressive modulus of scaffold containing MSNs was higher than that of the scaffold without MSNs.Furthermore,fluorescein isothiocyanate(FITC)was used as model molecule to investigate the release behavior of S1P from MSNsincorporated PLLA(MSNs/PLLA)nanofibrous scaffold.The result showed that the composite scaffold largely reduced the initial burst release and exhibited prolonged release of FITC than MSNs.Thus,these results indicated that S1P-loaded composite nanofibrous scaffold has potential applications for bone tissue engineering.     

Mg-Nd-Zn-Zr镁合金表面超疏水SiO2薄膜的制备及其表征

以微弧氧化层(MAO)为预处理过渡层,正硅酸乙酯(TEOS)和甲基三乙氧基硅烷(MTES)为主要原料,采用sol-gel和浸渍-提拉相结合的方法在Mg-Nd-Zn-Zr(NZ30K)镁合金表面获得甲基(-CH3)疏水基团表面修饰的超疏水SiO2薄膜,实现了NZ30K镁合金表面的超疏水改性.同时研究了微弧氧化层的表面特征、sol-gel过程中TEOS/乙醇摩尔比(TEOS/EtOH)和MTES添加量(MTES/TEOS摩尔比)对所制备超疏水SiO2薄膜表面形貌和润湿特性的影响.结果表明:NZ30K镁合金经过微弧氧化处理后,表面呈现的微米-纳米尺度上多孔的粗糙结构,其表面体现为亲水性,但有利于提高超疏水SiO2薄膜与NZ30K基材的结合力;当TEOS/EtOH摩尔比为1/30,MTES/TEOS摩尔比为1/2时,SiO2薄膜表面的静态接触角达到151°,其表面具有超疏水特性;而进一步提高MTES/TEOS摩尔比至1时,其静态接触角有所提高,达到153°.红外光谱(FT-IR)表明NZ30K镁合金表面SiO2薄膜的超疏水特性是由于MTES的引入使得-CH3疏水官能团能够成功地嫁接到SiO2粒子的表面.