双模板法制备介孔二氧化硅纳米蚕茧

用十八烷基三甲基溴化铵(STAB)作模板剂,左旋香茅醇(CN)为结构助剂,利用溶胶-凝胶法,在CN/STAB摩尔比1∶1条件下制备了介孔二氧化硅纳米蚕茧;采用扫描电镜和透射电镜分析了产物的结构,并对其进行了氮气吸附-脱附测试.结果表明,所制备的介孔二氧化硅纳米蚕茧的孔道与蚕茧表面平行;搅拌速度对介孔二氧化硅纳米蚕茧的长度有较大的影响,随着搅拌速度的增加,其长度减小.     

纳米银负载的炭气凝胶制备及抗菌性能研究

以常压干燥法制备的酚醛有机气凝胶为原料,通过在硝酸银溶液中浸渍使银吸附或沉积在有机气凝胶上,在常压条件下干燥并炭化制得纳米银负载的炭气凝胶。利用扫描电镜(SEM)、透射电镜(TEM)、X-射线衍射(XRD),比表面积及孔径分析等方法研究了浸渍前后凝胶密度和结构的变化,以及制备条件对银负载炭气凝胶的载银量和凝胶结构的影响;研究了载银炭气凝胶对大肠埃氏杆菌(ATCC25922)和金黄色葡萄球菌(ATCC25923)的抗菌效果。结果表明,这类银负载炭气凝胶对大肠杆菌和金黄色葡萄球菌均有很强的杀灭能力,预期炭气凝胶在作为催化剂或吸附杀菌材料方面有良好的应用前景。     

SBA-15负载CeO2纳米晶的溶胶-凝胶一步合成

以P123为模板剂, 正硅酸乙酯和硝酸铈为前驱体, 通过溶胶-凝胶路线在酸性条件下合成了SBA-15负载氧化铈(CeO2与SiO2质量比为28.7%)有序介孔材料. 采用热重/差热分析(TGA/DTA)、X射线衍射(XRD)、透射电镜(TEM)和氮气吸附等手段对所合成材料进行了表征. 结果表明, 合成的材料具有类似于SBA-15的结构, 孔径、孔容和比表面积分别为38.7 Å, 0.46 cm3/g和570 m2/g. X射线衍射(XRD)、透射电镜(TEM)、X射线能谱(EDS)和选区电子衍射花样联合表征证实了铈物种以高分散的CeO2纳米晶的形式分布在介孔基体中.     

Na~+浓度对反应体系成胶特性及SiO_2凝胶粉末性能的影响

以水玻璃为原料，乙酸乙酯为潜伏酸试剂，采用溶胶—凝胶法制备超细二氧化硅凝胶粉末。研究了成胶反应过程中Ｎａ＋ 浓度对反应体系成胶特性及最终所得二氧化硅凝胶粉末性能的影响，并用透射电镜和氮气物理吸附实验手段对粉末的有关性能进行了测试表征     

陈化温度和pH值对氨基功能化介孔氧化硅吸附CO_2性能的影响

本研究采用溶胶-凝胶法,分别以十二烷基肌氨酸钠、氨丙基三甲氧基硅烷(APTMS)和正硅酸乙酯(TEOS)为结构导向剂(SDA)、共结构导向剂(CSDA)和硅源合成了氨基功能化的介孔氧化硅预产物。利用乙醇和乙醇胺混合液对预产物进行萃取后获得氨基功能化介孔氧化硅。利用红外光谱、元素分析、N2吸-脱附、透射电镜等手段对材料进行了表征。红外光谱结果证明通过萃取方法可较好地去除表面活性剂;N2吸附结果表明所有样品都具有介孔结构;元素分析和透射电镜结果说明反应陈化温度、pH值等合成条件对材料孔道内表面的氨基含量和材料结构有较大的影响。CO2吸附实验证明在低陈化温度、相对较低的pH值下合成的材料具有较高的CO2吸附量。     

两种新型多孔金属-有机凝胶的合成、表征与气体吸附性能

以1,4-二(3-乙酰丙酮基)苯(DAB)为有机配体分别与铝离子和铬离子反应,合成出2个新型的金属-有机凝胶:Al-湿凝胶和Cr-湿凝胶,通过直接干燥法得到相应的2种多孔干凝胶:Al-干凝胶和Cr-干凝胶.通过X射线粉末衍射仪(PXRD)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)、傅里叶变换红外光谱仪(FTIR)、热重分析仪(TGA)、X射线能谱仪(EDS)和氮气吸附-脱附仪对凝胶材料的结构和形貌进行了表征.结果显示,2种多孔金属有机凝胶材料是由球状纳米粒子堆积而成,具有较高的比表面积、丰富的微孔及少量的介孔结构.气体吸附性能测试结果表明,Al-干凝胶的比表面积为790.3 m2/g,在1.01×105Pa,77 K下能够吸附117.45 cm3/g的氢气,在273 K下能够吸附60.74 cm3/g的二氧化碳.     

具有MIL-100和MIL-101结构巨孔羧酸钪配位聚合物

用溶剂热方法首次以DMF为溶剂合成了具有MIL-100和MIL-101结构的巨孔均苯三甲酸钪(1)和对苯二甲酸钪(2)配位聚合物,通过将钯金属纳米粒子沉积到均三苯甲酸钪(1)的骨架结构中的方法,获得了后功能化的载有钯纳米粒子的配位聚合物孔材料Pd@1,并对以上材料进行了X-射线粉末衍射、扫描电镜、透射电镜和氮气吸附表征。     

三维生物高分子/氧化石墨烯复合凝胶对阳离子染料吸附的研究

采用一种简便的方法制备了生物高分子调控的氧化石墨烯凝胶用于水污染处理.将生物高分子白蛋白(BSA)、壳聚糖(CS)、及脱氧核糖核酸(DNA)与氧化石墨烯(GO)共混,自组装形成水凝胶,最后冻干得到生物高分子/氧化石墨烯复合凝胶.通过扫描电镜、原子力显微镜、纳米粒度分析仪等分析复合凝胶的组装结构与表面电位.结果表明凝胶呈现内部联通的三维多孔结构,该结构有利于被吸附分子的快速内部扩散.红外光谱证明了生物高分子被成功负载到了凝胶网络中.然后将该复合凝胶用于阳离子染料的吸附,吸附实验表明这类生物高分子/氧化石墨烯复合凝胶对阳离子染料有很好的吸附效果,同时也对阴离子和非离子毒性分子有一定的吸附能力.研究了吸附时间,初始浓度,pH值等对凝胶吸附量的影响,并考察了凝胶的解吸附.最后详细探讨了GO-BSA、GO-CS和GO-DNA凝胶对亚甲基蓝(MB)吸附的动力学和吸附等温式.经吸附动力学拟合,生物高分子/氧化石墨烯复合凝胶吸附MB复合二级动力学模型和Langmuir等温吸附,对MB分子是单分子层吸附,吸附初期为大孔隙扩散,后期为粒子内扩散.     

高钒掺杂量MCM-41合成及表征

采用溶胶-凝胶法,在氨性条件下合成出高钒掺杂量介孔MCM-41。以XRD,氮气吸附/脱附,透射电镜,ICP和拉曼光谱等技术对材料的结构进行了表征。结果表明当钒硅物质的量的比达到0.14时材料仍保持规整介孔结构(尽管当钒/硅物质的量的比超过0.11时开始有V₂O₅晶体出现)。所合成材料室温下在苯的过氧化氢直接羟基化反应中表现出良好的催化性能。     

疏水二氧化硅气凝胶对甲苯蒸气吸附性能研究

吸附法是控制挥发性有机物(VOCs)的重要方法,对吸附材料的研究有着重要的意义。为了开发出吸附量高、稳定性好的吸附材料,利用溶胶-凝胶法制备出疏水二氧化硅气凝胶,并对其进行了低温氮气吸附、傅里叶变换红外光谱和热重分析,同时对疏水二氧化硅气凝胶进行了甲苯蒸气的静态、动态和循环吸附实验,研究其对甲苯蒸气的吸附性能。结果表明,所制疏水二氧化硅气凝胶为比表面积达732m~2/g的介孔吸附材料,其表面具有疏水性甲基基团,吸附容量高达1.6g/g,吸附稳定性强,动态吸附温升最高达12℃,用Logistic模型拟合吸附穿透曲线相似度高。     

One-Pot Synthesis of Novel Amino-Functionalized Fe<Subscript>3</Subscript>O<Subscript>4</Subscript> Hybrid Microspheres for Cu(II) Removal from Aqueous Solutions

In this work, we report the development of novel amino-functionalized Fe₃O₄ hybrid microspheres adsorbent from a facial and one-step solvothermal route by using FeCl₃·6H₂O as a single iron source and 3-aminophenoxy-phthalonitrile as ource of amino groups. During solvothermal process, the nitrile groups of 3-aminophenoxy-phthalonitrile would bond with the Fe₃O₄ through the phthalocyanine cyclization reaction to form the amino-functionalized Fe₃O₄ magnetic nano-material, which was confirmed by Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and thermo-gravimetric analyzer (TGA). From the scanning electron microscope (SEM) and transmission electron microscopy (TEM) observation, the resulting monodispersed amino-functionalized Fe₃O₄ hybrid microspheres with the diameters of 180–200 nm were synthesized via the self-assembly process. More importantly, as-prepared Fe₃O₄ nano-materials with abundant amino groups exhibited high separation efficiency when they were used to remove the Cu(II) from aqueous solutions. Furthermore, the adsorption isotherms of Fe₃O₄ nano-material for Cu(II) removal fitted the Langmuir isotherm model, in which the calculated maximum adsorption capacity could increase from 5.51 to 16.25 mg g^–1 at room temperature. This work demonstrated that the amino-functionalized Fe₃O₄ magnetic nano-materials were promising as efficient adsorbents for the removal of heavy metal ions from wastewater in low concentration.     

Synthesis of Amino-Functionalized Hexagonal Mesoporous Silica for Adsorption of Pb2+

Highly ordered amino‐functionalized hexagonal mesoporous silica (HMS‐NH₂) had been synthesized successfully by co‐condensation. The resultant materials were characterized by means of XRD, TEM, FT‐IR, N₂ ad‐desorption and ²⁹Si NMR to confirm the ordered mesoporous structure and the functionalization of the amino groups. The sample was employed as a Pb²⁺ adsorbent in aqueous solutions at room temperature. Both Lagergren's first order kinetic model and Lagergren's second order kinetic model were used to describe the adsorption data. It was found that the pseudo second order model fitted the sorption kinetic data better than the pseudo first order model. According to the information analyzed from AAS, HMS‐NH₂ had a Pb²⁺ adsorption amount of over 90.7 mg·g^?1, showing a promising application for the treatment of wastewater containing Pb²⁺ ions.     

多孔有机骨架:基于傅氏烷基化反应的合成与气体吸附性质

通过傅氏烷基化反应成功地合成了基于四苯锗烷构筑单元的多孔有机骨架材料PAF-9。用红外光谱,粉末X射线衍射,固体核磁共振,热重分析和低温氮气吸附-脱附表征了PAF-9材料的微结构与孔道性质。表征数据表明PAF-9具有非常高的热稳定性和化学稳定性,同时具有较高的比表面积。该PAF材料的BET比表面积为334 m²·g^-1。此外,得到的PAF材料对二氧化碳具有较好的吸附能力。     

多孔有机骨架:基于傅氏烷基化反应的合成与气体吸附性质

通过傅氏烷基化反应成功地合成了基于四苯锗烷构筑单元的多孔有机骨架材料PAF-9。用红外光谱,粉末射X线衍射,固体核磁共振,热重分析和低温氮气吸附-脱附表征了PAF-9材料的微结构与孔道性质。表征数据表明PAF-9具有非常高的热稳定性和化学稳定性,同时具有较高的比表面积。该PAF材料的BET比表面积为334m²·g^-1。此外,得到的PAF材料对二氧化碳具有较好的吸附能力。     

五乙烯六胺修饰的MCF基吸附剂的制备及其CO2吸附性能研究

以三嵌段共聚物P123 (EO₂₀-PO₇₀-EO₂₀)为模板剂合成了介孔泡沫氧化硅(MCF)材料. MCF经过五乙烯六胺(PEHA)修饰后用于捕捉CO₂. 采用扫描电镜(SEM)、透射电镜(TEM)、N2吸附-脱附、傅里叶变换红外(FTIR)光谱、热重分析(TGA)对MCF和MCF-PEHA进行了表征. 结果表明, PEHA对MCF改性后, 并没有破坏MCF载体本身的结构. MCF-PEHA的CO₂吸附量在75℃时达到最大. 随着PEHA含量的增加, MCF-PEHA的CO₂吸附量呈先增大后减小的趋势, 当PEHA含量为70% (w)时, CO₂吸附量达到最大, 为3.55 mmol·g^-1. 水汽促进了吸附剂的CO₂吸附性能. 研究结果还表明, MCF-70吸附剂经过四次吸脱附循环, 吸附性能基本保持不变, 表现出很好的可再生性能.     

磁性壳聚糖复合微球的制备及其Cu2+吸附性能

以球磨后的粉煤灰磁珠（MS）颗粒为磁核,通过溶胶凝胶法和反相微乳液法依次包覆SiO₂和壳聚糖（CS）,制备了MS@SiO₂@CS磁性微球。利用扫描电镜及能量色散谱仪、热重分析仪、红外光谱仪、X射线衍射仪、振动样品磁强计对所得样品的结构和磁性进行了系统表征。结果表明,磁珠颗粒表面实现了逐层包覆,较均匀的分散于壳聚糖基体中,MS@SiO₂@CS微球的比饱和磁化强度可达7.04 emu·g^-1。Cu²⁺离子吸附实验表明,所得磁性壳聚糖微球对Cu²⁺具有良好的吸附能力,最大吸附量可达11.08 mg·g^-1;而且可通过磁选法高效固液分离。吸附动力学研究表明,MS@SiO₂@CS微球对Cu²⁺离子的吸附符合准二级动力学模型,以化学吸附为主。     

Hyper-cross-linked polymers based on triphenylsilane for hydrogen storage and water treatment

The present research focuses on the synthesis and applications of a series of hyper-cross-linked polymer networks obtained from the one-step Friedel–Crafts reaction of triphenylsilane and formaldehyde dimethyl acetal. The materials were characterized through FTIR, ¹³C NMR, PXRD, TGA, N₂ adsorption-desorption isotherms, H₂ sorption and dye adsorption. These materials exhibited increased surface areas of approximately 441–1101 m² g^?1 with increasing ratio of monomer to cross-linker. The H₂ storage capacity of the polymer networks reached 1.19 wt % (5.96 mmol g^?1) under 1.03 bar and 77.3 K. In addition, the material showed excellent adsorption capacity of 806 mg g^?1 for Congo Red and retained their adsorption capacity after recycling nine times. Taken together, the results demonstrate that the obtained hyper-cross-linked polymers could be applied to H₂ storage and water treatment.     

A Novel Affinity Support Material for the Separation of Immunoglobulin G from Human Plasma

2‐Methacrylamidohistidine (MAH) as a pseudospecific ligand was synthesized from methacryl chloride and histidine. Spherical beads with an average size of 50–63 μm were obtained by the radical suspension polymerization of MAH and 2‐hydroxyethyl methacrylate (HEMA) conducted in an aqueous dispersion medium. Owing to the reasonably rough character of the bead surface, P(HEMA‐co‐MAH) beads had a specific surface area of 17.6 m²·g^–1. Synthesized MAH was characterized by NMR. P(HEMA‐co‐MAH) beads were characterized by swelling studies, FT‐IR spectroscopy, scanning electron microscopy (SEM) and elemental analysis. P(HEMA‐co‐MAH) affinity beads with a swelling ratio of 65% were used in the separation of human immunoglobulin G (HIgG) from aqueous solutions and human plasma. The maximum HIgG adsorption on the P(HEMA‐co‐MAH) adsorbents was observed at pH 7.4 for phosphate and at pH 6.0 for morpholinoethanesulfonic acid buffers. The HIgG adsorption onto the PHEMA adsorbents was negligible. Higher adsorption values (up to 46.5 mg·g^–1) were obtained when the P(HEMA‐co‐MAH) adsorbents were used in aqueous solutions. Much higher amounts of HIgG were adsorbed from human plasma (up to 73.8 mg·g^–1). Adsorption capacities of other blood proteins were obtained as 3.2 mg·g^–1 for fibrinogen and 4.6 mg·g^–1 for albumin. The total protein adsorption was determined to be 82.2 mg·g^–1. The pseudospecific affinity beads allowed one‐step separation of HIgG from human plasma. HIgG molecules could be repeatedly adsorbed and desorbed with these adsorbents without noticeable loss in their HIgG adsorption capacity.     

酸法纳米纤维素模板剂合成介孔TiO2及光催化活性

以生物可再生资源的酸法纳米纤维素为模板剂,四氯化钛为钛源,采用液相水解-沉淀法制备了具有介孔结构的TiO2光催化剂。采用低温N2物理吸附-脱附、透射电镜(TEM)、X射线衍射(XRD)、热重-量热扫描(TG/DSC)、傅里叶变换红外(FTIR)、X射线光电子能谱(XPS)等对介孔TiO2进行了表征,并以甲基橙为模型物,考察了介孔TiO2光催化活性。结果表明,以酸法纳米纤维素为模板剂合成的TiO2光催化活性显著提高,且具有良好的孔隙结构,平均孔径5.03 nm、总孔容积0.35 cm3.g-1、比表面积192m2.g-1;纤维素模板剂合成的TiO2表面羟基数量降低;纤维素长链分子结构之间的羟基与TiO2表面羟基的键合,可有效限制TiO2前驱体的生长和团聚,并抑制锐钛矿相TiO2向金红石相转变。