制备条件对疏水SiO2气凝胶结构和性能的影响

以价廉的水玻璃为原料,通过六甲基二硅氧烷和三甲基氯硅烷混合改性剂对制备的SiO2水凝胶进行表面改性,避免了溶剂交换,并常压干燥得到疏水的SiO2气凝胶.研究了改性剂用量对气凝胶疏水性和结构的影响.疏水气凝胶与水的接触角在100～130°范围内.常压干燥制备的气凝胶具有典型的气凝胶结构特征,孔洞尺寸、密度和比表面积分别在5～6.5 nm,100～160 kg/m3和500～720 m2/g范围内,颗粒尺寸小于100 nm.疏水气凝胶在空气和氮气中的热稳定性分别为284 ℃和490 ℃.     

间苯二酚—甲醛基碳气凝胶的制备及其应用

超级电容器是新型储能器件之一，电极材料是影响其性能的关键因素。以间苯二酚和甲醛为主要原料，采用反相悬浮聚合的方法，通过常压干燥和碳活化过程获得高比表面积的碳气凝胶材料。制备的碳气凝胶材料比表面积达到1 783.6 m2/g，具有丰富的微孔结构，其比电容达到122.4 F/g，作为3 000 F超级电容器的电极材料，经过循环充放电测试，证实其具有良好的循环稳定性。以常压干燥方式制备的碳气凝胶应用于超级电容器中，表现出的电化学性能优异，不仅提供了碳气凝胶产业化新思路，也表明碳气凝胶在储能领域具有非常广阔的应用前景。     

氧化物气凝胶材料的制备及在F-T合成中的应用

F-T合成是将生物质和天然气等转化为汽油、柴油等液体燃料的重要过程。氧化物气凝胶是具有低密度、高比表面积、大孔和高热稳定性的材料,通过气凝胶材料制备的F-T合成催化剂具有较高的活性中心分散度和较好的传质性能。综述气凝胶催化剂在F-T合成反应中的研究,并对气凝胶材料制备过程中的关键步骤--干燥方法进行讨论,着重介绍通过溶剂置换和表面改性等方法在常压干燥条件下制备氧化物气凝胶材料的研究进展,展望气凝胶F-T合成催化剂未来的发展方向和应用前景。     

常压干燥法制备碳纤维增强型碳气凝胶

在传统方法制备碳气凝胶的基础上,以常压干燥代替超临界干燥,成功制备了碳气凝胶CRFs以及碳纤维针刺毡增强型碳气凝胶CF/CRFs,并通过SEM、BET测试方法对两者的内部微观结构进行了表征。制备的CRF具有典型的三维连续网络结构,催化剂含量不同影响了CRF的骨架颗粒和孔径大小。在CF/CRFs内部,碳纤维针刺毡和CRF能达到较好的复合效果,附着在纤维表面的CRF保持了纳米网络结构,但是纤维对CRF内部的骨架颗粒和孔径具有显著的影响,由力学分析得知碳纤维针刺毡的复合使CRF具有较好的抗弯和抗压性能。     

石棉绒增强SiO2气凝胶隔热材料常压工艺研究

气凝胶是一种优质隔热材料.本文以石棉绒纤维作为气凝胶的增强材料,以水玻璃为硅源,通过常压干燥工艺进行SiO2气凝胶块体保温隔热材料的制备.研究了湿凝胶制备工艺流程及洗涤工艺对气凝胶材料结构及性能的影响.研究发现,以石棉绒为增强材料常压制备SiO2湿凝胶的最佳制备工艺为:在水、纤维和分散剂配制的纤维分散悬浮液中首先加入乙醇搅拌均匀,然后与水玻璃和氟硅酸钠配制的水玻璃凝胶液搅拌混合,再注模固化;在固化湿凝胶的洗涤和溶剂置换工艺中,以水为洗涤溶剂效果好,产品性能高.以石棉绒为增强材料,采用常压干燥工艺制备的SiO2气凝胶隔热材料具有收缩率小,产品规整,密度小,孔隙率高,及较好的强度和隔热性能.     

水玻璃为源的超疏水型SiO2气凝胶块体制备与表征

采用廉价的水玻璃为硅源,通过乙醇溶剂替换及六甲基二硅醚和盐酸混合液对湿凝胶的表面基团改性,常压干燥出疏水介孔的SiO2气凝胶块体。制得的SiO2气凝胶块体具有超疏水性,在0～400℃附近,疏水角约155°～130°,其密度为80～200 mg/cm3,比表面积为568 m2/g,孔体积为2.9cm3/g,其室温下的热导率为0.026W/（m K）。     

碳气凝胶电极用于NaCl溶液电容性除盐的研究

碳气凝胶是一种新型多孔碳材料,具有比表面积大、电导率高的特点。本文通过常压干燥制备了碳气凝胶,研究测试了其结构特性,用N aCl溶液模拟海水,利用CD I原理,以碳气凝胶作电极进行了N aC l溶液的除盐实验。实验表明,决定碳气凝胶的除盐效果的主要因素为比表面积和电导率。在不同配比结构中,以R/C为1500、M值为30%的碳气凝胶电极的除盐效果最佳。利用双电层电容模型解释探讨了碳气凝胶电极的除盐机理。     

二氧化硅气凝胶制备条件的选择

二氧化硅气凝胶是典型的纳米多孔轻质材料,由于具有独特的性能并在许多领域存在潜在的应用价值而受到广泛关注。本文从气凝胶制备过程中的硅源的选择、溶剂的选择、制备工艺的选择、催化剂等方面进行了研究,有利于确定常压干燥制备二氧化硅气凝胶的生产条件。     

碳气凝胶电极用于NaCI溶液电容性除盐的研究

碳气凝胶是一种新型多孔碳材料，具有比表面积大、电导率高的特点。本文通过常压干燥制备了碳气凝胶，研究测试了其结构特性，用NaCl溶液模拟海水，利用CDI原理，以碳气凝胶作电极进行了NaCl溶液的除盐实验。实验表明，决定碳气凝胶的除盐效果的主要因素为比表面积和电导率。在不同配比结构中，以R/C为1500、M值为30％的碳气凝胶电极的除盐效果最佳。利用双电层电容模型解释探讨了碳气凝胶电极的除盐机理。     

添加剂PVB对炭气凝胶制备工艺及结构的影响

采用溶胶—凝胶法,以间苯二酚(R)、甲醛(F)为原料、无水碳酸钠(C)作催化剂、聚乙烯醇缩丁醛(PVB)为添加剂、无水乙醇作溶剂,通过常温常压干燥和高温炭化制备炭气凝胶。考察了中间产物有机凝胶的热解行为和催化剂浓度及PVB用量对炭气凝胶孔隙结构的影响。结果表明:PVB的加入不仅加强了有机凝胶的网络结构,使其更利于常温常压干燥,而且能够较好地调控炭气凝胶的孔径分布;在一定的PVB加入量范围内,随着PVB加入量的增加,炭气凝胶的比表面积增加,孔径分布也更加集中;催化剂浓度对炭气凝胶的比表面积及孔径分布有较大的影响,当R/C=300,PVB/R=1/10时比表面积达到最大值(386m~2/g)。     

纳米孔超级绝热材料气凝胶的制备与热学特性

以正硅酸四乙酯(TEOS)为硅源，通过溶胶–凝胶及超临界干燥过程制备了SiO2气凝胶. 同时，采用相对廉价的多聚硅(E–40)为硅源，以三甲基氯硅烷(TMCS)为表面修饰剂，硅油为干燥介质, 在常压条件下制备了同样具有纳米多孔结构的SiO2气凝胶. 用透射电镜、扫描电镜及孔径分布仪对其结构进行了表征，并用动态热线法对其热学特性进行了测试. 结果表明: 两种方法制备的气凝胶均是典型的纳米孔超级绝热材料，后者热导率略高但成本低许多，所以更具应用推广潜力.     

Starch-derived carbon aerogels with high-performance for sorption of cationic dyes

Environmentally green carbon aerogels have been prepared as adsorbents for dye-containing wastewater. The aerogels were prepared by carbonization of starch aerogels synthesized from soluble starch through a sol-gel process followed by drying at ambient pressure. The Brunauer-Emmett-Teller (BET) surface areas and pore size distribution were measured by N₂ adsorption/desorption, and the surface zeta-potential and microstructure of carbon aerogels were characterized using a scanning electron microscope (SEM) and zeta-potential analyzer. SEM images indicate that the carbon aerogels consist of flakes with side length of 60-120 μm and thickness of 3-4 μm. The flakes are irregular in shape and composed of spherical carbon nanoparticles of 10-30 nm. The carbon aerogels have both microporous and mesoporous structures and exhibit high specific surface areas, the highest value is 1571 m²/g. The mean diameter of the micropores is 0.89 nm and that of the mesopores is 2-10 nm. At pH = 10, the carbon aerogels have a zeta-potential of −40 mV and exhibit high adsorption capacities for cationic dyes, such as crystal violet (CV), methyl violet (MV) and methylene blue (MB), from aqueous solution. The largest adsorption capacities for CV, MV and MB are 1515, 1423 and 1181 mg/g, respectively.     

Fabrication and nano-structure control of carbon aerogels via a microemulsion-templated sol-gel polymerization method

Carbon aerogels were successfully fabricated by a microemulsion-templated sol-gel polymerization method. When a suitable molar ratio of surfactant to resorcinol (S/R) and an appropriate resorcinol-formaldehyde concentration were selected, the organic gels thus obtained could be dried with little shrinkage by heating at ambient pressure. The size of carbon nano-particles and the pore size of carbon aerogels thus produced decrease with an increase of S/R. The highest specific surface area and specific mesopore volume of the carbon aerogels prepared by our method were 620 m² g⁻¹ and 1.14 cm³/g, respectively.     

载体制备工艺对Pt/CA催化剂甲醇氧化催化性能的影响

比较研究了炭气凝胶(CA)的制备工艺条件对其表面微观结构及以其为载体的催化剂Pt/CA甲醇氧化催化活性的影响.结果表明,常压干燥制得的CA表面以微孔为主,而超临界CO2干燥制得的CA表面主要以中孔为主,而且比表面积、表面孔容和平均孔径更大;超临界CO2干燥比常压干燥更适合制备高活性甲醇氧化Pt/CA催化剂的载体材料;CA制备过程中催化剂Na2CO3的用量(常用R/C表示,其中R代表制备CA的原料间苯二酚,C代表制备CA的催化剂Na2CO3)为200至1000的范围内,R/C的增大会引起超临界CO2干燥制得CA的表面平均孔径随之增加,R/C为300时制得的CA具有最大的BET比表面积和表面孔容,以其为载体制得的催化剂具有最好的甲醇氧化催化性能.     

Preparation of low-density carbon aerogels by ambient pressure drying

With the addition of hexamethylenetetramine (HMTA) and alcohol as solvent, an ambient pressure drying technique was developed for the fabrication of low-density organic aerogels and related carbon aerogels. When a suitable ratio of resorcinol to HMTA (R/H ratio) and ratio of resorcinol to solvents (R/S ratio) are selected, the low-density alco-gels obtained can be dried under ambient pressure conditions without observable shrinkage. The addition of HMTA increases the size of carbon nano-particles and the pore size of the aerogels that are produced. The carbon aerogels prepared in this work have similar nano-particle structures typical of the aerogels prepared with CO₂ or by the isopropanol supercritical drying technique.     

溶胶凝胶一步溶剂交换与表面改性制备疏水硅气凝胶

以正硅酸乙酯为硅源,采用酸碱两步催化的溶胶-凝胶法,以无水乙醇/六甲基二硅氮烷/正己烷为溶剂交换与表面改性试剂,通过一步溶剂交换与表面改性和常压干燥工艺制备疏水SiO2气凝胶。用傅立叶变换红外光谱(FTIR)、X射线衍射(XRD)、热重-差示(TG-DSC)、场发射扫描电镜(F-SEM)和比表面积(BET)等检测手段对样品的结构、形貌和性能进行了表征。结果表明,将传统的溶剂交换与表面改性由多个步骤改为一步完成,使制备周期从原来的6d缩减到3d,不仅缩短了周期,而且使所得的SiO2气凝胶样品具有842.63m2/g的高比表面积、130kg/m3的低密度、15nm的超细颗粒、2～170nm的孔洞结构和良好的疏水性能。     

Enhanced thermal shrinkage behavior of phenolic-derived carbon aerogel-reinforced by HNTs with superior compressive strength performance

A novel carbon/m-HNTs composite aerogel was synthesized by introducing the modified halloysite nanotubes (m-HNTs) into phenolic (PR) aerogels through chemical grafting, followed with carbonization treatment. In order to explore the best proportion of HNTs to phenolic, the micromorphology of PR/m-HNTs were investigated by SEM before carbonization, confirming 10 wt% of m-HNTs is most beneficial to the porous network of aerogels. The interaction between PR and HNTs was studied by FTIR spectra, and microstructure evolution of the target product-carbon/m-HNTs composite aerogel were illustrated by SEM and TEM techniques. SEM patterns indicated that the carbon/m-HNTs aerogels maintain a stable porous structure at 1000 °C (carbonization temperature), while a ~20 nm carbon layer was formed around m-HNTs generating an integral unit through TEM analysis. Specific surface area and pore size distribution of composite aerogels were analyzed based on mercury intrusion porosimetry and N₂ adsorption–desorption method, the obtained results stayed around 500 m²g^?1 and 1.00 cm³g^?1 (pore volume) without significant discrepancy, compared with pure aerogel, showing the uniformity of pore size. The weight loss rate (26.76%) decreased greatly compared with pure aerogel, at the same time, the best volumetric shrinkage rate was only 30.83%, contributed by the existence of HNTs supporting the neighbor structure to avoid over-shrinking. The highest compressive strength reached to 4.43 MPa, while the data of pure aerogel was only 1.52 MPa, demonstrating the excellent mechanical property of carbon/m-HNTs aerogels.     

Carbon aerogels derived from cresol–resorcinol–formaldehyde for supercapacitors

The objective of the present paper is to demonstrate the possibility to synthesize mixed carbon aerogels (denoted C_mRF) from cresol (C_m), resorcinol (R) and formaldehyde (F), as an alternative economic route to the classical RF synthesis. These porous carbon aerogels can be used as electrode materials for supercapacitors with a high volume-specific capacitance. Organic precursor gels were synthesized via polycondensation of a mixture of resorcinol and cresol with formaldehyde in an aqueous alkaline (NaOH) solution. After gelation and aging the solvent was removed via drying at ambient pressure to produce organic aerogels. Upon pyrolysis of the organic aerogels at 1173 K, monolithic carbon aerogels can be obtained. By controlling the catalyst (Cat) molar ratio (C_m+R/Cat) in the range 200–500, up to 70% of the resorcinol can be replaced with the cheap cresol. The resulting homogeneous organic aerogels exhibit a drying shrinkage below 15% (linear). The shrinkage and mass loss upon pyrolysis of the mixed aerogels increase with increasing cresol content. Nitrogen adsorption at 77 K was employed to characterize the microstructure of the carbon aerogels. The data show that the porous structure of mixed carbon aerogels is similar to that of RF carbon aerogels. Cyclic voltammetry measurements show that the as-prepared C_mRF carbon aerogels exhibit a high volume-specific capacitance of up to 77 F/cm³.     

CuO(CoO,MnO)/SiO2纳米复合气凝胶催化剂载体的制备及其在合成碳酸二苯酯中的应用

以正硅酸乙酯为硅源,以乙酸铜、乙酸钴和乙酸锰的水溶液为前驱体,采用溶胶–凝胶法和CO2超临界干燥工艺制备了CuO(CoO,MnO)/SiO2纳米复合气凝胶。采用场发射扫描电镜、透射电镜和电子散射能谱分析等对纳米复合气凝胶的微观结构和组成进行了表征。采用Brunauer–Emmett–Teller法测定了纳米复合气凝胶的比表面积、孔径及孔径分布。以纳米复合气凝胶为载体制备了负载型催化剂,用于催化合成碳酸二苯酯(diphenyl carbonate,DPC),并用气相色谱仪对反应液进行了分析。结果表明:纳米复合气凝胶的粒径为20～100nm,孔径为2～8nm,平均孔径为3.16nm,比表面积为664.4m2/g;过渡金属的摩尔含量为13.77%;催化合成DPC的质量收率达27.14%。