超临界干燥制备疏水型二氧化硅气凝胶

文章以正硅酸乙酯为原料,经溶胶-凝胶过程制备二氧化硅醇凝胶,采用三甲基氯硅烷作为表面改性剂,对醇凝胶进行化学表面修饰,超临界干燥,制备了疏水性二氧化硅气凝胶粉末。运用红外光谱、BET、扫描电镜、XRD对其结构、形貌及化学组成进行了分析。结果表明：该样品是表面连有疏水基团-CH3的疏水性SiO2气凝胶,呈连续网络结构的球状纳米粒子,孔径分布主要集中在2～4nm,是热稳定性较高的非晶、多孔、轻质介孔材料。     

疏水性二氧化硅气凝胶的常压制备与表征

采用溶胶-凝胶技术,以正硅酸乙酯为有机前驱体,三甲基氯硅烷为改性剂,在常压下干燥制备出疏水性二氧化硅(SiO2)气凝胶,同时采用密度测量、比表面积和孔径分布仪、扫描电镜、热重分析仪对SiO2气凝胶进行表征。文章重点研究反应物配比和表面修饰对SiO2气凝胶性能的影响。结果表明,采用正硅酸乙酯、水、乙醇体积配比为25︰6︰80和三甲基氯硅烷的正己烷溶液表面修饰合成的SiO2气凝胶性能质量较好。     

疏水SiO2气凝胶的制备及表征

以正硅酸乙酯(TEOS)为硅源,三甲基氯硅烷(TMCS)为改性剂,经老化、表面疏水改性,常压干燥制备了高比表面积疏水SiO2气凝胶.用傅立叶变换红外光谱仪(FT-IR)、扫描电镜(SEM)、比表面及孔径分布仪、热重分析仪(TG-DSC)对其疏水特性及结构进行表征.结果表明:疏水SiO2气凝胶与水的接触角达145°,在空气中的热稳定温度为269 ℃;且比表面积达1035 m2/g,具有典型的气凝胶结构特征,孔径尺寸和密度分别达9.7 nm和0.129 g/cc,骨架颗粒尺寸小于30 nm.     

SiO_2气凝胶的常温法合成研究及表征

以正硅酸乙酯（TEOS）为硅源,采用酸、碱两步催化的溶胶-凝胶法,通过L9（34）四因素三水平正交试验,研究了无水乙醇（ETOH）、草酸（H2C2O4）和氨水（NH3 H2O）之间的摩尔比以及酸碱间隔时间对气凝胶性能的影响,并对所得产品结构和性能进行了比表面（BET）、傅立叶转换、红外线光谱（FTIR）和扫描电镜（SEM）表征,从而首次实现了SiO2气凝胶的常温合成。实验结果表明：原料最佳摩尔比为TEOS∶ETOH∶H2C2O4∶NH3.H2O=1∶7∶3.5∶2.5,酸碱最佳间隔时间为18 h,SiO2气凝胶的平均粒径为6.58 nm,密度为100 kg/m3,孔径分布为2～30 nm,比表面达到938.17 m2/g,室温条件下合成的SiO2气凝胶,不亚于高温合成法的产品性能。     

疏水SiO2气凝胶的制备及应用研究进展

介绍了SiO2气凝胶的特性,阐述了疏水性SiO2气凝胶的制备方法,综述了气相氧化法、表面后处理法、原位法等制备疏水性SiO2气凝胶的原理和方法,简述了疏水SiO2气凝胶在热学、光学、化学(吸附和催化)及医学等领域的应用现状,最后展望了疏水性SiO2气凝胶的发展和应用前景,其在隔热、超疏水功能纺织材料上的应用也具有较好的发展前景.     

疏水性二氧化硅气凝胶的合成及表征

本文以正硅酸乙酯为原料,经溶胶-凝胶过程制备二氧化硅醇凝胶,再利用二甲基二氯硅烷对醇凝胶进行化学表面修饰,最后用超临界干燥方法制备了疏水性二氧化硅气凝胶.运用红外光谱、BET、扫描电镜、X射线衍射等测试方法对制得样品的结构、形貌及化学组成进行了分析.结果表明该样品是表面存在疏水基团-CH3 的疏水性SiO2 气凝胶,是呈连续网络结构的球状纳米粒子,孔径分布主要集中在2～10 nm,是热稳定性较高的非晶、多孔、轻质介孔材料.     

二氧化硅气凝胶的制备工艺与应用

三维纳米孔隙结构的二氧化硅气凝胶具有孔隙率高、密度低、比表面积大等基本特征,这些优异的特性使二氧化硅气凝胶在许多领域得到广泛研究和应用。二氧化硅气凝胶一般通过溶胶-凝胶过程、老化、干燥处理得到。主要总结了二氧化硅气凝胶的制备过程及机理,介绍二氧化硅气凝胶的相关领域的应用,并对二氧化硅气凝胶材料的发展前景进行了展望。     

Influence of Catalyst (Citric Acid) Concentration on the Physical Properties of TEOS Silica Aerogels

In the present paper, the experimental results on the influence of catalyst (citric acid) concentration on the physical properties of TEOS silica aerogels, are reported. The aerogels have been prepared by hydrolysis and polycondensation of tetraethoxysilane (TEOS) using citric acid (CTA) as a new catalyst followed by supercritical drying in an autoclave. In order to obtain the best quality silica aerogels in terms of monolithy, high transparency, low density, large surface area and high porosity with uniform pore size distribution, the catalyst concentrations were varied from 0.0005 M to 0.1 M by keeping the molar ratio of TEOS : EtOH : H₂O constant at 1 : 5 : 7, respectively. It has been found that the lower (<0.001) CTA concentration resulted in low density, smaller surface area but opaque aerogels whereas higher (>0.005 M) CTA concentration resulted in high density, large surface area, highly transparent but cracked aerogels. On the other hand, medium (between 0.001 and 0.005 M) CTA concentration resulted in monolithic, low density, large surface area and highly transparent silica aerogels. The pore size distribution (PSD) for higher (0.1 M) and lower (0.0005) CTA concentrations shifted towards smaller and larger pore radii respectively, whereas for medium (0.001 M) CTA concentration, the PSD is narrow and uniform, which reduces the differential pressure during supercritical solvent extraction leading to monolithic silica aerogels. These results have been supported and discussed by considering the particle and pore sizes observed by Scanning Electron Microscopy (SEM). The surface area was measured by BET analysis.     

常压制备低密度SiO2气凝胶的正交分析及表征

选择5因素4水平的L16(45)正交试验,以正硅酸乙酯(tetraethoxysilane,TEOS)为原料,采用酸碱两步催化溶胶-凝胶法和常压干燥制备了SiO2气凝胶,分析了正交实验因素对结果的影响,并对气凝胶的形貌、表面基团、疏水性、孔结构进行了表征.实验结果表明:表面改性对制备低密度SiO2气凝胶影响最大,正交试...     

二氧化硅气凝胶的研究现状及应用前景

二氧化硅气凝胶由于其特殊的网络结构使其具有密度小、隔热性好、孔隙率高、比表面积大、传声速率低等优良性能。从1931年开始,经过广大研究者几十年的深入研究,二氧化硅气凝胶有了更广阔的发展。本文介绍了以不同原料制备二氧化硅气凝胶的方法,论述了二氧化硅气凝胶的干燥技术,概述了二氧化硅气凝胶的改性措施,分析了二氧化硅气凝胶的应用前景。     

聚醚砜疏水膜的制备和性能表征

以质量分数15%的聚醚砜(PES)为膜材料,以N,N-二甲基乙酰胺为溶剂,分别以聚乙二醇(PEG400),无机小分子磷酸和有机小分子丙酮为添加剂,研究了添加剂种类及浓度对PES膜性能的影响。结果表明,同种添加剂,随PES分子量增大制得膜的孔隙率增大。不同添加剂,大分子PEG孔隙率随浓度先增大后减小,而磷酸随浓度变化不显著,由接触角测定,发现正面亲水性明显强于反面,抗污染性优于反面。     

SiO2气凝胶制备过程中缩裂问题的研究

基于实验,分析了SiO2气凝胶在制备过程中收缩开裂的原因,并系统研究了原料和溶剂(水和乙醇)的用量及催化剂的使用、老化等因素对SiO2气凝胶结构的影响,利用这些因素来实现对其进行微观结构控制,采用乙醇超临界干燥技术解决该材料制备过程中的缩裂问题。     

Noble Metal Immersion Spectroscopy of Silica Alcogels and Aerogels

We have fabricated aerogels containing gold and silver nanoparticles for gas catalysis applications. The technique of immersion spectroscopy is extended to porous or heterogeneous media allowing the surface area of metal available for catalytic gas reaction to be determined. Specifically, we apply the predominant effective medium theories to the heterogeneous interlayer surrounding each particle to determine the average fractional composition of each component in this inhomogeneous layer. The technique is satisfactory for statistically random metal particle distributions but needs further modification for aggregated or surfactant modified systems. Additionally, the kinetics suggest that collective particle interactions in coagulated clusters are perturbed during silica gelation resulting in a change in the aggregate geometry.     

不同粒径含氟丙烯酸酯共聚乳液的合成及膜表面疏水性能研究

采用半连续种子乳液聚合的方式,以丙烯酸丁酯、甲基丙烯酸甲酯和甲基丙烯酸六氟丁酯为原料制备了粒径分别为30nm、75nm、210nm左右的含氟丙烯酸酯共聚物乳液。通过乳胶粒核壳结构设计与大小粒径乳液机械共混改性2种方法研究了如何在较少含氟单体用量的情况下达到较好的表面疏水性能。利用X射线光电子能谱、动态光散射仪、接触角测定仪等分析手段,研究了共聚物膜的表面性能和共聚物乳液粒径的大小及分布,测试结果表明,核壳结构乳液成膜后壳层含氟量较高,膜表面接触角大于90,°疏水性能强;而大小粒径乳液共混物成膜后表面含氟量较低,却仍能得到90°以上的接触角,表明乳胶膜表面具有粗糙结构,具有一定的仿荷叶效应。     

Thermal Insulation Characteristics of Polybenzoxazine Aerogels

Polybenzoxazine (PBO) aerogels with low densities and low thermal conductivities are prepared from Bisphenol A (BPA) benzoxazine monomers by ring‐opened polymerisation using HCl as a catalyser at 10 °C. The obtained PBO aerogels have cross‐linked and 3D network structures with the densities ranging from 0.084 to 0.526 g cm^?3. The thermal conductivities under different pressures (3–10⁵ Pa, air) and different atmospheres (N₂, Ar, and CO₂, 10⁵ Pa) are investigated. The thermal conductivities are in the range of 0.0335–0.0652 W m K^?1 under ambient pressure and 0.0098–0.0571 W m K^?1 at 3 Pa. The thermal transfer mechanism under different gas pressures is analyzed with increasing pressure. Under different atmospheres, the thermal conductivities decrease as the molecular weight of the gas increases. Compared with the traditional organic foam insulating materials of phenolic foam, polyurethane and polystyrene, which have similar apparent densities, PBO aerogels exhibit lower thermal conductivity of 0.0335 W m K^?1 than that of traditional organic foam at room temperature.     

Hydrophobic,Pore‐Tunable Polyimide/Polyvinylidene Fluoride Composite Aerogels for Effective Airborne Particle Filtration

Polyimide (PI) aerogels have great potential as filter materials, owing to their unique porous structure and excellent thermodynamic properties. In this work, polyvinylidene fluoride (PVDF) is introduced into the 3D network structure of crosslinked PI by phase separation to prepare PI/PVDF hybrid aerogels. By adding different amounts of PVDF, effective control of the aerogel porous structure is achieved, as a result, the air permeability of the hybrid aerogel is significantly improved while still achieving a filtration efficiency of airborne particulates of more than 99.8%. PVDF is aggregated and dispersed on the surface or inside of the aerogel in the form of nanoparticles, which effectively increases the hydrophobicity of the material. The contact angle of the prepared PI hybrid aerogel is ≈150°, and the water absorption is as low as 2.2%, which enables the aerogel to maintain structural stability in humid environments. In addition, the aerogel exhibits good adsorption effects on organic solvents.     

Adsorption of Ce(IV) Ions from Aqueous Solution by Silica Aerogels

The adsorption process of Ce(IV) ions from aqueous solution by the silica aerogels was studied. The silica aerogels with hydrophobicity were prepared by the sol-gel process, supercritical drying, and heat treatment. The SEM image and nitrogen adsorption-desorption isotherm show that the heat-treated silica aerogel was a co-continuous porous structure with high BET surface area and narrow pore size distribution. The adsorption of Ce(IV) ions onto the silica aerogels was found to be fitted well by pseudo-second-order kinetics and Langmuir isotherm model. The activation energy for Ce(IV) adsorption onto silica aerogels could be calculated to be about 17.88 kJ/mol, which implied that the attractive forces of adsorption were weak electrostatic forces accompanying most ion-exchange reactions. The thermodynamic parameters showed that the adsorption process was spontaneous and endothermic.     

Sorption and other properties of polytetrafluoroethylene/cellulose composite aerogels

Polytetrafluoroethylene/cellulose composite aerogels containing PTFE from 0 to 40 wt.% were obtained by drying the corresponding suspension mixtures at a temperature of 50°C. Cellulose isolated from the stem of Sosnowski hogweed was used as the main component of the aerogels. In present work, the composite aerogels were heated in an inert atmosphere at a temperature of 370°C to partially hydrophobize cellulose and remove surfactants that were present in the initial PTFE suspension. It was found that at this temperature, the thermal degradation of cellulose proceeded differently in the presence and absence of PTFE. The maximum water contact angle (156°) was obtained for the sample with 10 wt.% PTFE. Hydrophobized samples of aerogels were studied with the help of infrared spectroscopy, scanning electron microscopy, and powder x-ray diffractometry and tested as sorbents for various solvents. It was found that the volume of solvent absorbed by the aerogel, in the case of a sample with a PTFE content of 40 wt.%, can even exceed the initial volume of the absorber.     

Hydrophobic or Hydrophilic Fumed Silica as Filler of Polyurethane Adhesives

Two hydrophilic and two hydrophobic fumed silicas of different characteristics were added to solvent-based polyurethane adhesives (PU). IR spectroscopy, contact angle measurements and rheology (viscosity measurements, determination of viscoelastic properties) were used to monitor the variation of properties of PU adhesives produced by addition of silica. Immediate (green) adhesion was determined by T-peel testing of halogenated synthetic rubber/PU adhesive/halogenated synthetic rubber joints. Silica addition produced a noticeable increase in the PU adhesive viscosity which can be related to the variation of viscoelastic properties. Viscosity of PU adhesives containing hydrophilic silica slightly increased with time after preparation; the increase was less significant in PU adhesives with hydrophilic silica. In the rheological studies, silica imparted shear thinning and negative thixotropy to PU adhesives due to a better dispersion of the silica in the polyurethane during shearing. The addition of silica produces an increase in the storage modulus (G') of PU adhesives, the values obtained being independent of the hydrophilic or hydrophobic nature of the fumed silica. The increase of G' and the changes in tan δ of PU adhesives containing silica corresponded to an improvement in the green adhesion properties of chlorinated rubber/PU adhesive/chlorinated rubber joints. In general, in disagreement with previous results,¹ the presence of silica did affect the properties of solvent-based PU adhesives, but these properties were not dependent on the type of silica (hydrophobic or hydrophilic) used in this study.