纳米孔SiO2气凝胶块

以工业水玻璃为硅源,采用三甲基氯硅烷[（CH3）3SiCl,TMCS]／正已烷（C6H14）／EtOH溶液对二氧化硅水凝胶进行表面改性处理,使水凝胶的溶剂交换和表面改性在一步同时完成。研究了pH值、改性剂对气凝胶的影响。结果表明,所制备的气凝胶具有典型的气凝胶结构特征,孔洞尺寸、比表面积分剐在8～12nm、600～640m^2／g范围内。颗粒尺寸小于100nm。     

以工业水玻璃为原料制备纳米孔SiO2气凝胶块体材料

以工业水玻璃为硅源,采用三甲基氯硅烷[(CH3)3SiCl,TMCS]/正己烷(C6H14)/EtOH溶液对二氧化硅水凝胶进行表面改性处理,使水凝胶的溶剂交换和表面改性在一步同时完成.研究了pH值、改性剂对气凝胶的影响.结果表明,所制备的气凝胶具有典型的气凝胶结构特征,孔洞尺寸、比表面积分别在8～12 nm、600～640 m2/g范围内,颗粒尺寸小于100 nm.     

SiO2气凝胶快速合成

以廉价的水玻璃为硅源，用乙醇（EtOH）／三甲基氯硅烷（TMCS）／庚烷混合溶液浸泡水凝胺，使对水凝胶的溶剂交换和表面改性在一步完成，在环境干燥条件下合成了SiO2气凝肢，所合成的SiO2气凝肢为轻质透明的块状固体，密度为0．128—0．165g／cm^3，孔隙率92.4％～94．2％。利用FT-IR、SEM、TEM和BET吸附对气凝肢的微观结构和形貌进行了研究，结果表明，气凝胶为纳米介孔结构，粒子直径和孔径分布均匀，断面呈现明显的蜂窝状结构，孔径13nm左右，比表面积约618m^2／g，表面带有较多的Si—CH3基团。     

用工业水玻璃制备纳米孔二氧化硅气凝胶块体材料

以工业水玻璃作为硅源，采用三甲基氯硅烷[（CH3）3SiCl，TMCS]、正己烷（C6H14）、乙醇溶液对二氧化硅水凝胶进行表面改性处理，使水凝胶的溶剂交换和表面改性在一步同时完成。过程包括：1）在水玻璃中[Na2O与SiO2的物质的量比为1：（3．1—3．3）]加入浓硫酸调节pH，用磁力搅拌器搅拌均匀，然后倒入模具中，在室温下静置，使之成为湿凝胶；2）以三甲基氯硅烷、正己烷为改性剂，将二者的混合溶液倒入盛有湿凝胶的模具中，在室温下静置一段时间，然后在无水乙醇溶液中浸泡2d，然后进行干燥得到气凝胶。所制备的气凝胶具有典型的气凝胶结构特征，孔洞尺寸、     

疏水SiO2气凝胶的常压制备及在建筑隔热涂料中的应用

以廉价的工业级正硅酸乙酯为原料,经过酸碱两步催化制备二氧化硅凝胶,分别以三甲基氯硅烷(TMCS)/六甲基二硅氧烷(HMDSO)溶液和TMCS/n-C6H14溶液对凝胶进行改性,常压干燥下制得产品。用FT-IR、TEM、XRD等手段对样品进行表征,并考察了产品的疏水性能和在外墙涂料中的隔热性能。在相同的条件下,前者可以使凝胶溶剂交换和表面改性同时完成,而后者则不能。以TMCS/HMDSO改性所得产品为无定型非晶态结构,具有5～10 nm孔径。改性后的SiO2气凝胶具有较强的疏水性,在外墙建筑涂料中具有优良的隔热性能。     

疏水SiO2气凝胶制备

以自制的硅溶胶为原料，通过三甲基氯硅缈六甲基二硅氧烷（trimethylehlorosilsne／hexamethyldlsiloxane，TMCS／HMDSO）混合液对制得的水凝胶直接进行表面改性，用乙醇洗涤以后，在常压条件下干燥后得到疏水的SiO2气凝胶。研究表明；当溶胶液pH值从3变到5，最终得到的气凝胶的密度随pH值的增大逐渐减小到最低点后又有所增大，而气凝胶的比表面积则呈相反的变化趋势。当改性剂TMCS／H20的摩尔比大于0．1时，最终可得到疏水的气凝胶，当其大于0．2后气凝胶的密度和疏水性变化不大。Si02气凝胶密度和比表面积分别在100-160kg／m^3和539-720m^2／g范围。     

疏水SiO2气凝胶制备

以自制的硅溶胶为原料，通过三甲基氯硅缈六甲基二硅氧烷（trimethylehlorosilsne／hexamethyldlsiloxane，TMCS／HMDSO）混合液对制得的水凝胶直接进行表面改性，用乙醇洗涤以后，在常压条件下干燥后得到疏水的SiO2气凝胶。研究表明；当溶胶液pH值从3变到5，最终得到的气凝胶的密度随pH值的增大逐渐减小到最低点后又有所增大，而气凝胶的比表面积则呈相反的变化趋势。当改性剂TMCS／H20的摩尔比大于0．1时，最终可得到疏水的气凝胶，当其大于0．2后气凝胶的密度和疏水性变化不大。Si02气凝胶密度和比表面积分别在100-160kg／m^3和539-720m^2／g范围。     

疏水SiO2气凝胶的低成本制备

以自制的硅溶胶为原料,通过三甲基氯硅烷／六甲基二硅氧烷(trimethylchlorosilane／hexamethyldisiloxane,TMCS／HMDSO)混合液对制得的水凝胶直接进行表面改性,用乙醇洗涤以后,在常压条件下干燥后得到疏水的SiO2气凝胶。研究表明：当溶胶液pH值从3变到5,最终得到的气凝胶的密度随pH值的增大逐渐减小到最低点后又有所增大,而气凝胶的比表面积则呈相反的变化趋势。当改性剂TMCS／H2O)的摩尔比大于0．1时,最终可得到疏水的气凝胶,当其大于0．2后气凝胶的密度和疏水性变化不大。SiO2气凝胶密度和比表面积分别在100～160kg／m^3和539～720m^2／g范围。     

常压制备疏水性二氧化硅气凝胶及表面结构表征

用咪唑盐离子液体[C6Mim][BF4]作溶剂和催化剂,经由溶剂置换、常压分级干燥,制备出大块SiO2气凝胶。气凝胶表面结构决定了气凝胶是否具有疏水性,我们用不同比例的甲基三甲氧基硅烷(MTMS)和正硅酸乙脂(TEOS)前驱体来改变气凝胶孔表面Si—OH、Si—O—CH3、Si—CH3组成,网络表面结构用1HNMR核磁共振和傅里叶红外衍射表征。结果表明疏水基团和亲水基团共同组成了气凝胶材料的表面,疏水试验也表明样品具有很好的疏水性。     

疏水性SiO2气凝胶常压干燥制备与表征

以正硅酸乙酯(TEOS)为硅源,以NH4F为催化剂,实现了纳米多孔SiO2气凝胶材料的常压干燥制备,采用三甲基氯硅烷(TMCS)进行疏水改性,以减少样品在使用过程中的收缩和塌陷.结果表明:TMCS疏水改性的SiO2气凝胶样品的表观密度为0.191 g/cm3,导热系数为0.031 W/(m· K),比表面积为667 m2/g.SEM和TEM的测试结果表明,所得样品为纳米介孔材料.接触角的测定分析表明,TMCS疏水改性的SiO2气凝胶样品与水的接触角为147°,表现出良好的疏水性.400 ℃热处理后,气凝胶因失去大量的甲基基团,由疏水性变为亲水性.     

Fabrication and characterization of the monolithic hydrophobic alumina aerogels

The monolithic hydrophobic mesoporous alumina aerogels were successfully synthesized by acid–base sol–gel polymerization of aluminium chloride hexahydrate (AlCl₃·6H₂O) in deionized water/alcohol solution (v/v = 3:7). To minimize shrinkage during drying, alumina hydrogels were aged in tetraethylorthosilicate (TEOS)/acetonitrile solution, and modified using trimethylchlorosilane (TMCS)/acetonitrile solution. Properties of the final product were examined by contact angle measurement, FTIR, FESEM, TEM and BET analyses. Surface modification was confirmed by FTIR spectroscopy. It was found that hydrophobic property of the alumina aerogels was affected by the contents of TMCS. When the molar ratio of TMCS to AlCl₃·6H₂O is 0.35, hydrophobic alumina aerogels shows lower bulk density (0.453 g/cm³) and higher surface area (495 m²/g) than those of unmodified alumina aerogels (0.933 g/cm³, 413 m²/g).     

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。     

二氧化硅气凝胶最佳制备工艺的确定

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。并通过正交试验,确定了制备凝胶的最佳工艺条件是:pH=5,TEOS∶乙醇∶水(摩尔比)=1∶4∶8;利用FTIR、XRD和SEM等方法对二氧化硅气凝胶改性特征和添加DCCA前后的物理性质进行表征。     

Effects of Solvent Exchange Period and Heat Treatment on Physical and Chemical Properties of Rice Husk Derived Silica Aerogels

In this study, hydrophobic silica aerogels were synthesized from rice husk ash-derived sodium silicate through sol-gel processing, solvent exchange, surface modification and ambient pressure drying. By volume, 10% of trimethylchlorosilane (TMCS) in 90% of n-hexane was used as a hydrophobic solution in the surface modification process. The physical and chemical properties of silica aerogels were characterized by density and porosity measurements, scanning electron microscopy (SEM), Fourier transforms infrared (FTIR) spectroscopy, Brunauer–Emmett–Teller theory (BET) and dynamic scanning calorimetry (DSC). The hydrogels prepared were in the form of 2.5 ± 0.5 mm beads and then converted into alcogels through solvent exchange with ethanol for repetition of 3, 6 and 9 days. It is found that the optimal quality of silica aerogels with the BET surface area as high as 668.82 m²/g was obtained from the alcogels of the solvent exchange period of 9 days. Depending on the size of the gel’s block, a longer solvent exchange period will ensure adequate removal of pore water. Post heat treatment on silica aerogels obtained from the 9 days of solvent exchange at 200, 300 and 400 °C for 2 h results in slight decreased of aerogel’s density from 0.048 g/cm³ to 0.039 g/cm³ and the hydrophobicity of the aerogels is decreased above 380 °C as confirmed by DSC analysis.

     

常压制备疏水性二氧化硅气凝胶

以正硅酸乙酯(TEOS)为硅源,氢氟酸作催化剂,采用溶胶-凝胶法常压下制备二氧化硅气凝胶,并研究催化剂、乙醇、水等因素对凝胶过程的影响。采用傅里叶变换红外分析(FT-IR)、电子扫描探针(SPM)等对二氧化硅气凝胶的结构和性能进行研究。结果表明,经三甲基氯硅烷(TMCS)表面改性处理后的气凝胶表现出了很好的疏水性能。该气凝胶密度为200~400 kg/m³,与水的接触角大于120°。当n(TEOS)∶n(乙醇)∶n(H₂O)∶n(HF)=1∶6∶4∶0.25时,得到的气凝胶各方面的综合性能最好。凝胶时间随着水和氢氟酸用量增加而缩短,随乙醇用量的增加而增加。     

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。     

常压干燥法制备疏水性SiO2气凝胶

利用正硅酸乙酯做先躯体,盐酸与氨水做催化剂,通过二步法制备了二氧化硅气凝胶,并利用三甲基氯硅烷和正己烷做表面改性剂采用共沸法逐级对湿凝胶进行表面改性.测试分析了气凝胶的密度、表观、疏水性、比表面积、孔径分布和热稳定性.结果表明:气凝胶的物理特性及其疏水性受到三甲基氯硅烷与正己烷的体积比(ψ)的影响,其密度随着ψ增大而减小,当ψ=3%时,气凝胶的疏水性最好;所制得的SiO2在350℃仍具有良好的热稳定性,并且具有高比表面积(838.6 m2/g)和孔体积(2.10cm3/g).     

Preparation of silica aerogel from oil shale ash by fluidized bed drying

The silica aerogel with high specific surface area and large pore volume was successfully synthesized using oil shale ash (OSA) via ambient pressure drying. The oil shale ash was burned and leached by sulfuric acid solution, and then was extracted using sodium hydroxide solution to produce a sodium silicate solution. The solution was neutralized with sulfuric acid solution to form a silica gel. After washing with water, the solvent exchange with n-hexane, and the surface modification with hexamethyldisilazane (HMDZ), the aged gel was dried by fluidization technique and also using a furnace to yield silica aerogels. The physical and textural properties of the resultant silica aerogels were investigated and discussed. The results have been compared with silica aerogel powders dried in a furnace. From the results, it is clear that the properties of silica powders obtained in fluidized bed are superior to that of powders dried in the furnace. Using fluidization technique, it could produce silica aerogel powders with low tapping density of 0.0775 g/cm³, high specific surface area (789 m²/g) and cumulative pore volume of 2.77 cm³/g.