硅酸铝纤维和玻璃纤维复合二氧化硅气凝胶材料的制备与性能

分别以硅酸铝纤维和玻璃纤维为骨架材料,采用溶胶-凝胶、常压干燥制得纤维复合二氧化硅气凝胶材料,并对材料进行了结构和性能的测试分析。结果表明,二氧化硅气凝胶附着于纤维表面,提高了材料力学强度。硅酸铝纤维复合二氧化硅气凝胶材料的隔音性能优于玻璃纤维复合二氧化硅气凝胶材料。两种纤维复合二氧化硅气凝胶材料耐高温、燃烧性能均达到A级。硅酸铝纤维复合二氧化硅气凝胶材料和玻璃纤维复合二氧化硅气凝胶材料的产烟毒性分别为AQ₁级和AQ₂级,导热系数分别为0.034 W/（m·K）和0.033 W/（m·K）。     

热处理对粉煤灰酸渣基二氧化硅气凝胶结构和疏水性的影响

粉煤灰酸渣是粉煤灰经酸溶提铝后的副产品,主要化学成分为无定形二氧化硅,其资源化利用不仅解决了粉煤灰酸渣堆存带来的环境问题,还能获得附加值较高的二氧化硅气凝胶。以粉煤灰酸渣制备的水玻璃为原料,通过溶胶-凝胶—溶剂交换/表面改性—常压干燥工艺成功制备了低密度（0.083 g/cm³）、高比表面积（708 m²/g）、高疏水性（接触角为143°）的多孔二氧化硅气凝胶。通过热重-差热分析、红外光谱分析、接触角测试、扫描电镜分析、氮气吸附-脱附测试等手段对热处理前后二氧化硅气凝胶的结构和疏水性进行了表征。结果表明,随着热处理温度升高,二氧化硅气凝胶的比表面积增大、疏水性逐渐减弱直至消失。300 ℃热处理后,二氧化硅气凝胶仍具有较强的疏水性（接触角约为128°）,密度为0.080 g/cm³。当热处温度为400~600 ℃时,二氧化硅气凝胶仍具有中孔结构,由疏水性变为亲水性,密度从0.073 g/cm³增加到0.078 g/cm³。     

包载槲皮素P/O/W多重皮克林乳液的制备及表征

为解决槲皮素溶解度低透皮性能差的问题，以疏水二氧化硅AEROSIL?R202、亲水二氧化硅AEROSIL?200为乳化剂，一缩二丙二醇和甘油为内醇相，制备水包油包醇（P/O/W）多重Pickering乳液，用其对槲皮素进行了包载。考察了内醇相（一缩二丙二醇和甘油）质量分数、疏水二氧化硅AEROSIL?R202质量分数、水乳比、亲水二氧化硅AEROSIL?200质量分数对P/O/W多重Pickering乳液性能的影响，得到最佳制备条件为：内醇相〔m（甘油）：m（一缩二丙二醇）=6：4〕质量分数为20%、疏水二氧化硅质量分数为3%、m（水）：m（初乳）=5：5、亲水二氧化硅质量分数为2%。对各相染色用激光共聚焦显微镜（CLSM）观察证明，成功制备了P/O/W多重Pickering乳液。X射线衍射仪（XRD）结果表明，槲皮素经多重乳液包载后结晶峰消失，表明该多重乳液对槲皮素有良好的包载效果。离心法测定包载槲皮素P/O/W多重乳液载药量达0.45 %± 0.02%。体外透皮实验和猪皮CLSM显示，槲皮素经该多重乳液包载后透皮性能得到改善，这主要是由于槲皮素在内醇相〔m（甘油）：m（一缩二丙二醇）=6：4〕中的溶解度可达60±2.1 mg/g，远大于在水 (<0.5 μg/g)或油 (<1 mg/g)中的溶解度。     

自疏水溶胶-凝胶体系制备疏水SiO2气凝胶

以聚二乙氧基硅氧烷（polydiethoxysiloxane,PDEOS）和甲基三乙氧基硅（methyltriethoxysilane,MTES）,以及氨水、水和乙醇组成自疏水的溶胶-凝胶体系,经过溶胶-凝胶过程可形成疏水的二氧化硅凝胶,经正己烷溶剂交换后,可在常压条件下干燥后得到疏水二氧化硅气凝胶.研究表明：自疏水溶胶-凝胶体系中TMES/PDEOS的质量比大于0.3时,可得到疏水二氧化硅气凝胶,其密度和比表面积分别为380～420 kg/m^3和965～1 020 m^2/g.     

常压制备疏水型二氧化硅气凝胶及透光率分析

采用溶胶-凝胶法,通过常压干燥制备了疏水型二氧化硅气凝胶。研究了pH、水解时间等因素对二氧化硅气凝胶透光率的影响。以正硅酸乙酯为原料,通过酸（草酸）-碱（氨水）两步催化,采用溶胶-凝胶法常压干燥制备了疏水型介孔二氧化硅气凝胶。正硅酸四乙酯、乙醇、草酸、氨水物质的量比为1∶4∶5∶0.2,草酸和氨水的浓度分别为0.008、0.05 mol/L时,采用二甲基二氯硅烷为改性剂常压制备了二氧化硅气凝胶。透射电镜、扫描电镜测试表明：二氧化硅气凝胶具有纳米介孔结构。接触角测定表明：二氧化硅气凝胶与水的接触角为148°,表现出疏水性。     

钛硅复合气凝胶的制备工艺与光催化能力研究

采用溶胶-凝胶工艺,经乙醇为溶剂的超临界干燥路线制备二氧化钛-二氧化硅复合气凝胶.对不同组成、不同煅烧温度和时间制备的气凝胶的光催化能力进行比较后,得出最佳工艺条件:二氧化钛与二氧化硅物质的量比为1:1,超临界干燥后600 ℃煅烧2 h.形成的复合气凝胶网络结构完善,有均匀的纳米多孔结构;比表面积达355.6 m2/g,孔容为0.32 mL/g,最可几孔半径为0.82 nm,平均孔半径为2.52 nm;其中二氧化钛为锐钛矿型,二氧化硅为无定形.     

纤维增强型二氧化硅气凝胶复合材料常压制备及表征

采用溶胶-凝胶法分别制备了木质素纤维、聚丙烯纤维、聚酯纤维、玻璃纤维、聚丙烯腈纤维等5种纤维增强型二氧化硅气凝胶复合材料,并对其进行了表征。结果表明：聚丙烯腈纤维增强二氧化硅气凝胶复合材料的收缩率最小（仅为9%）,且比表面积最大（为583 m2/g）;玻璃纤维增强二氧化硅气凝胶复合材料的块体光滑度最好;聚丙烯纤维增强二氧化硅气凝胶复合材料的透明度最高。纤维本身材质的差别导致了其与凝胶粒子的结合程度有所差异,因而对复合材料块体的透明度、比表面积、收缩率产生影响,而5种纤维增强二氧化硅气凝胶复合材料的疏水性能均非常良好。     

从稻壳中获得二氧化硅气凝胶的研究

研究了稻壳在盐酸中浸泡、煮沸、回流、干燥后,置于600℃燃烧,并保温2 h,制得了一系列二氧化硅气凝胶样品。重量法分析表明这些二氧化硅气凝胶中二氧化硅质量分数为99%以上,并采用了激光粒度仪、比表面测定仪（BET方法）、X射线衍射仪（XRD）、红外光谱仪（FT-IR）和扫描电镜（SEM）等研究了二氧化硅气凝胶样品,同时对使用稻壳能够成功制备二氧化硅气凝胶方法进行了探讨。     

DTAB表面活性剂在硅气凝胶干燥中的应用

使用十二烷基三甲基溴化铵（DTAB）阳离子表面活性剂溶液对湿凝胶进行处理,可降低凝胶中液体表面张力,从而得到保持较完整孔隙结构的硅气凝胶。结果表明,采用DTAB水溶液浸泡湿凝胶的方法要优于在凝胶形成前加入DTAB的方式。使用浓度为1.48×10-2 mol/L的DTAB水溶液浸泡湿凝胶可得到孔隙率为81.8%、平均孔径为15.749 nm、总孔体积为2.836 cm3/g、比表面积为923 m2/g的二氧化硅气凝胶;其吸脱附曲线明显高于其他添加浓度的吸脱附曲线,表明具有较高的吸附能力;在TEM图中可明显看出其具有孔隙结构。DTAB处理过的气凝胶明显优于未经处理的二氧化硅气凝胶。     

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。     

Effect of protic solvents on the physical properties of the ambient pressure dried hydrophobic silica aerogels using sodium silicate precursor

Considering the importance of the highly porous, low density, transparent and nanostructured hydrophobic silica aerogels in the scientific and industrial applications, the experiments have been carried out to prepare the low density silica aerogels using the 1.12 specific gravity water glass (sodium silicate, Na₂SiO₃) precursor, ammonium hydroxide (NH₄OH) catalyst, trimethylchlorosilane (TMCS) silylating agent, various first exchanging protic solvents and hexane as a second exchanging aprotic solvent. The first exchanging solvents used were: methanol, ethanol, propanol, isopropanol, butanol, isobutanol and hexanol. The molar ratio of the Na₂SiO₃:H₂O:NH₄OH:TMCS was kept constant at 1:56:0.02:0.4 respectively. The ambient pressure dried method was used for the preparation of hydrophobic silica aerogels. The effect of the exchanging protic solvents on the physical properties of the aerogels such as density, % of volume shrinkage, % of porosity, % of optical transmission, thermal conductivity, thermal stability and contact angle of the aerogels with water, were studied. FTIR studies were carried out to confirm the silylation of the aerogel samples. It was found that the exchanging protic solvents have profound effect on the physical and hydrophobic properties of the aerogels. Low density (0.07 g/cm³), high porosity (96.6 %), low thermal conductivity (0.091 W/mK), high contact angle (166°) silica aerogels could be prepared by using the isopropanol first exchanging solvent followed by the hexane as the second exchanging solvent along with the TMCS silylating agent with sodium silicate precursor.     

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。     

磷肥副产硅胶洗涤工艺试验研究

在预试验的基础上,研究了磷肥副产硅胶洗涤的影响因素,利用正交试验优化洗涤条件。采用响应曲面法,建立洗涤效率的回归模型,优化得到最佳洗涤工艺条件。结果表明,硅胶洗涤的最佳工艺条件为液固比10∶1,洗涤时间2 h,搅拌强度400 r/m in。在此条件下,经过5次水洗,磷肥副产硅胶中F、N、P的平均洗涤效率可达86.10%,95%以上水溶性杂质被脱除。     

Effect of sodium bicarbonate solution on methyltrimethoxysilane-derived silica aerogels dried at ambient pressure

Here we present an economical ambient pressure drying method of preparing monolithic silica aerogels from methyltrimethoxysilane precursor while using sodium bicarbonate solution as the exchanging solvent. We prepared silica aerogels with a density and a specific surface area of 0.053 g∙cm⁻³ and 423 m²∙g⁻¹, respectively. The average pore diameter of silica aerogels is 23 nm as the pore specific volume is 1.11 cm³∙g⁻¹. Further, the contact angle between water droplet and the surface of silica aerogels in specific condition can be as high as 166°, which indicates a super-hydrophobic surface of aerogels.     

Thermal,mechanical, and acoustic properties of silica‐aerogel/UPVC composites

The properties of silica‐aerogel/UPVC composites have been investigated with emphasis on sound and heat insulation. UPVC is a material of construction for window profiles and drainage pipes. Hydrophobic silica aerogels were synthesized using silicate sodium as a precursor through a two‐step sol–gel process. The physical and textural properties of the synthesized silica aerogels such as density, surface area, and particle size were analyzed using SEM and BET analysis. Then, the synthesized aerogels were mixed with Unplastisized Polyvinyl Chloride (UPVC) compound at five different weight ratios in an internal mixer to find out the effects of silica aerogels on the thermal, mechanical, and acoustical characteristics. The prepared UPVC/aerogel composites were characterized for tensile properties, impact strength, hardness, Vicat softening temperature, thermal conductivity, sound absorption, and sound transmission loss. The results revealed that adding silica aerogel in to the matrix of UPVC increases its hardness and softening temperature while decreases impact strength. The thermal conductivity of UPVC was decreased by up to 50% using silica aerogel. The sound absorption property of UPVC was increased up to three times by using silica aerogels due to its high porosity. Silica aerogel increased the maximum sound transmission loss of UPVC in the low frequency range. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44685.     

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.     

阻燃纳米二氧化硅气凝胶的仿生制备进展

摘要l自然界中的稻秆是一种二氧化硅（SiO2）／纤维素的纳米复合材料,SiO2与纤维素在纳米尺度的复合,使稻秆质轻和刚柔并具。效仿天然植物复合材料的构筑原理,纳米纤维素模板法仿生制备轻质阻燃材料纳米二氧化硅气凝胶。综述了二氧化硅的仿生制备、二氧化硅气凝胶的制备,探讨了仿生制备的轻质阻燃材料纳米二氧化硅气凝胶的应用前景。     

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.