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Recovery and Reutilization of the Solvents and Catalyst Used in the Sol–Gel Synthesis of Silica Xerogel
ACS Sustainable Chemistry & Engineering ( IF 7.1 ) Pub Date : 2019-02-21 00:00:00 , DOI: 10.1021/acssuschemeng.8b06848
Xiansong Li 1 , Shiquan Liu 1
Affiliation  

Silica xerogels were synthesized via the hydrolysis and condensation of tetraethyl orthosilicate (TEOS) under the catalysis of n-butylamine (BA), followed by drying the formed wet gel under ambient pressure at 120 °C. The solvents (water and ethanol) and catalyst enclosed in wet gels were recovered during the drying process. It was found that the relative percentage of ethanol in the recovered liquids increased, while those of water and butylamine decreased. The recovered liquids were directly used for four runs, and then the contents of BA, H2O, and TEOS were adjusted to maintain the reactant ratios to be the same as those in the first run, facilitating a fast sol and gel formation. Totally 12 silica xerogels with high degree of three-dimensional Si–O–Si network were synthesized. The results indicate that all the silica xerogels are composed of aggregated particles sized 20–250 nm, resulting in porous networks with specific area, pore volume, and pore diameter in the range of 290–690 m2/g, 1.54–2.40 cm3/g, and 17.4–68.2 nm, respectively. The compositional change in the recovered liquids, the drying time, and the volume of wet gel had influence on the aggregation, degree of condensation, and surface area of the cyclically synthesized xerogels. The synthesis route not only saves resources but also does not generate any waste, providing a sustainable sol−gel way to synthesize materials.

中文翻译:

二氧化硅干凝胶的溶胶-凝胶合成中使用的溶剂和催化剂的回收和再利用

丁胺(BA)的催化下,通过原硅酸四乙酯(TEOS)的水解和缩合反应合成二氧化硅干凝胶,然后在环境压力下于120°C干燥形成的湿凝胶。干燥过程中回收了湿凝胶中的溶剂(水和乙醇)和催化剂。发现回收液体中乙醇的相对百分比增加,而水和丁胺的相对百分比下降。回收的液体直接用于四次运行,然后BA,H 2的含量调节O和TEOS以保持反应物比率与第一轮相同,从而促进快速的溶胶和凝胶形成。总共合成了12种具有高度三维Si–O–Si网络的二氧化硅干凝胶。结果表明,所有二氧化硅干凝胶均由尺寸为20–250 nm的聚集颗粒组成,形成的多孔网络的比面积,孔体积和孔径在290–690 m 2 /g,1.54–2.40 cm 3范围内/ g和17.4–68.2 nm。回收液体的组成变化,干燥时间和湿凝胶的体积对环状合成干凝胶的聚集,缩合程度和表面积都有影响。合成路线不仅节省资源,而且不会产生任何浪费,为合成材料提供了可持续的溶胶-凝胶方式。
更新日期:2019-02-21
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