室温条件下乙腈为溶剂炭气凝胶的制备与机理分析

吴培弟|　周　斌|　杜　艾; 张志华|　吴广明|　沈　军

室温条件下乙腈为溶剂炭气凝胶的制备与机理分析

同济大学上海市特殊人工微结构材料与技术重点实验室|上海 20092

基金项目: 国家自然科学基金（51102184，51172163），国家科技支撑计划（2009BAC62B02），同济大学青年优秀人才培养行动计划（2010KJ068）和教育部博士点基金（20090072110047，20100072110054）.

详细信息

中图分类号: TQ 127.1+1
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出版历程
- 收稿日期: 2012-07-29
- 录用日期: 2013-01-05
- 修回日期: 2012-10-09
- 刊出日期: 2012-12-20

Preparation of carbon aerogels at room temperature using acetonitrile as solvent

Tongji University, Shanghai Key Laboratory of Special Artificial Microstructure Materials and Technology, Shanghai 20092, China)

Funds: National Natural Science Foundation of China(51102184,51172163),National Key Technology Research and Development Program of China(2009BAC62B02),Program for Young Excellent Talents if Tongij University (2010KJ068)and Doctoral fund of Ministry of Education of China (20090072110047, 20100072110054).

摘要

摘要: 与传统炭气凝胶制备不同，在室温条件下以乙腈为溶剂，间苯二酚和甲醛为前驱体，盐酸为催化剂，采用溶胶-凝胶、超临界干燥结合高温炭化工艺制备炭气凝胶（密度低至约50 mg·cm-3）。红外光谱、比表面积和孔径分布、扫描电子显微镜（SEM）和X射线衍射等测试表明，所制炭气凝胶是一种类石墨结构的非晶态材料，具有纳米骨架网络结构，比表面积达1 300 m2·g-1。对比不同配比气凝胶的SEM发现,气凝胶的颗粒尺寸为40 nm～70 nm。分析溶胶-凝胶过程中的温度变化和乙腈在凝胶化中作用得知,由于盐酸的催化和反应放热共同作用，实现了室温下间苯二酚和甲醛的加成和缩聚反应，并最终形成凝胶；乙腈在反应中起着一种分散剂的作用。
- 炭气凝胶 /
- 室温 /
- 乙腈 /
- 反应热
Abstract: Carbon aerogels were synthesized at room temperature by a sol-gel polymerization route using resorcinol and formaldehyde as precursors, acetonitrile as solvent and hydrochloric acid as catalyst, followed by CO2 supercritical drying and carbonization. FT-IR, SEM, XRD and nitrogen adsorption were used to characterize the microstructure of the aerogels. Results showed that the carbon aerogels are graphite-like amorphous materials with nano-skeleton networks formed by nanoparticles around 40-70 nm in diameter, whose specific surface area is up to 1 300 m2·g-1 and lowest density about 0.050 g/cm3. The heat of condensation and the catalytic action of hydrochloric acid made it possible to form gels at room temperature. The high surface area and low density of the as-prepared carbon aerogels were ascribed to a strong interaction between acetonitrile and —OH groups by hydrogen bonding.
- Carbon aerogels /
- Room temperature /
- Acetonitrile /
- Heat