隔氧水热反应制备单分散炭微球的实验研究

Experimental study on preparation of mono-disperse carbon microspheres by oxygen isolated hydrothermal reaction

以葡萄糖为前驱物,在氮气保护氨水辅助的隔氧体系中水热合成单分散炭微球。考察了不同碳源、配料种类、氨水浓度和通氮时间对炭微球粒径分布和形貌的影响。采用SEM、BET、XRD、FT-IR、XPS、粒度仪对炭微球的形貌和成分进行表征,用差热法分析了炭微球的热稳定性。结果表明,氨水浓度与通氮气保护对炭微球的形貌与粒径分布影响显著,在0.1 g/m L葡萄糖溶液、0.05 mol/L氨水溶液和以200 cm3/min的速率通入氮气保护20 min的实验条件下,可制备出平均粒径为11.5μm且表面富含官能团—OH、CO、—COOH的单分散炭微球。

Mono-disperse carbon microspheres are hydrothermally synthesized in an oxygen isolated system protected by nitrogenous gas and assisted by aqueous ammonia,with glucose as precursor. Effects of different carbon sources,types of matching materials,concentration of aqueous ammonia and nitrogen protection time on the particle size distribution and morphology of carbon microspheres are investigated. The morphology and composition of the synthesized carbon microspheres are characterized by SEM,BET,XRD,FT-IR,XPS and particle size analyzer. Its thermogravimetric performance is analyzed by TGA. The experimental results show that both the concentration of aqueous ammonia and nitrogen protection have significant effects on morphology and particle size distribution of carbon microspheres. Monodispersed carbon microspheres with an average particle size of 11. 5 μm and abundant surface functional groups such as—OH,CO and —COOH can be obtained under conditions of 0. 1 g·m L^-1 glucose solution,0. 05 mol·L^-1 ammonia solution and under 20 min of nitrogen protection with an input rate of 200 cm3·min.