酚醛树脂基球形微-介双阶多孔炭的软模板法制备

Preparation of Spherical Micro-mesopore Hierarchical Carbon from Phenol-Formaldehyde via Soft Template Method

将苯酚和甲醛在碱性条件下聚合,然后在酸性条件下与软模板剂F127自组装形成中间相,经高温煅烧合成球形微-介双阶多孔炭。通过扫描电子显微镜、透射电子显微镜、氮气吸附-脱附和热重分析技术对样品进行了形貌观察和性能测试。结果表明,pH值、软模板剂用量和活化温度对样品形貌有调控作用。当软模板剂F127的质量分数为20%、pH值为0.5和活化温度为700℃时,可制备出直径为100～200 nm的球形炭,球形粒子分散均匀,排列规整,呈明显蠕虫状排列的孔隙结构,比表面积为503 m2/g,孔容积0.416 cm3/g,介孔孔径集中分布在2.9 nm,微孔主要分布在1.3 nm。随着活化温度升高,炭球的比表面积和孔容积增大,平均孔径减小。F127的热解形成介孔结构,碳前驱体高温下的径向收缩形成微孔结构。

A facile soft-template method was developed for the synthesis of spherical micro-mesoporous hierarchical carbon material（SHC） by first reacting phenol with formaldehyde under basic conditions,and then self-assembling with Pluronic F127 as the template.The surface morphology and the performance of the material were examined with the surface area and porosity measurements,scanning electron spectroscopy（SEM）,transmission electron microscope（TEM） and thermal analysis.The results showed that the morphologies of the samples were regulated by the soft-template,pH and activation temperature.The optimum conditions were determined as the following： the mass fraction for the surfactant is 20%,pH value is 0.5 and the activation temperature is 700 ℃.The prepared porous carbon under the above conditions exhibits spherical structure with a uniformly diameter of 100-200 nm and is well dispersed.Vermicular and bimodal pores of 2.9 nm and 1.3 nm were observed.The maximum surface area and the pore volume reach 503.20 m2/g and 0.42 cm3/g,respectively.The results reveal that the surface area and the pore total volume of samples increase with the increasing of activation temperature.However,the pore size of the samples shows a reverse trendency.