以75μm天然鳞片石墨为原料、HClO4-CH3 COOH混合酸为电解液,采用电化学法制备可膨胀石墨。通过单因素实验分析影响因素对石墨膨胀容积的影响,并对制得的可膨胀石墨和膨胀石墨的形貌、结构进行SEM和XRD表征,以及含硫量测定。结果表明：无硫可膨胀石墨的最佳制备条件为：石墨(g)与电解液(mL)配比1∶7,HClO4(mL)与CH3COOH(mL)体积比4∶1,电流密度0.06 A/cm2,反应温度20℃,反应时间60 min,电解液质量分数70%。制得无硫可膨胀石墨的膨胀容积为150 mL/g。该研究为无硫可膨胀石墨的制备提供了一种途径。%This paper is devoted to an experimental study on the preparation of the sulfur-free ex-pandable graphite using HClO4 and CH3 COOH as electrolyte, the 75 μm natural flake graphite as raw material and employing electrochemical method. The study involves analyzing the influence factors on the expansion volume( EV) by single factor experiments and characterizing the morphology and structure of expandable graphite and expanded graphite by SEM and XRD, and determining the content of sulfur. The study suggests that the optimum preparation conditions for sulfur-free expandable graphite are: graphite (g)∶electrolyte(mL) =1∶7, HClO4(mL)∶CH3COOH(mL) =4∶1,current density of 0. 06 A/cm2,reac-tion temperature of 20 ℃, reaction time of 60 min, the concentration of mixed acid of 70%, and the maximum EV of up to 150 mL/g. The study provides a way for the preparation of sulfur free and expand-able graphite.
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