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以内蒙古固定碳质量分数为98.86%的天然鳞片石墨为原料,高锰酸钾、硝酸与高氯酸的混酸为氧化插层剂,采用化学氧化法直接插层制备可膨胀石墨。探究混酸配比(质量比)及用量、高锰酸钾质量分数、反应温度、反应时间等因素对可膨胀石墨膨化效果的影响。最佳制备工艺条件为:m(石墨)∶m(高锰酸钾)∶m(混酸)为1∶0.10∶4.5,混酸中硝酸的质量分数为8%,反应温度为40℃,反应时间为45 min,此条件下制得的可膨胀石墨的膨胀容积为410 m L/g。各阶段产物的XRD、FTIR、SEM分析表明,插层后碳层边缘呈现卷曲、张裂和剥离,层间距增大,膨胀后形成独特的“微胞”蠕虫状、贯通柳叶状、不规则多边形的三级孔隙结构。
In this paper, natural flake graphite with a fixed carbon content of 98.86% in Inner Mongolia was used as raw material, mixed acid of potassium permanganate, nitric acid and perchloric acid was used as the oxidative intercalation agent, and the expandable graphite was directly intercalated by chemical oxidation. The effects of mixed acid ratio (mass ratio) and dosage, potassium permanganate mass fraction, reaction temperature and reaction time on the puffing effect of expandable graphite were investigated. The optimal preparation conditions were as follows: m (graphite): m (potassium permanganate): m (mixed acid) 1: 0.10: 4.5; the mass fraction of nitric acid in the mixed acid was 8%; the reaction temperature was 40 ℃; the reaction time was 45 min, the expanded volume of expandable graphite prepared under this condition is 410 m L / g. The results of XRD, FTIR and SEM of the products at different stages show that the edge of the carbon layer is curly, cracked and peeled off after intercalation, and the interlayer spacing increases. After expansion, the unique “micelles” worm- Three-level pore structure of irregular polygons.