以报废液体推进剂硝酸-27S、鳞片石墨、高锰酸钾、硫酸和冰醋酸为原料,采用化学氧化法制备高倍可膨胀石墨。考察了高锰酸钾、硝酸-27S(水吸收液)、冰醋酸用量等因素对可膨胀石墨膨胀容积的影响;通过正交实验确定最佳工艺;采用扫描电镜(SEM)和X射线衍射(XRD)对可膨胀石墨进行表征。结果表明:最佳工艺为鳞片石墨(g)∶高锰酸钾(g)∶硝酸-27S(水吸收液)(mL)∶硫酸(mL)∶冰醋酸(mL)=1∶1∶1.25∶1.25∶2,于40℃下反应90 min,所获可膨胀石墨的最大膨胀容积为320 mL.g-1;对膨胀容积影响最大的因素为KMnO4用量;SEM和XRD证实了石墨层间化合物的存在。
Highly-expandable graphite was prepared by chemical oxidization using flake graphite as the host material and waste liquid propellants of nitric-27S,potassium permanganate,sulfuric acid and acetic acid as guest compounds.Various factors influencing the volume expansion were studied,such as the amounts of potassium permanganate,nitric-27S and acetic acid.Optimum preparation conditions were obtained using orthogonal experimental design.The preparation of graphite intercalation compounds was confirmed by SEM and XRD.Results showed that the most expandable graphite with a expansion volume of 320 mL·g-1 was obtained at 40 ℃ for 90 min using flake graphite,potassium permanganate,nitric-27S,sulfuric acid and acetic acid in the following respective amounts: 1 g,1 g,1.25 mL,1.25 mL and 2 mL.The amount of potassium permanganate is the most important factor affecting the expansion volume.