利用硝酸-27S制备无硫可膨胀石墨的工艺研究

Study on Sulfur-Free Expandable Graphite Preparation Techniques by Nitric-27S

为实现报废推进剂硝酸-27S的再利用,用硝酸-27S和KMnO4做氧化剂,乙酸酐做插层剂制备无硫可膨胀石墨。考察了反应温度、反应时间以及硝酸-27S水吸收液、KMnO4、乙酸酐用量等因素对可膨胀石墨膨胀容积的影响。采用扫描电镜(SEM)和X射线衍射仪(XRD)对可膨胀石墨形貌及结构进行了表征。实验确定的最佳工艺为:m(C):m(KMnO4):V(硝酸-27S水吸收液):V(乙酸酐)=1g:1g:4mL:3mL,于25℃反应120min。所得可膨胀石墨的最大膨胀容积为220mL/g,不含硫。

In order to recycle abandoned liquid propellants of nitric-27S,sulfur-free expandable graphite was prepared using nitric-27S and reagent KMnO4 as oxidant,and（CH3CO）2O as inserting reagent.The effect of reaction temperature,reaction time,the amount of nitric-27S（absorbed in water）,KMnO4 and（CH3CO）2O on expanded volume of expanded graphite was studied.The appearance and structure of expandable graphite was characterized by SEM and XRD.Optimal preparation conditions obtained by orthogonal test were：the best ratio of m（graphite）：m（KMnO4）：V（Nitric-27S absorbed in water）：V（acetic anhydride）,1 g：1 g：4 mL：3 mL;reaction time,120 min under the temperature of 25℃.The sulfur-free product with maximum expanding volume of 220 mL/g was obtained.