PREPARATION OF GRAPHITIC OXIDE
PREPARATION OF GRAPHITIC OXIDE
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DOI：
10.1021/ja01539a017
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发表时间：
1958-01-01
影响因子：
15
通讯作者：
OFFEMAN, RE
中科院分区：
文献类型：
--
作者：
HUMMERS, WS;OFFEMAN, RE
石墨氧化物，有时称为石墨酸，已经被人们所知几乎有世纪了。1859年，布罗迪（Brodie）首先用氯酸钾和发烟硝酸组成的氧化混合物反复处理锡兰石墨制得。从那时起，已经设计了许多其他的方法来形成石墨氧化物，几乎所有的都依赖于含有一种或多种浓酸和氧化材料的强氧化混合物。3-6目前最常用的方法是最初的Brodie合成法和Staudenmaier描述的一种方法，其中石墨在浓硫酸和硝酸中用氯酸钾氧化。该领域最近的工作人员，如Hofmann和Frenzel 5和Hamdi 7，使用Staudenmaier方法发现该过程耗时且危险。Stauden-maier-Hofmann-Hamdi法是在浓硫酸、浓硝酸（63%）和石墨的混合物中加入氯酸钾。将氯酸钾缓慢并小心地搅拌到混合物中，历时一周，同时冷却。放出的二氧化氯用惰性气体如二氧化碳或氮气除去。该过程需要超过10 g。在本方法中，石墨氧化成氧化石墨是通过用浓硫酸、硝酸钠和高锰酸钾的基本上无水的混合物处理石墨来完成的。在45 ℃以下的温度下，整个过程需要不到两个小时的时间完成，并且可以安全地进行，只要在遵守温度限制方面保持合理的注意。
Graphitic oxide, sometimes called graphitic acid, has been known for almost a century. It* was first prepared by Brodie2 34in 1859 by repeated treatment of Ceylongraphite with an oxidation mixture consisting of potassium chlorateand fum-ing nitric acid. Since then, many other procedures have been devised for forming graphitic oxide, nearly all dependent upon strong oxidizing mix-tures containing one or more concentrated acids and oxidizing materials. 3-6 The methods most commonly used at the pres-ent time are the original Brodie synthesis and one described by Staudenmaier, 6 in which the graphite is oxidized in concentrated sulfuric and nitric acids with potassium chlorate. Recent workers in the field such as Hofmann and Frenzel5 and Hamdi7 using the Staudenmaier method found the process time consuming and hazardous. The Stauden-maier-Hofmann-Hamdi method involved the ad-dition of potassium chlorate to a mixture of con-centrated sulfuric acid, concentrated (63%) nitric acid and graphite. The potassium chlorate was stirred slowlyand carefully into the mixture over a period of one week with cooling. The chlorine dioxide evolved was removed with an inert gas such as carbon dioxide or nitrogen. The process required more than 10 g. of potassium chlorate for each gram oftreated graphite and explosion was a constant hazard.In the present method, 8 the oxidation of graphite to graphitic oxide is accomplished by treating graphite with essentially a water-free mixture of concentrated sulfuric acid, sodium nitrate and potassium permanganate. The entire process re-quires less than two hours for completion at tem-peratures below 45 and can be carried out safely providing reasonable care is maintained in observing the temperature limitations.