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中科院金属所新突破 氧化石墨烯实现绿色制备
发布时间:2020-08-06    文章来源:    浏览次数:732

中科院金属所新突破 氧化石墨烯实现绿色制备


氧化石墨烯是一种重要的石墨烯衍生物,最初主要作为宏量制备石墨烯的前驱体,近年来由于其不同于石墨烯的诸多独特物理化学性质和广阔应用前景而越来越受到人们的重视。最近,金属所沈阳材料科学国家研究中心先进炭材料研究部提出了一种电解水氧化的新方法,打破了150多年来通过强氧化剂对石墨进行氧化的传统思路,实现了氧化石墨烯的安全、绿色、超快制备。该成果于1月10日在Nature Communications上在线发表。



氧化石墨烯由于存在大量的含氧官能团,在水中具有良好的分散性,且易于组装和功能化,因此已被广泛用于制备多功能分离膜、高导高强纤维、超轻超弹性气凝胶等多种功能材料,并且在电化学储能、催化、生物医药、复合材料等方面表现出良好应用前景。



据介绍,中科院金属研究所的研发人员是在浓硫酸中将石墨插层,然后在稀硫酸中对插层石墨进行氧化。氧同位素示踪和自由基捕获实验表明,氧化石墨烯中的氧元素主要来源于电解液中的水,电解水产生的大量高活性氧自由基与石墨反应生成了氧化石墨烯。反应中硫酸几乎没有损耗,也不生成其它物质,可被重复用于电化学反应。该方法有效解决了氧化石墨烯制备长期面临的爆炸危险、环境污染及反应周期长的问题,有望大幅降低制备成本,有利于氧化石墨烯的工业化应用。



目前,氧化石墨烯主要是通过剥离氧化石墨来进行制备。而氧化石墨的制备迄今已有150多年的历史,无论是最早的Brodie方法(1859年),还是后来发展起来的Staudenmaier和 Hummers方法,都是基于石墨与大量浓硝酸、浓硫酸、高锰酸钾等复合强氧化剂的反应来实现,不仅存在爆炸的风险,而且污染严重,反应周期长。以目前最常用的Hummers方法为例,氧化剂由浓硫酸和高锰酸钾构成,其与石墨的典型物料比(质量比)为40:3:1(浓硫酸:高锰酸钾:石墨),反应最终会产生超过1000质量单位的酸性废水。并且,高活性的Mn2O7中间产物在高温下可能会发生爆炸,而氧化反应的完成需要数小时到上百小时






Graphene oxide has been widely used in the preparation of multifunctional separation membranes, high conductivity high strength fibers, ultra light super elastic aerogels and other functional materials because of its good dispersibility, easy assembly and functionalization in water. Due to its large number of oxygen-containing functional groups, it has good application prospects in electrochemistry, energy storage, catalysis, biomedicine, and composite materials.





According to reports, the R & D personnel of the Institute of metals, Chinese Academy of Sciences, intercalated graphite in concentrated sulfuric acid, and then oxidized the intercalated graphite in dilute sulfuric acid. Oxygen isotope tracing and free radical trapping experiments show that the oxygen element in graphene oxide mainly comes from water in electrolyte, and a large number of highly active oxygen radicals produced by electrolyzed water react with graphite to form graphene oxide. In the reaction, sulfuric acid has almost no loss and no other substances are generated, so it can be used repeatedly in electrochemical reaction. This method can effectively solve the problems of explosion hazard, environmental pollution and long reaction period in the preparation of graphene oxide, which is expected to greatly reduce the preparation cost and is conducive to the industrial application of graphene oxide.





At present, graphene oxide is mainly prepared by stripping graphite oxide. The preparation of graphite oxide has a history of more than 150 years. The earliest Brodie method (1859) or the staudenmaier and Hummers methods developed later are based on the reaction of graphite with a large number of strong oxidants such as concentrated nitric acid, concentrated sulfuric acid, potassium permanganate, etc., which not only has the risk of explosion, but also has serious pollution and long reaction cycle. Taking Hummers method as an example, the oxidant is composed of concentrated sulfuric acid and potassium permanganate, and the typical material ratio (mass ratio) of the oxidant to graphite is 40:3:1 (concentrated sulfuric acid: potassium permanganate: graphite), and the reaction will eventually produce more than 1000 units of acid wastewater. Moreover, the highly active mn2o7 intermediate may explode at high temperature, and the oxidation reaction takes several hours to hundreds of hours

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