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2.2. Synthesis of graphite oxide Graphite oxide was synthesized through a modified Hummers method [30] from nature graphite flake. 2 g of graphite and 1 g of NaNO3 were dissolved in 46 mL of concentrated H2SO4 under an ice bath. After about 15 min of stirring, 6 g of KMnO4 was gradually added into the suspension with stirring as slowly as possible in order to control the reaction temperature below 20 ◦C. The suspension was stirred for 2 h, and then maintained at 35 ◦C for 30 min. 92 mL of deionized water was slowly poured into the suspension,resulting in a quick increase in temperature, and the temperature should be controlled lower than 98 ◦C. After 15 min, the suspension was then further diluted to approximately 280 mL with warm deionized water. 20 mL of 30% H2O2 was added for the purpose of removing the residual KMnO4 and MnO2 to change the color into luminous yellow. Then, the suspension was filtered and washed with warm 5% HCl aqueous solution and deionized water, respectively, until no sulfates were detected and the pH of the filtrate was adjusted to 7. The sample of graphite oxide was dried under vacuum at 50 ◦C to a constant weight, and then milled to an ideal particle size. |
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2.2 氧化石墨的合成 通过改良Hummers法利用天然石墨合成氧化石墨。冰浴条件下，将2g石墨和1g NaNO3溶解到46ml浓硫酸中，经过大约15min搅拌，6g KMnO4逐渐加入到悬浮液中，同时尽可能慢搅拌控制反应温度在20°C以下。悬浮液搅拌2h.然后在35°C下保持30min。92ml去离子水缓慢倒入悬浮液导致温度快速上升，温度应控制在98°C以下。经过15min，用温的去离子水将悬浮液进一步稀释到大约280ml。加入20ml 30％H2O2去除残留的KMmO4和MnO2，改变颜色至明亮的黄色。然后过滤悬浮液，用温5％HCl水溶液和去离子水清洗。相对来说，直到检测不出硫酸盐，滤出液PH大约为7。将氧化石墨样品在50°C真空条件下干燥至恒重，然后研磨至理想颗粒大小。 [ 发自手机版 https://muchong.com/3g ] |
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3楼2015-03-03 21:32:11
