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小木虫论坛-学术科研互动平台 » 材料区 » 微米和纳米 » 合成表征 » 求助：经典Hummers法合成氧化石墨，最后加双氧水，怎么不变黄色？
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396533450

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猫咪宝贝

【答案】应助回帖

感谢参与，应助指数 +1
加双氧水是停止水浴之后，迅速加进去的，反应很迅速，立马就变金黄色了！
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11楼2012-05-04 09:23:14
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swllover

铁杆木虫 (著名写手)

【答案】应助回帖

感谢参与，应助指数 +1
The Hummers method with minor modification was used for the preparation of GOs from graphite. Briefly, to the concentrated H2SO4(10 mL) in a flask at 80 °C were added (NH4)2S2O8 (0.9 g) and P2O5(0.9 g), and the mixture was stirred until the reagents were completely dissolved. Graphite (1 g) was added, and the resulting mixture was allowed to react at 80 °C for 4.5 h. Upon being cooled to room temperature, the reaction mixture was diluted with water (250 mL) and kept for ∼12 h. It was then filtered and washed repeatedly with water, followed by drying in a vacuum oven. The solid sample was added to concentrated H2SO4 (40 mL) in a flask cooled in an ice bath. To the mixture in the flask was added slowly KMnO4(5 g over 40 min), during which the temperature was kept at <10 °C. The resulting mixture, with a change in color from black to greenish-brown, was heated at 35 °C for 2 h, followed by dilution with water (85 mL; Caution!the temperature must be kept at <35 °C throughout!) and further stirring for 2 h. The reaction mixture was poured into a large
beaker, to which water (250 mL) and then aqueous H2O2
(30%,10 mL) were added. Bubbles from the aqueous mixture along with a color change to brilliant yellow were observed. The mixture was allowed to settle for ∼12 h. The clear supernatant was decanted, and the sediment was washed repeatedly with an aqueous H2SO4 (5 wt %), H2O2(0.5 wt %), and HCl (10 wt%) solution, followed by washing repeatedly with water until no layers were observed in the centrifugation. The sample was then dialyzed (MWCO ∼ 3500) against water for 7 days to yield a clean aqueous dispersion of GOs
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不必遗憾。若是美好，叫做精彩。若是糟糕，叫做经历。
12楼2012-05-04 20:55:47
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1559349638

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12楼: Originally posted by swllover at 2012-05-04 20:55:47:
The Hummers method with minor modification was used for the preparation of GOs from graphite. Briefly, to the concentrated H2SO4(10 mL) in a flask at 80 °C were added (NH4)2S2O8 (0.9 g) and P2O5(0 ...

thank you!如题，我问的是经典的，不是改进的！氧化石墨可以合成完全没有问题，但是要用经典的HUMMER法。
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The so-called turning-around is that u not only miss the sun in day time but also the stars at night.
13楼2012-05-04 23:28:28
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