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1559349638

银虫 (著名写手)

[求助] 求助:经典Hummers法合成氧化石墨,最后加双氧水,怎么不变黄色?

经典Hummers法低、中、高温反应各两小时,合成氧化石墨,最后加双氧水,一直是棕色,怎么变不成想要的黄色,出错在什么地方?
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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.
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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
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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609644581

木虫 (正式写手)

【答案】应助回帖

感谢参与,应助指数 +1
是不是试剂的问题?如果一直出现不了黄色,那可能就是试剂的问题了!我有时不加双氧水就变成黄色,让我很费解!
科研男!
2楼2012-05-02 22:26:10
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BUCT帅帅

金虫 (小有名气)

【答案】应助回帖

感谢参与,应助指数 +1
我也遇到了这个问题,我之前怀疑是双氧水变质了问题,后来换了新的双氧水也不行。
我现在认为问题可能在温度控制上。主要是控制最后阶段的高温阶段,加水的时候尽量慢,不要升温太快。我同学做的没有高温阶段,最后就变黄了。详细可参考hongjie dai的文章
PEMFC
3楼2012-05-02 22:28:02
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1559349638

银虫 (著名写手)

引用回帖:
2楼: Originally posted by 609644581 at 2012-05-02 22:26:10:
是不是试剂的问题?如果一直出现不了黄色,那可能就是试剂的问题了!我有时不加双氧水就变成黄色,让我很费解!

不是试剂的问题,亲
The so-called turning-around is that u not only miss the sun in day time but also the stars at night.
4楼2012-05-02 22:32:19
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