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kkangle8

铁虫 (初入文坛)

[求助] 修正hummers合成氧化石墨

请各位能否帮我看下步骤是否正确  尤其是细节部分 希望能够指出并修正
1在冰水浴中装配好250ml反应瓶
2加入浓H2SO4(一般加多少ml) 搅拌下加入2g石墨粉和1g硝酸纳固体混合物
3缓慢加入6gKMnO4(温度不超过10度)
4在冰水浴条件下搅拌2h取出 室温搅拌反应5天
5将样品用H2SO4稀释 搅拌2h
6加入6mlH2O2 搅拌2h
7用H2SO4,H2O2混合物及HCl反复洗涤  用蒸馏水再洗涤  得沉淀GO
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xihuashida9682

木虫 (著名写手)

【答案】应助回帖

引用回帖:
2楼: Originally posted by javas2010 at 2011-11-10 22:01:58:
兄弟可以试试这个配方,我们实验室一直这样做的(具体的细节自己控制)
natural graphite powder (2.0 g) was added to cooled (0 ◦C)  H2SO4 (350 ml). Then, KMnO4 (20 g) and NaNO3 (3 g) were added g ...

用这个方法做的氧化石墨很难洗涤。

(1)我用离心洗涤时,先用稀盐酸洗比较容易,用去离子水洗时,越洗越粘稠,体积膨胀越厉害,颜色越深,越难沉淀,以至于最终成了糖浆,沉淀不了,难以干燥。

(2)如果改成过滤方法,请问你们怎么操作的。好像无法用普通滤纸抽滤,因为最终产物都粘在滤纸上了,而且过滤速度越来越慢;用玻璃砂芯漏斗也存在这个问题。我想改成滤膜会不会同样存在这个问题呢?滤膜的要求是什么呢?

请知情者指导,谢谢。
9楼2011-11-12 08:15:30
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javas2010

铁杆木虫 (著名写手)

【答案】应助回帖


lchpy(金币+1): thanks for your information 2011-11-11 08:13:20
兄弟可以试试这个配方,我们实验室一直这样做的(具体的细节自己控制)
natural graphite powder (2.0 g) was added to cooled (0 ◦C)  H2SO4 (350 ml). Then, KMnO4 (20 g) and NaNO3 (3 g) were added gradually while stirring. The mixture was then  transferred to a 30◦C water bath and stirred for 20 min. Deionized  water (250 ml) was slowly added and the temperature  was increased to 98 ◦C. The mixture was maintained at that  temperature for 30 min. The reaction was terminated by adding de-ionized water (500 ml) followed by adding H2O2 solution (40 ml, 30%). The color of the mixture changed to
brilliant yellow, indicating the oxidation of pristine graphite to  GO. Then, the mixture was filtered and washed with diluted HCl to remove metal ions. Finally, the product was washed repeatedly with distilled water until the pH was seven. The sample of GO was obtained after drying. To prepare the  GONS, the as-obtained GO was re-dispersed in distilled water。
含泪播种的人一定能含笑收获!
2楼2011-11-10 22:01:58
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二小小木虫

木虫 (正式写手)

引用回帖:
2楼: Originally posted by javas2010 at 2011-11-10 22:01:58:
兄弟可以试试这个配方,我们实验室一直这样做的(具体的细节自己控制)
natural graphite powder (2.0 g) was added to cooled (0 ◦C)  H2SO4 (350 ml). Then, KMnO4 (20 g) and NaNO3 (3 g) were added g ...

哥们 你们做出来的黄色很亮吗?我感觉我的没有达到亮黄那种程度
3楼2011-11-11 15:07:20
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冷月孤魂

银虫 (正式写手)

请问楼主有没有Hummers法以及改良Hummers法制GO的文献呢?能否分享一下
4楼2011-11-11 16:52:21
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