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07231210

金虫 (小有名气)

[求助] Improved Synthesis of Graphene Oxide制备氧化石墨烯,急求 已有1人参与

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有没有人用Improved Synthesis of Graphene Oxide做过实验啊,需不需要用冰浴加料啊,急急急!万分感谢!
For the improved method, a 9:1 mixture of concentrated H2SO4/H3PO4 (360:40 mL) was added to a mixture of graphite flakes (3.0 g, 1 wt equiv) and KMnO4 (18.0 g, 6 wt equiv), producing a slight exotherm to 35_40 °C. The reaction was then heated
to 50 °C and stirred for 12 h. The reaction was cooled to rt and poured onto ice (_400 mL) with 30% H2O2 (3 mL). For workup, the mixture was sifted through a metal U.S. Standard testing sieve (W.S. Tyler, 300 _m) and then filtered through polyester fiber (Carpenter Co.) The filtrate was centrifuged (4000 rpm for 4 h), and the supernatant was decanted away. The remaining solid material was then washed in succession with 200 mL of water, 200 mL of 30% HCl, and 200 mL of ethanol (2_); for each wash, the mixture was sifted through the U.S. Standard testing sieve and then filtered through polyester fiber with the filtrate being centrifuged (4000 rpm for 4 h) and the supernatant decanted away. The material remaining after this extended,
multiple-wash process was coagulated with 200 mL of ether, and the resulting suspension was filtered over a PTFE membrane with a 0.45 _m pore size. The solid obtained on the filter was vacuum-dried overnight at room temperature, obtaining 5.8 g of product.
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xiejf

专家顾问 (文学泰斗)

麦麦爸爸爱小牛

【答案】应助回帖

★ ★
感谢参与,应助指数 +1
07231210: 金币+2, 有帮助 2012-09-19 09:30:14
不需要用冰浴,加双氧水前可以加入适量的冰水稀释浓酸。
麦麦爸爸爱小牛
2楼2012-09-18 20:42:56
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07231210

金虫 (小有名气)

引用回帖:
2楼: Originally posted by xiejf at 2012-09-18 20:42:56
不需要用冰浴,加双氧水前可以加入适量的冰水稀释浓酸。

用这种方法做出来的效果好吗
3楼2012-09-19 08:23:33
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xiejf

专家顾问 (文学泰斗)

麦麦爸爸爱小牛

引用回帖:
3楼: Originally posted by 07231210 at 2012-09-19 08:23:33
用这种方法做出来的效果好吗...

反正我是这么做的
麦麦爸爸爱小牛
4楼2012-09-19 09:03:07
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mjj1215

金虫 (初入文坛)

楼主加完双氧水之后你是怎么处理的,下面的处理感觉很麻烦,能直接酸洗在水洗处理吗
5楼2012-10-16 16:06:58
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华莎

新虫 (初入文坛)

【答案】应助回帖

用的这种方法做的,得到了亮黄色的溶液,5000转离心就能差不多,真空干燥后,测XRD,在10左右的衍射峰不强,比硅片的峰高不了多少,是没烘干吗?
6楼2018-11-14 12:51:43
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