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644249741

银虫 (小有名气)

[求助] 【求助】重复2013年Nanoscale文献合成Fe3O4时,发现柠檬酸钠不溶于二乙二醇,怎么办? 已有2人参与

重复文献One-step synthesis of monodisperse, water-soluble ultra-small Fe3O4 nanoparticles for potential bio-application,Nanoscale, 2013, 5, 2133
文献步骤为In a typical synthesis of 3.1 nm Fe3O4 nanoparticles, anhydrous FeCl3 (4 mmol) was first vigorously mixed with 40 mL of DEG to form a clear solution. Then, Na3Cit (1.6 mmol) was added and the mixture was heated at 80 °C with stirring to form a clear solution. After dissolving anhydrous NaOAc (12.0 mmol) in the above solution, the mixture was transferred into a Teflon-lined stainless-steel autoclave (100 mL capacity) and sealed in air. Following this, the autoclave was kept at 200 °C for 6 h. After being allowed to cool naturally to room temperature, the black products were collected by centrifugation (12 000 rpm, 30 min)and washed with ethanol three times.
就是把无水氯化铁溶解于DEG中形成清液,然后加入柠檬酸钠置于80°C中水浴至澄清,最后加入乙酸钠,混合均匀转移至反应釜中200°C反应6h。。。我们实验室没有无水的氯化铁,我就用六水的来试试,结果能溶解,但是柠檬酸钠就溶解不了,80°C搅拌1h都溶解不了,超声过也没变化,加入乙酸钠后,乙酸钠溶解了一部分。。。现在应该怎么办啊?做不好第一步就没法转移进反应釜了都。。。跪求大神帮忙~~~
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bachier

金虫 (职业作家)

【答案】应助回帖

感谢参与,应助指数 +1
将柠檬酸钠溶解在水中,浓度高点,然后取水溶液加入。
2楼2015-08-14 11:35:18
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小白two

新虫 (小有名气)

【答案】应助回帖

感谢参与,应助指数 +1
我都是用乙二醇做,赵东元院士和李亚栋院士的思路都比较接近,铁盐,乙酸钠,柠檬酸钠丢进去,搅拌一个小时就差不多了
3楼2015-08-14 14:49:20
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644249741

银虫 (小有名气)

引用回帖:
3楼: Originally posted by 小白two at 2015-08-14 14:49:20
我都是用乙二醇做,赵东元院士和李亚栋院士的思路都比较接近,铁盐,乙酸钠,柠檬酸钠丢进去,搅拌一个小时就差不多了

我想问你是全部都一起丢的吗?可是文献中都是分批搅拌至均匀的啊???请问这是你的硕士毕业论文吗?有没有相类似的硕士论文参考一下的?谢谢啊~
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4楼2015-08-14 16:02:57
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