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sunshaokai

金虫 (正式写手)

[求助] 求助!柠檬酸三纳在乙二醇中不溶解啊?怎么办! 已有1人参与

参考赵东元 Angew. Chem. Int. Ed. 2009, 48, 5875-5879.
实验步骤:Typically, FeCl3 (0.65 g, 4.0 mmol) and trisodium citrate (0.20 g, 0.68 mmol) were first dissolved in ethylene glycol (20 mL), afterward, NaAc (1.20 g) was added with stirring. The mixture was stirred vigorously for 30 min and then sealed in a Teflon-lined stainless-steel autoclave (50 mL capacity). The autoclave was heated at 200 °C and maintained for 10 h, and then allowed to cool to room temperature. The black products were washed with ethanol and deioned water for several times.

和另外一篇文献One-step synthesis of monodisperse, water-soluble ultra-small Fe3O4 nanoparticles for potential bio-application. Nanoscale 2013, 5, 2133-2141.
实验步骤: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.

制备水溶性Fe3O4,发现柠檬酸三纳在EG(乙二醇)或者DEG(二乙二醇)中很难溶解啊,无论是超声还是加热,都是一个个小晶体颗粒沉在容器底部,大家有做过的吗?都是怎么溶解比较好呢?非常感谢!

[ Last edited by sunshaokai on 2013-6-18 at 13:38 ]
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sunshaokai

金虫 (正式写手)

引用回帖:
5楼: Originally posted by dabaoxf1 at 2013-12-23 22:05:12
请问,你们 这个问题最终怎么解决的?

解决了,80℃水浴加热0.5h,溶解的很好。
6楼2013-12-24 14:29:51
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sp2286770

至尊木虫 (职业作家)

坚忍的完美主义者

【答案】应助回帖

感谢参与,应助指数 +1
那是个盐,不好溶解,但是是水热法啊,加热到沸点以上的,那时候溶剂性质变化很大,所以不溶解没关系,室温肯定不好溶。
2楼2013-06-18 13:42:45
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sunshaokai

金虫 (正式写手)

引用回帖:
2楼: Originally posted by sp2286770 at 2013-06-18 13:42:45
那是个盐,不好溶解,但是是水热法啊,加热到沸点以上的,那时候溶剂性质变化很大,所以不溶解没关系,室温肯定不好溶。

谢谢回复!但是文献中都是说得到澄清溶液后开始水热合成,而且不溶解的话,溶液不均匀,可能会导致晶体生长的不均匀。。。
3楼2013-06-18 14:18:48
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sp2286770

至尊木虫 (职业作家)

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【答案】应助回帖

★ ★
sunshaokai: 金币+2, 有帮助 2013-06-18 14:48:13
水可以溶解,乙醇也可以的。加点试试?
4楼2013-06-18 14:42:24
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