两篇文献合成MOF-235方法不一样?
文献1:
For synthesis of MOF-235 at first, 0.2 g of terephthalic acid and 0.205 g of FeCl3·6H2O were dissolved in 60 mL of N,N-dimethylformamide (DMF) and then 2 mL of the reaction solution and 2 mL of ethanol transferred into a Teflon-lined autoclave and heated at 358 K for 24 h. The orange crystals were washed with DMF/ethanol mixture and dried.
参考文献:Sorption of methane, hydrogen and carbon dioxide on metal-organic framework, iron terephthalate (MOF-235) ;Journal of Industrial and Engineering Chemistry 18 (2012) 1149–1152
文献2:
An exact amount of terephthalic acid (0.205 g, 1.23 mmol; Sigma–Aldrich, 98%) was mixed with 60 mL of DMF (DC Chem., 99%). Then the mixture was stirred
for 10 min till a clear solution was formed. After that FeCl3·6H2O (0.200 g, 0.738 mmol; Duksan, 99.7%) was added into the solution and stirred for 5 min. The reactant mixture of 30 mL and 30 mL of ethanol (DC Chem., 96%) were loaded into a Teflon-lined autoclave, sealed and placed in a preheated electric oven (80C) for 1 day. Orange powder of MOF-235 was collected by centrifugation and was washed with a DMF/ethanol mixture at least three times. Then the product was dried overnight at 150 ◦C to remove DMF and then stored in a glass vial.
参考文献:Adsorptive removal of methyl orange and methylene blue from aqueous solution with a metal-organic framework material, iron terephthalate (MOF-235);Journal of Hazardous Materials185 (2011) 507–511
区别:
对苯二甲酸的用量不一样,一个是0.2g;另一个是0.205g。
FeCl3·6H2O 也不一样,一个是0.205g;另一个是0.2g。
加入顺序不一样,一个是先后顺序加入;另一个是混合全部加入。
最后烘干方式不一样,一个是自然烘干;另一个是加热烘干。
才疏学浅 不知道哪种才是正确的
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[ Last edited by TonyGeN on 2013-10-16 at 19:29 ]
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你按照两种原料的分子量的比来算一下需要多少质量吧,其实相差0.005g可以忽略的。
加入先后顺序在这里并不重要,因为都是要烧釜的。你喜欢的话还可以先将反应液超声一下。
至于烘干的方法,只要结构不坏的话,怎么样都可以,
好奇LZ合成这个干嘛用
吸附MB?
两者相差不大,有时候MOF的合成方法会稍有变化,结构不会变化。
比照文献合成没多大意义,大部分是粗粗写的,有些细节也是有所保留。比例问题只能靠你自已去实验了。这个就是大家经常讨论的参考文献无法重复的问题,其实很正常的
恩恩 同意楼上意见