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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即使俩个数据都对 实际合成的时候也不一定能出来啊 还得自己试
超声一下的作用是让原料在刚开始的时候混合的更加好一些吧。。。影响其实并不是很大的
偶遇羊仔
,
我之前有一次合成出了MOF-235,具体就是FeCl3,bdc,然后加几滴HF就OK了
情况不一样的,文献只是提供一个可能性,做,还得自己做
请问楼主有MOF-235的电镜照片吗?为什么我合出来的东西里面太多杂质了 这是怎么回事?