兩篇文獻合成MOF-235方法不一樣?
文獻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.
參考文獻: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
文獻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.
參考文獻: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
區(qū)別:
對苯二甲酸的用量不一樣,一個是0.2g;另一個是0.205g。
FeCl3·6H2O 也不一樣,一個是0.205g;另一個是0.2g。
加入順序不一樣,一個是先后順序加入;另一個是混合全部加入。
最后烘干方式不一樣,一個是自然烘干;另一個是加熱烘干。
才疏學(xué)淺 不知道哪種才是正確的
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[ Last edited by TonyGeN on 2013-10-16 at 19:29 ]
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即使倆個數(shù)據(jù)都對 實際合成的時候也不一定能出來啊 還得自己試
超聲一下的作用是讓原料在剛開始的時候混合的更加好一些吧。。。影響其實并不是很大的
偶遇羊仔
,
我之前有一次合成出了MOF-235,具體就是FeCl3,bdc,然后加幾滴HF就OK了
情況不一樣的,文獻只是提供一個可能性,做,還得自己做
請問樓主有MOF-235的電鏡照片嗎?為什么我合出來的東西里面太多雜質(zhì)了 這是怎么回事?