兩篇文獻(xiàn)合成MOF-235方法不一樣?
文獻(xiàn)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(xiàn):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(xiàn)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(xiàn):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(duì)苯二甲酸的用量不一樣,一個(gè)是0.2g;另一個(gè)是0.205g。
FeCl3·6H2O 也不一樣,一個(gè)是0.205g;另一個(gè)是0.2g。
加入順序不一樣,一個(gè)是先后順序加入;另一個(gè)是混合全部加入。
最后烘干方式不一樣,一個(gè)是自然烘干;另一個(gè)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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你按照兩種原料的分子量的比來(lái)算一下需要多少質(zhì)量吧,其實(shí)相差0.005g可以忽略的。
加入先后順序在這里并不重要,因?yàn)槎际且獰。你喜歡的話還可以先將反應(yīng)液超聲一下。
至于烘干的方法,只要結(jié)構(gòu)不壞的話,怎么樣都可以,
好奇LZ合成這個(gè)干嘛用
吸附MB?
兩者相差不大,有時(shí)候MOF的合成方法會(huì)稍有變化,結(jié)構(gòu)不會(huì)變化。
比照文獻(xiàn)合成沒(méi)多大意義,大部分是粗粗寫(xiě)的,有些細(xì)節(jié)也是有所保留。比例問(wèn)題只能靠你自已去實(shí)驗(yàn)了。這個(gè)就是大家經(jīng)常討論的參考文獻(xiàn)無(wú)法重復(fù)的問(wèn)題,其實(shí)很正常的
恩恩 同意樓上意見(jiàn)