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红衫骁将

木虫 (著名写手)

[求助] 铜钌负载型催化剂的防氧化问题

最近在制备Cu-Ru-载体催化剂,过滤干燥,最后用氢-氩混合气预还原催化剂后,在高压釜内反应,底物却基本没有反应,问题出现在哪里呢?(期间必然接触空气,难道能够做到不接触空气?文献中也是使用高压釜呀)求高手解决,金币有的是,你懂的

一 the solid was reduced in a flow of pure H2 at 220◦C for 3 h and then 300◦C for 3 h. The as-made catalysts were labeled as Ru-Cu/TMG-BEN.
一The reaction was  carried out in a 7 mL autoclave reactor under stirring

二 The collected sample was dried in an Ar flow(100 cm-3g-1 min-1) at 80◦C for 12 h, and then treated in a 20% H2/Ar flow (100 cm-3 g-1 min-1) at 300◦C for 1.0 h.
二 The reaction was carried out in a 100 mL stainless steel autoclave
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zyhou

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【答案】应助回帖

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感谢参与,应助指数 +1
jiangyun2: 金币+1, 谢谢回帖交流,欢迎常来~~ 2013-09-22 21:47:18
红衫骁将: 金币+20 2014-02-23 15:22:33
这里需要仔细!
先把液体在高压釜中配制好,还原的催化剂在保护气体中降温,从还原管转移到反应器时,不要关保护气,快速倒入高压釜中,
这样接触空气的机会就小很多了!
2楼2013-09-22 21:30:44
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红衫骁将

木虫 (著名写手)

引用回帖:
2楼: Originally posted by zyhou at 2013-09-22 21:30:44
这里需要仔细!
先把液体在高压釜中配制好,还原的催化剂在保护气体中降温,从还原管转移到反应器时,不要关保护气,快速倒入高压釜中,
这样接触空气的机会就小很多了!

但是从还原管拿出来总需要称质量吧?干燥后还原前质量跟还原后质量默认一样?理论上这样转移可行,但是实际操作貌似很难,从还原管拿出来必然接触空气呀
3楼2013-09-23 09:25:35
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