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【求助】 ATRP加样顺序有讲究吗?
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我是先把CuBr, HMTETA,和溶剂加进去，freeze-vaccum-thaw三次，溶液变成蓝色，然后在氮气保护下打开橡皮塞加入引发剂粉末，在freeze下针入单体，再freeze-vaccum-thaw三次，氮气下升温反应。 貌似溶液几个小时后变得很粘，有绿色不溶颗粒。可是GPC测不到有效信号。 请各位ATRP高手指导一下。看看有什么问题，怎么改进。 [ Last edited by wellok101 on 2008-11-20 at 21:30 ] |
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2楼2008-11-20 13:07:54
3楼2008-11-20 13:17:01
striveme
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4楼2008-11-21 13:36:33
5楼2008-11-21 13:51:34
| In principle, the compounds should be added as following order: monomer, solvent (dissolving and degasing), initiator (degasing), catalyst (degasing), and then finally the ligand (degasing at least three times). Without ligand the reaction will not start, therefore, you are safe to add it at the latest step. I'm sure you are going to succeed if you follow this. The particles you observed during the polymerization is a bad sign, which normally suggests the polymerization fail. Good luck! |
6楼2008-11-21 14:23:09
7楼2008-11-21 21:07:05
xbhchina
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8楼2008-11-22 11:50:59
9楼2008-11-22 16:33:54
10楼2008-12-03 18:39:50