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【请教】 大家说说这句英文实验时具体该怎么操作?ATRP聚合!!!
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The mixture was stirred for 10 min and then degassed by three freeze-pump-thawcycles. The flask was placed in a water bath maintained at 25℃ , Finally, p-TsCl (0.0076 g, 0.040 mmol) was added. ATRP聚合时,三次冷冻-解冻循环后,如何将固体的引发剂顺利加入又不带入空气? 我试过配成溶液,除氧后注入,用乙醇溶解的p-TsCl ,结果引发不了 大家帮我分析一下,谢谢啦 [ Last edited by wellok101 on 2008-3-13 at 14:31 ] |
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A typical polymerization is described. CuCl (0.0119 g, 0.120 mmol) was added to a dry 50 mL Schlenk flask with a magnetic stirring bar, and the Schlenk flask was evacuated and flushed with argon. Distilled DMAEMA (21.0 mL, 125 mmol), HMTETA (0.0326 mL, 0.120 mmol), degassed methanol (13.0 mL) and distilled water (2.0 mL) were added to the Schlenk flask using degassed syringes. The mixture was stirred for 10 min and then degassed by three freeze-pumpthaw cycles. The flask was placed in a water bath maintained at 25G0.2 8C. Finally, p-TsCl (0.0076 g, 0.040 mmol) was added. The reaction mixture was stirred for 10 h. The polymerization was terminated by exposing the reaction vessel to air and 10 mL of THF was added. The solution was passed through a basic alumina column and eluted with additional 100 mL of THF. The volume of the solution was reduced using a rotary evaporator and the concentrated solution was poured into hexane for precipitation, yielding a polymer with Mn,GPCZ410,000, PDIZ1.18 and 81% monomer conversion. |
2楼2008-03-13 02:44:56
3楼2008-03-13 08:40:07
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4楼2008-03-13 14:20:08