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282347421金虫 (小有名气)
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[交流]
【求助】固体酸碱双功能催化剂 已有1人参与
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2.1. “One-pot” catalyst synthesis Siloxane starting materials were purchased from Gelest. Tri- block copolymer poly(ethylene glycol)-block-poly(propylene glycol)-block-poly(ethylene glycol) P123 (4.0 g, 0.688 mmol, Mn 5800) was weighed into a Teflon bottle. Then 2.0 M HCl (120.0 mL, 240.0 mmol) and H2O (6.0 mL, 333.0 mmol) were added and stirred at 40 ◦C until the P123 was fully dis- solved. TEOS (8.2 mL, 37.8 mmol) was then added to the reaction, and the mixture was stirred at 40 ◦C for another 45 min prehydrolysis time. Then 2-(4-chlorosulfonylphenyl)- ethyltrimethoxysilane (0.65 g, 50/50 w/w solution in dichloro- methane, 1.0 mmol) was added, to allow for hydrolysis of the sulfonyl chloride, followed by 3-aminopropyltrimethoxysilane (0.19 mL, 1.0 mmol). The respective acid component was sub- stituted for the sulfonyl chloride for different acid functional- izations. This mixture was stirred at 40 ◦C for 20 h, then aged at 100 ◦C for 24 h. The mixture was then cooled to room temper- ature, and the resulting solid was filtered and rinsed repeatedly with excess H2O (4 × 500 mL), then allowed to dry overnight on an aspirating filter. The dried solid was then extracted with EtOH (400 mL per g) by refluxing in EtOH for 24 h to remove P123. The solid was again filtered and rinsed repeatedly with EtOH (4 × 500 mL), then dried overnight on the aspirator to obtain a dry white solid, which was further dried at 80 ◦C under vacuum for 24 h. 大家帮忙解答一下，上述为一篇固体酸碱双功能催化剂的制备方法，想请教一下，他是在酸性情况下制备的，那么最后表面的碱性胺应该会被“质子”化，那么怎么去质子化，是不是用过量的水冲洗就可以了？ |
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2楼2010-04-23 23:36:32
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