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金虫 (小有名气)

应助: 0 (幼儿园)
金币: 1067.8
散金: 4
帖子: 143
在线: 98.3小时
虫号: 729141
注册: 2009-03-23
性别: GG
专业: 应用化学

[交流] 【求助】固体酸碱双功能催化剂已有1人参与

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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