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yxy1014169

银虫 (小有名气)

[交流] 制备MCM-41模版剂去除问题。

制备MCM-41模版剂去除的方法有哪些?一般常用的就是在马弗炉中煅烧,以前记得看过用什么萃取的方法的,但是文献找不到了。有知道这方面的朋友能不能来交流一下。有相关的文献上传上来最好,谢谢!
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xhtangxh

木虫 (著名写手)

有木有虫

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nxl5096224(金币+5,VIP+0):多谢应助哈!
除了焙烧方式,可以参考以下文献(处理对象不一定是MCM-41,但有借鉴意义):

Isothermal template removal from MCM-41 in hydrogen flow
Microporous Mesoporous Mater., 2007, 98(1-3): 242-248

Simple removal of oligomeric surfactants and triblock copolymers from mesostructured precursors of ordered mesoporous aluminum organophosphonates
Microporous Mesoporous Mater., 2007, 101(1-2): 207-213

Removal of organic templates from mesoporous SBA-15 at room temperature using UV/dilute H2O2
Microporous Mesoporous Mater., 2006, 96(1-3): 413-418

Low temperature oxidative template removal from SBA-15 using MnO(4)(-)solution and carbon replication of the mesoporous silica product
J. Mater. Chem., 2006, 16(33): 3396-3401

Crystalline-like molecularly ordered mesoporous aluminosilicates derived from aluminosilica-surfactant mesophases via benign template removal
J. Phys. Chem. B, 2006, 110(18): 9122-9131

Influence of the extraction methods to remove organic templates from Al-MCM-41 molecular sieves
Mater. Chem. Phys., 2005, 93(1): 133-137

Extraction of cationic surfactant templates from mesoporous materials by CH3OH-modified CO2 supercritical fluid
TALANTA 2005, 66(4): 943-951

High quality mesoporous materials prepared by supercritical fluid extraction: effect of curing treatment on their structural stability
Microporous Mesoporous Mater., 2005, 80(1-3): 157-163

Preparation of supported mesoporous thin films concerning template removal by supercritical fluid extraction
LANGMUIR 2005, 21(4): 1171-1174

Non-thermal calcination by ultraviolet irradiation in the synthesis of microporous materials
Microporous Mesoporous Mater., 2004, 76(1-3): 17-22

Mild methods for removing organic templates from inorganic host materials
Angew. Chem.-Int. Ed., 2004, 43(30): 3878-3880

Structural consequences of mild oxidative template removal in the synthesis of modified MCM-41 silicates
J. Mol. Structure, 2003, 651: 323-330

Vacuum removal of the template in MCM-41 silica studied by the positron annihilation method
J. Colloid Interface Sci., 2003, 262(2): 466-473

Novel method for soft template removal in the synthesis of MCM-41 mesoporous materials
Solid State Phenomena, 2003, 90-91: 79-84

In situ surfactant removal from MCM-type mesostructures by ozone treatment
J. Mater. Chem., 2001, 11(2): 589-593

Simultaneous modification of mesopores and extraction of template molecules from MCM-41 with trialkylchlorosilanes
Chem. Commun., 1999, (23): 2373-2374

Novel methods for the synthesis of MCM-41 mesoporous molecular sieves and the recovery of template
ACTA PHYSICO-CHIMICA SINICA, 1999, 15(4): 333-337

Supercritical fluid extraction of surfactant template from MCM-41
Chem. Commun., 1998, (13): 1407-1408

Effect of methanol concentration on CTAB micellization and on the formation of surfactant-templated silica (STS)
Chem. Mater., 1998, 10(6): 1490-1500

文献自己找好了,恕不提供。
2楼2007-09-20 19:26:27
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changqw

捐助贵宾 (正式写手)

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nxl5096224(金币+3,VIP+0):谢谢应助咯!
制备介孔材料脱出模板的方法主要有焙烧法和萃取两种。
下面介绍一下两种方法的适用范围:
焙烧法:适用于制备介孔硅铝酸盐,比如说你说到的MCM-41,采用焙烧法比溶剂萃取的方法更好,因为焙烧有利于使介孔材料进一步缩合,从而提高介孔材料的稳定性,尤其是热稳定性。但焙烧温度不能过高,若太高会导致介孔结构坍塌。
萃取法:主要适用于制备那些具有较高结晶度的介孔氧化物材料(如氧化铁等),这些材料如果用超分子模板和聚合物模板制备时,焙烧很容易导致介孔结构的坍塌。
至于文献,我毕业快几个月 了,没有带来,不过记得1992年nature和J.Am.Chem.Soc上各有一篇,这两篇文献是最经典的两篇制备介孔材料的文章,其中就涉及到MCM-41和MCM-48。
也许你在看关于介孔材料的中文文献时,你会看到"自从1992年,——————“,去找来看看吧,1992年的这两篇文章是介孔材料发展的里程碑。

[ Last edited by changqw on 2007-9-20 at 22:10 ]
3楼2007-09-20 22:06:03
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yxy1014169

银虫 (小有名气)

非常感谢楼上两位的热心回答,谢谢!~
4楼2007-09-20 23:48:37
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physchemboy

银虫 (小有名气)

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rabbit7708(金币+2,VIP+0):谢谢补充,辛苦了!:)
我想就3楼的答复补充一下。重要方法有两种,焙烧和乙醇脱洗。我想补充说明的就是焙烧后硅基的表面羟基会很少,而乙醇脱洗则硅基表面含有较多的表面羟基,这些羟基对介孔材料的表面官能团化至关重要。如果你是想制备MCM-41后使其官能团化,那就得考虑考虑了
5楼2007-09-24 18:25:20
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