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Preparation method of imidazole functionalized amphiphilic periodic mesoporous organic silicon material

A mesoporous organosilicon and functionalization technology, which is applied in chemical instruments and methods, organic chemistry, compounds of group 4/14 elements of the periodic table, etc., can solve the problem of less morphology and achieve simple steps and good morphology , high regularity effect

Inactive Publication Date: 2013-11-20
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are relatively few articles on the preparation of ionic liquid materials and the morphology is relatively poor (B. Karimi, et al., Chem. Commun., 2010, 46, 6947.)

Method used

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  • Preparation method of imidazole functionalized amphiphilic periodic mesoporous organic silicon material
  • Preparation method of imidazole functionalized amphiphilic periodic mesoporous organic silicon material
  • Preparation method of imidazole functionalized amphiphilic periodic mesoporous organic silicon material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Material containing 10% functionalized imidazole silicon source and BTEE copolymerization

[0033] (1) Weigh 2.5g of 1-vinylimidazole into a 100mL round bottom flask, use 50mL of toluene as solvent, stir at 1000rmp at 0°C until completely dissolved; dissolve 3.5g of 1,3-propane sultone in 15mL of toluene , slowly added dropwise to the round bottom flask of step (1) at 0°C, and the dropwise addition was completed in 10 minutes. After 30 minutes at 0°C, the temperature was raised to 40°C at a rate of 8°C / min, and the reaction was maintained at 1000rmp for 5 days, and the pressure was reduced. After filtration, it was washed with anhydrous ether (20mL×3) to obtain a highly deliquescent white solid, which was dried under vacuum at 50°C for 12h. The product quality is 5.28g, and the yield is 63.4%. The white solid obtained is dissolved in a 25mL round-bottomed flask with 2mL of water, and the mass concentration of 98% concentrated sulfuric acid is slowly added dro...

Embodiment 2

[0039] Example 2: Material containing 20% ​​functionalized imidazole silicon source and BTEE copolymerized

[0040] Step (1) of this embodiment is the same as that of Embodiment 1.

[0041] (2) This step is basically the same as step (2) of Example 1, except that the dark red liquid obtained in the added step (1) is 1.257g, triethoxysilane is 0.57mL, and Kmarstedt catalyst is 0.15mL . The mass of the obtained brown viscous liquid was 1.835 g.

[0042] (3) This step is basically the same as step (3) of Example 1, except that the weight of the brown viscous liquid obtained in the added step (2) is 1.835g, and the amount of BTEE is 3mL; the quality of the obtained product is 6.096g .

[0043] (4) Same as step (4) of Example 1. The resulting product mass was 5.481 g.

[0044] from Figure 5 It can be seen in the d 100 There is a strong diffraction peak at d 110 and d 200 A weak diffraction peak at , indicates that the material has an ordered two-dimensional hexagonal meso...

Embodiment 3

[0046] Example 3: Material containing 30% functionalized imidazole silicon source and BTEE copolymerization

[0047] Step (1) of this embodiment is the same as that of Embodiment 1.

[0048] (2) This step is basically the same as step (2) of Example 1, except that the dark red liquid obtained in the added step (1) is 1.886g, triethoxysilane is 0.86mL, and Kmarstedt catalyst is 0.25mL . The mass of the obtained brown viscous liquid was 2.697g.

[0049] (3) This step is basically the same as step (3) of Example 1, except that the weight of the brown viscous liquid obtained in the added step (2) is 2.697g, the amount of BTEE is 2.6mL, and the time for dropping is 10min; The resulting product mass was 6.337 g.

[0050] (4) Same as step (4) of Example 1. The resulting product mass was 5.883 g.

[0051] from Figure 8 It can be seen in the d 100 There is a strong diffraction peak at d 110 and d 200 A weak diffraction peak at , indicates that the material has an ordered two-...

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Abstract

The invention discloses a preparation method of imidazole functionalized amphiphilic periodic mesoporous organic silicon material. The method comprises the following steps of: synthesizing functionalized vinyl imidazole by 1-vinyl imidazole and 1, 3-propane sultone, forming a functionalized silicon source containing imidazole group by clicking triethoxysilane with the functionalized vinyl imidazole, slowly hydrolyzing the silicon source and 1, 2-di(triethoxy silicon base) ethane (BTEE) under the action of special surfactant and strong acid to form the PMO (Periodic Mesoporous Organosilicas) material with specific appearance. The PMO material prepared by the above technology has the following advantages that the material in the invention has better appearance and higher regularity; the material in the invention has a lipophilic group, and also can be modified with hydrophilic group later, so that the material can play due role in a wider field; the method in the invention has simple steps, is easy to operate, and can modify the groups having special functions according to actual needs, so that the method has certain development space.

Description

technical field [0001] The invention relates to a material preparation technology, in particular to a preparation method of an imidazole-functionalized amphiphilic ordered mesoporous organic silicon material. Background technique [0002] Ionic liquids have many advantages that traditional solvents cannot match: odorless, non-flammable, less pollution, good stability, etc. Because of these advantages, it is applied to the synthesis of organic and macromolecular substances as a green solvent, thereby receiving the attention of more and more chemists (J.Dupont, et al., Chem.Rev., 2002,102,3667. ; P. Wasserscheid, et al., Angew. Chem., Int. Ed., 2000, 39, 3772.). However, because ionic liquids are very expensive, and the production process is uneconomical, highly toxic, and harmful to the environment, their wide application has been greatly limited. In order to expand the application space of ionic liquids, chemists combined ionic liquids with some other solid carriers, which...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/28C08G77/34C07D233/60C07F7/18C08J9/00
Inventor 刘国华邓博心肖伟程探宇
Owner SHANGHAI NORMAL UNIVERSITY
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