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Bimetallic center metal-organic framework material capable of enhancing Lewis acidity and preparation method thereof

A Lewis acidic and organic framework technology, applied in the field of Lewis acidic double metal center metal-organic framework materials and its preparation, can solve the problems of single Lewis acidic site, unstable catalyst, harsh reaction conditions, etc., to achieve easy Large-scale preparation, low cost, easy to obtain results

Active Publication Date: 2018-11-02
XUZHOU NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, in order to truly apply the currently studied MOFs materials to the size-selective cyanosilylation reaction of aromatic aldehydes, scientists still need to solve the following problems: (1) Most of the reported MOFs catalytic materials have harsh reaction conditions and the catalysts are not stable enough (2) Traditional MOFs as catalysts generally only have a single Lewis acidic site, making their catalytic efficiency low

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  • Bimetallic center metal-organic framework material capable of enhancing Lewis acidity and preparation method thereof
  • Bimetallic center metal-organic framework material capable of enhancing Lewis acidity and preparation method thereof
  • Bimetallic center metal-organic framework material capable of enhancing Lewis acidity and preparation method thereof

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Embodiment 1

[0027] A method for preparing a Lewis acidic bimetallic center metal-organic framework material, comprising the following steps:

[0028] S1, weigh 28mg 5,5'-methylene diisophthalic acid (H 4 MDIP), 42mg Cd(ClO 4 ) 2 .6H 2 O, placed in a glass sample bottle, add water, mix well;

[0029] S2. Put the glass sample bottle in the hydrothermal synthesis reaction kettle, then place the hydrothermal synthesis reaction kettle in the electric blast drying oven, keep the temperature at 120°C, and react for 24 hours. After the reaction is completed, cool to obtain colorless block crystals , filtered, washed with deionized water for 3 to 5 times, and dried at 100°C for 5 hours to obtain the metal-organic framework material Cd-MDIP, whose structure is as follows figure 1 As shown, it can be seen that there is a large rectangular pore in its 3D network structure, which lays a good foundation for ion adsorption and size-selective catalysis;

[0030] S3. Soak the crystal Cd-MDIP obtained...

Embodiment 2

[0041] A method for preparing a Lewis acidic bimetallic center metal-organic framework material, comprising the following steps:

[0042] S1, weigh 28mg 5,5'-methylene diisophthalic acid (H 4 MDIP), 47.8mg Cd(ClO 4 ) 2 .6H 2 O, placed in a glass sample bottle, add water, mix well;

[0043] S2. Put the glass sample bottle in the hydrothermal synthesis reaction kettle, then place the hydrothermal synthesis reaction kettle in the electric blast drying oven, keep the temperature at 115°C, and react for 26 hours. After the reaction is completed, cool to obtain colorless block crystals , filtered, washed with deionized water for 3 to 5 times, and dried at 90°C for 6 hours to obtain the metal-organic framework material Cd-MDIP;

[0044] S3. Soak the crystal Cd-MDIP obtained in step S2 in an aqueous solution containing an equimolar amount of ferric nitrate, stir for 3 minutes, then centrifuge at 8000r / min for 7 minutes, wash with deionized water for 3 to 5 times, and dry at 90°C f...

Embodiment 3

[0046] A method for preparing a Lewis acidic bimetallic center metal-organic framework material, comprising the following steps:

[0047] S1, weigh 30.8mg 5,5'-methylene diisophthalic acid (H 4 MDIP), 42mg Cd(ClO 4 ) 2 .6H 2 O, placed in a glass sample bottle, add water, mix well;

[0048] S2. Put the glass sample bottle in the hydrothermal synthesis reaction kettle, then place the hydrothermal synthesis reaction kettle in the electric blast drying oven, keep the temperature at 125°C, and react for 22 hours. After the reaction is completed, cool to obtain colorless block crystals , filtered, washed with deionized water for 3 to 5 times, and dried at 80°C for 8 hours to obtain the metal-organic framework material Cd-MDIP;

[0049] S3. Soak the crystal Cd-MDIP obtained in step S2 in an aqueous solution containing an equimolar amount of ferric nitrate, stir for 5 minutes, then centrifuge at 8000r / min for 7 minutes, wash with deionized water for 3 to 5 times, and dry at 80°C f...

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Abstract

The invention discloses a bimetallic center metal-organic framework material capable of enhancing Lewis acidity and a preparation method thereof. The method comprises the step of enriching Fe<3+> serving as a novel Lewis acid site into a pore channel of an MOF (Metal-Organic Framework) material, specifically comprising the following sub-steps: by taking 5, 5'-methylene diphthalic acid as a ligand,and taking MOF obtained by a hydrothermal reaction with cadmium perchlorate hexahydrate as a raw material, and adsorbing the Fe<3+>, thereby obtaining the novel bimetallic center metal-organic framework material. The material synthesized by the method disclosed by the invention has size selectivity of aromatic aldehyde catalyzed under mild conditions and cyanosilylation performance, has a bimetallic center, and is high in catalytic efficiency, excellent in cycling stability, simple and controllable in preparation process and capable of realizing large-scale production.

Description

technical field [0001] The invention belongs to the field of catalytic materials, and relates to a metal-organic framework catalytic material for efficiently catalyzing the size-selective cyano-silylation reaction of aromatic aldehydes, in particular to a bimetallic center metal-organic framework material with enhanced Lewis acidity and its preparation method. Background technique [0002] Cyanohydrins, as intermediates in biological processes and organic synthesis, are important compounds. The most common and practical preparation method is the reaction of aromatic aldehyde or ketone with trimethylsilyl cyanide (TMSCN). This cyanosilylation reaction is a typical C–C bond formation reaction catalyzed by Lewis acids, which can be used as electrophilic catalysts to activate carbonyl compounds. However, most of the reported catalysts have low catalytic efficiency, harsh reaction conditions, and cannot be recycled. Therefore, it is urgent to develop and develop recyclable cat...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J37/10C07F7/18
CPCB01J31/2213B01J37/10B01J2531/0244B01J2531/27C07F7/188
Inventor 李阳王健王梦秋付辅彬武鹏彦
Owner XUZHOU NORMAL UNIVERSITY