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Catalyst of basic ionic liquid immobilized on metal-organic frameworks and preparation method thereof

A metal-organic framework and liquid catalyst technology, which is applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., to achieve the effects of simple preparation methods, easy separation of products, and good catalytic activity

Inactive Publication Date: 2014-07-16
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still problems in the separation and reuse of catalysts for the catalytic research of this amino ionic liquid.

Method used

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  • Catalyst of basic ionic liquid immobilized on metal-organic frameworks and preparation method thereof
  • Catalyst of basic ionic liquid immobilized on metal-organic frameworks and preparation method thereof
  • Catalyst of basic ionic liquid immobilized on metal-organic frameworks and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The preparation of I.Cr-MIL-101: join 2.8g terephthalic acid into 80ml deionized water, stir evenly on magnetic stirrer, add 6.32gCr (NO 3 ) 3 .9H 2 O, 800μl HF, stirred for 2h, and put the resulting mixture into the reaction kettle. Put the reaction kettle into an oven, set the temperature at 220°C, and crystallize for 8 hours. After the reaction was completed, the reactor was taken out, cooled to 150° C. with water, and then naturally cooled to room temperature, and the color of the solid in the obtained product was emerald green. Then filter with suction, first filter with a large-pore sand core funnel (G2) to remove residual terephthalic acid, and then filter with a small-pore sand core funnel (G4) to obtain an emerald green solid product. Put the solid product and 95% ethanol aqueous solution in a reaction kettle, purify at 80°C for 24 hours, suction filter while it is hot and wash the solid product with 50°C hot ethanol; put the solid product obtained after the...

Embodiment 2

[0047] The preparation of I.Cu-HKUST-1: take by weighing 7.97g (33mmol) Cu(NO 3 ) 2 ·3H 2 O, dissolved in 10ml of deionized water, then weighed 3.85g (18.3mmol) trimesic acid (BTC) and dissolved in 110ml of ethanol. Then they were stirred until completely dissolved, and the two solutions were mixed and stirred for 30 minutes. Then it was transferred to a reactor and reacted at 120°C for 12h. Then cool, filter with suction, wash with deionized water (20ml x3) and absolute ethanol (10ml x3) respectively, and then dry in an oven at 80°C to obtain a blue Cu-HKUST-1 metal-organic framework material.

[0048] II. Preparation of amino-functionalized imidazole-based basic ionic liquid Amim-OH: same as in Example 1.

[0049] III. Catalyst preparation: 0.5 g of Cu-HKUST-1 obtained in step I was placed in a vacuum drying oven and dried at 150° C. for 12 hours. 0.3 g of the amino-functionalized imidazolium-based basic ionic liquid Amim-OH obtained in step II was dissolved in 25 mL of...

Embodiment 3

[0051] The preparation of I.Cu-HKUST-1: with embodiment 2.

[0052] II. Preparation of amino-functionalized imidazole-based basic ionic liquid Amim-OH: same as in Example 1.

[0053] III. Catalyst preparation: 0.5 g of Cu-HKUST-1 obtained in step I was placed in a vacuum drying oven and dried at 150° C. for 12 hours. 0.3 g of the amino-functionalized imidazolium-based basic ionic liquid Amim-OH obtained in step II was dissolved in 25 mL of DMF. Disperse the vacuum-dried Cu-HKUST-1 material into the DMF solution of Amim-OH, and stir at room temperature for 24h to obtain a suspension. The suspension obtained above was vacuum filtered, washed with DMF and ethanol (3×10 mL), and dried in vacuum at 80° C. for 12 h to obtain the catalyst Amim-OHCu-HKUST-1-DMF.

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Abstract

The invention relates to a catalyst of a basic ionic liquid immobilized on metal-organic frameworks and a preparation method thereof and belongs to the field of catalyst preparation technology and application. Through chemical anchoring post-synthetic modification, an amino-functionalized imidazolyl basic ionic liquid Amim-OH is introduced into nanocavities of MOFs; by chemical bonds between amino group and metal nonsaturated vacancy, an Amim-OH ionic liquid catalyst is immobilized so as to prepare a novel basic ionic liquid immobilized catalyst. The basic heterogeneous catalyst shows excellent catalytic performance and reusability in a Knoevenagel condensation reaction.

Description

technical field [0001] The invention relates to a metal-organic framework material immobilized alkaline ionic liquid catalyst and a preparation method thereof, belonging to the field of catalyst preparation technology and application. Background technique [0002] In recent years, metal-organic frameworks (MOFs) have attracted extensive research as a novel organic-inorganic hybrid porous material. This kind of material is a porous material formed by self-assembly of different metal ions and organic ligands, which has some special structural characteristics (such as large specific surface area and large pore volume) and very strong designability, adjustable sex. These unique advantages make MOFs have very good application prospects in the fields of gas storage, adsorption separation and heterogeneous catalysis. Specifically in the field of heterogeneous catalysis, different from other traditional porous catalytic materials, the pore size of the MOFs framework can be adjuste...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C253/30C07C255/34
CPCY02P20/50
Inventor 纪敏罗群兴
Owner DALIAN UNIV OF TECH
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