Ion covalent organic framework catalyst, and preparation method and catalytic applications thereof

A covalent organic framework and ionization technology, applied in organic compound/hydride/coordination complex catalysts, organic chemistry, chemical instruments and methods, etc., can solve the problems of poor catalytic effect of compounds and achieve high added value of products , good chemical stability, easy to operate

Active Publication Date: 2018-01-05
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The structural unit of this material contains cobalt-porphyrin complex, which can be used to catalyze the cycloaddition reaction between carbon dioxide and epoxy compounds. The catalytic effect of these compounds is very poor. We improved the previous invention and synthesized an ionized COFs material. Through simple ion exchange, we obtained catalysts with different catalytic groups, which are very effective for more types of substrates. good catalytic effect

Method used

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  • Ion covalent organic framework catalyst, and preparation method and catalytic applications thereof
  • Ion covalent organic framework catalyst, and preparation method and catalytic applications thereof
  • Ion covalent organic framework catalyst, and preparation method and catalytic applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of Example 1 Co(II)@TF-Py COF catalyst

[0029] 1) Preparation of TF-Py COF

[0030] Take TFPPy (62.1mg, 0.1mmol) and PyTTA (56.7mg, 0.1mmol) in an ampoule, add 1mL 1,4-dioxane, 1mL mesitylene, 0.7mL N,N-dimethylacetamide , ultrasonically mix evenly, add 0.1mL 3M acetic acid solution, mix evenly; freeze the ampoule bottle in liquid nitrogen, evacuate to 20Pa, blow nitrogen gas, and seal the nozzle with flame; react at 140°C for 72 hours; the reaction is over Afterwards, the ampoule was naturally cooled to room temperature, and the product was washed with acetone and tetrahydrofuran to remove unreacted substrate; the washed product (TF-Py COF) was vacuum-dried at 80°C for 12 hours.

[0031] 2) Reduction of imine bonds in the TF-Py COF framework to secondary amine bonds

[0032] Take 30mg of TF-Py COF (about 0.03mmol) and place it in 30ml of ethanol solution with a concentration of 1M sodium borohydride, and stir for 30min at room temperature; wash the reduc...

Embodiment 2-4

[0037] Preparation of Example 2-4M(II)@TF-Py COF catalyst

[0038] Preparation method as described in Example 1, its difference is as follows:

[0039] Example

Embodiment 5

[0040] Example 5 Catalytic conversion of CO by Co(II)@TF-Py COF catalyst 2 experiment

[0041] Co(II)@TF-Py COF was used as a heterogeneous catalyst to catalyze the reaction of carbon dioxide and epichlorohydrin to generate cyclocarbonate compounds. At 100°C, under the condition of carbon dioxide pressure of 1Mpa, epichlorohydrin (0.587ml, about 7.5mmol), cocatalyst tetrabutylammonium iodide (5.5mg, about 0.015mmol), Co(II)@TF-Py COF (12.18mg, 0.0075mmol of cobalt element) mixed and stirred for 12h, The product and the catalyst are separated by filtration or suction filtration, and the liquid phase is the catalyzed target cyclocarbonate compound, with a yield of 99%.

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Abstract

The invention discloses preparation of a novel heterogenous catalyst M(II)@TF-Py COF, and applications of a covalent organic framework (COFs) material loaded metal in synthesis of cyclic carbonate compounds via catalysis of carbon dioxide and epoxy compounds. The structure unit of the material contains a metal catalytic site, and can be used for catalyzing reaction of carbon dioxide with the epoxycompounds. COFs is relatively large in specific surface area, and possesses an open channel structure, so that it is beneficial for full and high efficiency reaction. Co(II)@TF-Py COF is capable of catalyzing conversion of carbon dioxide into cyclic carbonates. The reaction substrates can be changed, reaction yield is high, the catalyst can be recycled, operation is convenient, and product addedvalue is high.

Description

technical field [0001] The present invention relates to the preparation of a heterogeneous catalyst M(II)@TF-Py COF: after the covalent organic framework (COFs) material is ionized, the catalyst material containing different metal catalytic groups is exchanged through simple ion exchange, and the catalyst material is obtained by using It is used to catalyze the reaction of carbon dioxide and epoxy compounds to synthesize cyclic carbonate compounds. Background technique [0002] In the past few decades, scientists all over the world have done a lot of basic research work on the chemical conversion and application of carbon dioxide. The research on the chemical conversion and application of carbon dioxide is not only of great academic significance, but also in The industry also has very broad application prospects, and has high economic and social benefits. Carbon dioxide and epoxy compounds can react under the catalysis of catalysts to form cyclocarbonate compounds, and cycl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/10C07D317/36
CPCY02P20/584
Inventor 高艳安景学超冷文光冯璐
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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