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Chromium metal organic framework catalytic material and preparation method thereof

A technology of organic framework and catalytic materials, which is applied in the field of organic chemistry and material chemistry, and in the field of inorganic chemistry, can solve the problems of complex synthesis process, increased industrial cost, unfavorable energy saving and environmental protection, etc., and achieve good stability, high activity and excellent reaction conditions mild effect

Inactive Publication Date: 2015-12-23
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The first type of MOF catalyst can catalyze the reaction under milder conditions, but it can only be used under the condition of the simultaneous presence of a homogeneous co-catalyst (halogen ion), which causes the product to be separated and purified, complicating the synthesis process ; the second class of MOF catalysts can catalyze CO without the need for a homogeneous co-catalyst 2 Cycloaddition reaction, but requires higher reaction temperature (>100°C) and higher CO 2 pressure (>3MPa), which causes an increase in industrial costs, which is not conducive to energy saving and environmental protection
[0004] The above results indicate that CO can be catalyzed under mild and co-catalyst-free conditions. 2 Preparation of MOF heterogeneous catalysts for cycloaddition reactions remains a challenge

Method used

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  • Chromium metal organic framework catalytic material and preparation method thereof
  • Chromium metal organic framework catalytic material and preparation method thereof
  • Chromium metal organic framework catalytic material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Add 0.001mol chromium chloride, 0.00075mol 2-nitroterephthalic acid and 0.25mol deionized water 1 into the hydrothermal reaction kettle, and react at 180°C for 3 days; Washing with water and absolute ethanol for 3 times respectively; using 0.5mol deionized water 2 and 0.5mol absolute ethanol 1 as solvents respectively, activated in a microwave reactor at 130°C for 3 hours; Vacuum drying at 100°C for 12 hours at 133Pa to obtain MIL-101-NO 2 ; 0.001mol of the MIL-101-NO 2 Add 0.001mol stannous chloride monohydrate into 0.2mol absolute ethanol 2, react at 70°C for 10 hours, cool to room temperature, centrifuge, wash 3 times with concentrated hydrochloric acid, wash 3 times with deionized water, and wash 3 times with absolute ethanol times; vacuum drying at 100°C for 12 hours under a vacuum degree of 133Pa to obtain MIL-101-NH 2 ;

[0029] (2) At room temperature, 0.001mol of the MIL-101-NH 2 Disperse in a mixed solution of 0.1mol acetonitrile and 0.05molDMF; add 0....

Embodiment 2

[0039] (1) Add 0.001mol chromium chloride, 0.001mol 2-nitroterephthalic acid and 0.277mol deionized water 1 into the hydrothermal reaction kettle, and react at 180°C for 4 days; Wash with water and absolute ethanol for 3 times respectively; use 0.6mol deionized water and 0.6mol absolute ethanol as solvents respectively, and activate at 140°C for 2 hours in a microwave reactor; Dry under vacuum at 110°C for 13 hours to obtain MIL-101-NO 2 ; 0.001mol of the MIL-101-NO 2 Add 0.0015mol stannous chloride monohydrate into 0.22mol absolute ethanol 2, react at 80°C for 10 hours, cool to room temperature, centrifuge, wash 4 times with concentrated hydrochloric acid, wash 4 times with deionized water, and wash 4 times with absolute ethanol times; vacuum drying at 110°C for 13 hours under a vacuum degree of 133Pa to obtain MIL-101-NH 2 ;

[0040] (2) At room temperature, 0.001mol of the MIL-101-NH 2 Disperse in a mixed solution of 0.12mol acetonitrile and 0.05molDMF; add 0.004mol1,2-...

Embodiment 3

[0044] (1) Add 0.001mol chromium chloride, 0.002mol 2-nitroterephthalic acid and 0.3mol deionized water 1 into the hydrothermal reaction kettle, and react at 180°C for 5 days; Wash with water and absolute ethanol for 4 times respectively; use 0.7mol deionized water and 0.7mol absolute ethanol as solvents respectively, and activate at 150°C for 1 hour in a microwave reactor; Dry under vacuum at 120°C for 13 hours to obtain MIL-101-NO 2 ; 0.001mol of the MIL-101-NO 2 Add 0.0017mol stannous chloride monohydrate into 0.27mol absolute ethanol 2, react at 80°C for 12 hours, cool to room temperature, centrifuge, wash 4 times with concentrated hydrochloric acid, wash 4 times with deionized water, and wash 4 times with absolute ethanol times; vacuum drying at 120°C for 14 hours under a vacuum degree of 133Pa to obtain MIL-101-NH 2 ;

[0045] (2) At room temperature, 0.001mol of the MIL-101-NH 2 Disperse in a mixed solution of 0.14mol acetonitrile and 0.06molDMF; add 0.005mol1,2-dib...

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Abstract

The present invention provides a chromium metal organic framework catalytic material and a preparation method thereof, belongs to the cross technical field of inorganic chemistry, organic chemistry and material chemistry. The chromium metal organic framework catalytic material consists of 2-amino p-phthalic acid and chromium salt coordinated in the form of hexa-coordinate, and a quaternary phosphonium salt ionic liquid is modified to the amino group of the 2-amino p-phthalic acid The preparation method of the chromium metal organic framework catalytic material comprises first preparing a metal organic framework substrate by a solvothermal method, and then modifying the quaternary phosphonium salt ionic liquid to the substrate. The chromium metal organic framework efficiently catalyzes reaction of CO2 with epoxy compound in the presence of no homogeneous catalyst to form cyclic carbonic ester, and reaches a catalytic yield of more than 98%. The preparation method of the chromium metal organic framework catalytic material has the advantages of simple and easy synthetic method, and good reproducibility of synthesized samples.

Description

technical field [0001] The invention relates to the interdisciplinary technical fields of inorganic chemistry, organic chemistry and material chemistry, in particular to a bifunctional chromium metal-organic framework catalytic material with Lewis acidic sites and ionic liquid sites modified by bifunctional ionic liquids and a preparation method thereof. Background technique [0002] The main source of energy in today's modern society is still fossil fuels, and the energy generated by the combustion of fossil fuels accounts for 85% of the total energy demand. The problem that follows is a large amount of carbon dioxide (CO 2 ), resulting in the greenhouse effect. Over the past half century, atmospheric CO 2 Concentration from 609mg / m 3 increased to 746mg / m 3 , have a great impact on the global climate and ecological balance, leading to serious environmental and ecological problems, which will threaten the survival of human beings. However, CO 2 The most important C1 res...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J35/10C07D317/36
Inventor 施展马鼎璇李柏延刘康冯守华
Owner JILIN UNIV
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