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Bifunctional organic porous material and preparation method thereof

A dual-functional, organic framework technology, applied in the cross field, to achieve the effect of good selectivity, simple separation, and mild reaction conditions

Active Publication Date: 2018-10-19
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the problem of existing porous organic framework catalytic materials in catalytic CO 2 In the process of cycloaddition reaction, it is necessary to use toxic heavy metals as Lewis acids, synergistic catalysts and high temperature and pressure problems, and to provide a metal-free, environmentally friendly dual-functional porous organic framework catalytic material and its preparation method

Method used

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  • Bifunctional organic porous material and preparation method thereof
  • Bifunctional organic porous material and preparation method thereof
  • Bifunctional organic porous material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Step 1: Dissolve 0.5mmol tetrakis(4-alkynyltetraphenyl)methane, 1mmol 2,5-dibromopyridine, 0.0075mmol tetrakis(triphenylphosphine)palladium, and 0.0075mmol cuprous iodide in 4mL DMF and 2mL tris In the mixed solvent of ethylamine, the reaction system was subjected to freezing, evacuation and nitrogen filling three times, and then heated to 60° C. for 4 days to obtain a mixed solution.

[0033] Step 2: Filter the mixed solution obtained in Step 1, and wash the solid product 3 times with DMF, water, methanol and tetrahydrofuran solution respectively to remove soluble organic matter and catalyst, and dry it in vacuum at 80°C under the condition of vacuum degree of 133Pa After 15 hours, a porous organic framework material POF-PN containing pyridine sites was obtained.

[0034] Step 3: At room temperature, disperse 1 mmol of the POF-PN in 25 mL of toluene solution, add 1.5 mmol of bromoacetic acid under nitrogen protection and stirring conditions, heat up to 50 ° C and react...

Embodiment 2

[0050] Step 1: Dissolve 0.5mmol tetrakis(4-alkynyltetraphenyl)methane, 1mmol 2,5-dibromopyridine, 0.01mmol tetrakis(triphenylphosphine)palladium, and 0.01mmol cuprous iodide in 5mL DMF and 2mL tris In the mixed solvent of ethylamine, the reaction system was subjected to freezing, evacuation and nitrogen filling three times, and then heated to 70° C. for 4 days to obtain a mixed solution.

[0051] Step 2: Filter the mixed solution obtained in Step 1, and wash the solid product 3 times with DMF, water, methanol and tetrahydrofuran solution to remove soluble organic matter and catalyst, and dry it in vacuum at 90°C under a vacuum degree of 133Pa After 12 hours, a porous organic framework material POF-PN containing pyridine sites was obtained.

[0052] Step 3: At room temperature, disperse 1 mmol of the POF-PN in 25 mL of toluene solution, add 2 mmol of bromoacetic acid under nitrogen protection and stirring conditions, heat up to 50 ° C and react for 2 days; cool to room temperat...

Embodiment 3

[0059] Step 1: Dissolve 0.5mmol tetrakis(4-alkynyltetraphenyl)methane, 1.5mmol 2,5-dibromopyridine, 0.015mmol tetrakis(triphenylphosphine)palladium, and 0.015mmol cuprous iodide in 6mL DMF and 3mL In a mixed solvent of triethylamine, the reaction system was subjected to freezing, evacuation, and nitrogen filling three times, and then heated to 80° C. for 3 days to obtain a mixed solution.

[0060] Step 2: Filter the mixed solution obtained in Step 1, and wash the solid product 5 times with DMF, water, methanol and tetrahydrofuran solution respectively to remove soluble organic matter and catalyst, and dry it in vacuum at 100°C under a vacuum degree of 133Pa After 12 hours, a porous organic framework material POF-PN containing pyridine sites was obtained.

[0061] Step 3: At room temperature, disperse 1 mmol of the POF-PN in 30 mL of toluene solution, add 2 mmol of bromoacetic acid under nitrogen protection and stirring conditions, heat up to 70 ° C and react for 2 days; cool t...

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Abstract

The invention provides a metal-free and environmentally friendly bifunctional porous organic frame catalytic material and a preparation method thereof, and belongs to the field of preparation method of organic porous materials. The preparation method of the bifunctional porous organic frame material comprises that a porous organic frame substrate having pyridine sites is formed by polymerization connection of two organic building units and then is modified with bromoacetic acid to obtain carboxylic acid sites and bromoanion sites. The metal-free bifunctional porous organic frame material can efficiently catalyze the reaction of CO2 with an epoxy compound to form cyclic carbonate under a condition without the existence of a heterogeneous synergistic catalyst; the bifunctional porous organicframe material has the advantages that the preparation method is simple and easy to operate, and the material is non-toxic, friendly to environment and good in reproducibility of catalytic performance.

Description

technical field [0001] The invention relates to interdisciplinary technical fields such as organic chemistry, material chemistry, and catalytic chemistry, and specifically relates to a bifunctional organic porous material and a preparation method thereof. Background technique [0002] Human production and activities produce a large amount of carbon dioxide (CO 2 ) is widely recognized as a greenhouse gas that is having a devastating impact on the environment and ecological balance. However, CO 2 It is also a non-toxic, non-flammable and important C1 resource with abundant reserves, which can be transformed into a variety of industrial raw materials with economic value. Therefore, compared to CO 2 Simple adsorption capture treatment to CO 2 As a raw material, its chemical transformation has more practical significance and economic value. However, due to CO 2 It has high thermodynamic stability and kinetic inertness, and is not easily activated. During the reaction, high...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J35/10C08G61/12C07D317/36
CPCC07D317/36C08G61/122B01J31/06B01J2231/49C08G2261/3328C08G2261/354C08G2261/72C08G2261/3221C08G2261/124C08G2261/228C08G2261/312B01J35/61B01J35/60
Inventor 马鼎璇刘康
Owner QINGDAO UNIV OF SCI & TECH
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