Method and application of preparation of polynitrogen two-dimensional covalent organic framework materials using 1,3,5-triformylphloroglucinol as the center

A triformylphloroglucinol, covalent organic framework technology, applied in separation methods, chemical instruments and methods, other chemical processes, etc., can solve the practical application of two-dimensional covalent organic framework materials difficult gas separation membrane materials, gas Selective permeation, unsatisfactory separation effect, etc., to achieve the effect of improving gas separation performance, wide application and good synthesis repeatability

Active Publication Date: 2022-03-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2017, Tsuru et al. used two-dimensional covalent organic framework material (COF-1) to prepare ultra-thin two-dimensional covalent organic framework nanosheet membrane by means of peeling and vacuum filtration, and carried out gas separation tests. However, the separation effect Not ideal (H 2 / N 2 The separation ratio is only 4), which may be because the COF-1 nanosheet material (1.5nm) with a larger pore size will still have a larger pore size during the free stacking process, which is unable to treat CO 2 Gas plays a selective permeation role, and the untreated existing two-dimensional covalent organic framework materials are difficult to be used as gas separation membrane materials for practical application

Method used

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  • Method and application of preparation of polynitrogen two-dimensional covalent organic framework materials using 1,3,5-triformylphloroglucinol as the center
  • Method and application of preparation of polynitrogen two-dimensional covalent organic framework materials using 1,3,5-triformylphloroglucinol as the center
  • Method and application of preparation of polynitrogen two-dimensional covalent organic framework materials using 1,3,5-triformylphloroglucinol as the center

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1 NO 2 - Preparation of TpPa

[0041] Add 31 mg of 1,3,5-triformylphloroglucinol (Tp) and 34.5 mg of o-nitro-p-phenylenediamine (NO 2 -Pa) powder. 1.5 ml of 1,4-dioxane and 1,3,5-trimethylbenzene were added as solvents respectively. Add 0.5 ml of 3 mol per liter of acetic acid as a catalyst. The mixture was homogenized after sonication for 10 min. Then put the Pyrex glass tube into the liquid nitrogen bath to freeze. After the liquid in the tube solidifies, turn on the vacuum oil pump to pump air, and then take the sample tube out of the liquid nitrogen bath and wait for the liquid to melt. This freezing-pumping- The melting cycle needs to be performed three times. The vacuum-tight sample tube was placed in an oil bath at 120°C and heated for 72 hours to obtain a dark red powder. The powder was washed with tetrahydrofuran, methanol and acetone, extracted and washed with ethanol and dichloromethane, and dried under vacuum at 120°C for 12 hours to obtain NO ...

Embodiment 2

[0043] Example 2 NH 2 - Preparation of TpPa

[0044] Get 150 mg of NO produced in Example 1 2 -TpPa, 3 g SnCl 2 2H 2 O was placed in a round-bottomed flask, 5 ml of anhydrous tetrahydrofuran was added, and refluxed at 77°C for 3 hours under the protection of nitrogen.

[0045] Use 70 milliliters of 3 moles per liter of hydrochloric acid to quench after the reaction is completed, and then wash with 70 milliliters of 1 moles per liter of hydrochloric acid, deionized water, methanol and acetone for 3 times, and obtain a brown powder after vacuum drying at 120 degrees Celsius for 12 hours. Nitrogen two-dimensional covalent organic framework material NH 2 -TpPa.

[0046] X-ray diffraction (such as image 3 ) to confirm the product and simulated structure (such as Figure 4 ) is consistent, has a layered structure, and its (100) characteristic peak appears near 5°. FTIR characterization showed that, compared to NO 2 -TpPa spectral curve, NH 2 -TpPa at 1336cm -1 The nitro ...

Embodiment 3

[0047] Example 3 NO 2 - Preparation of TpPa nanosheets

[0048] The NO prepared in Example 1 2 10 mg of TpPa powder was dispersed in 100 ml of n-butanol solution, sealed in a 500 ml ball mill jar, and ball milled at a speed of 60 rpm for 1 hour. Subsequently, the ethyl acetate dispersion of the nanosheets was taken out and allowed to stand for 15 days to remove unopened large particles. The dispersion liquid obtained after standing has obvious Tyndall phenomenon, even after standing for one month, Tyndall phenomenon is still clearly visible. The scanning electron microscope pictures show that the nanosheets and the precursors present a very different morphology, and the flower cluster precursors present flake nanosheets after peeling off (such as Figure 8 ). Transmission electron microscope pictures show that the average size of nanosheets is about 500-1000 nanometers, and they are very easy to fold (such as Figure 9 ). Atomic force microscope pictures show that the th...

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Abstract

The invention discloses a method and application of a β-enaminone-based polynitrogen two-dimensional covalent organic framework material centered on 1,3,5-triformylphloroglucinol. The method comprises reacting 1,3,5-triformylphloroglucinol with o-nitro-p-phenylenediamine to generate a two-dimensional covalent organic framework material NO 2 ‑TpPa; set NO 2 ‑TpPa amino groups were reduced with stannous chloride to generate a novel multi-nitrogen two-dimensional covalent organic framework material NH 2 ‑TpPa process. Using the preparation method described in the invention, a novel crystalline multi-nitrogen two-dimensional covalent organic framework material can be obtained.

Description

technical field [0001] The present invention is a method for preparing a β-enaminoketone-based polynitrogen two-dimensional covalent organic framework material centered on 1,3,5-triformylphloroglucinol, which involves obtaining a novel polynitrogen two-dimensional covalent organic framework Materials have great application potential in the field of gas adsorption and gas separation membrane preparation. Background technique [0002] Since the 21st century, with the progress of global industry and the development of economy, energy consumption has been increasing day by day. Among them, fossil fuels such as coal, oil and natural gas account for more than 80% of the total energy consumption due to their high energy density and wide range of utilization. The main component of fossil fuel combustion exhaust is CO 2 , CO 2 Excessive emissions will lead to global temperature rise and damage the ecosystem, which is one of the problems to be solved urgently in our country. The m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00B01D53/02B01D53/22B01D71/72B01J20/22B01J20/30
CPCC08G83/00B01D53/02B01D53/228B01D71/72B01J20/226B01D2257/504Y02C20/40
Inventor 杨维慎王鹏远彭媛
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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