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Mechanochemical preparation method for covalent organic framework material and application

A covalent organic framework and mechanochemical technology, applied in the field of photocatalytic materials, can solve the problems of difficult synthesis of photocatalytic materials, affecting the application efficiency of materials, and the inhomogeneous crystallinity of generated materials, and achieves simple preparation methods and good industrial performance. The effect of applying the foreground and shortening the generation time

Active Publication Date: 2019-01-18
RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The main difficulty in the synthesis of materials by ball milling lies in the inhomogeneity and poor crystallinity of the generated materials, which affect the application efficiency of materials
A novel high-stability covalent organic framework photocatalyst, TpMA, synthesized by a hydrothermal method, exhibits better photocatalytic degradation of phenol and methyl orange than graphitized carbon nitride (g-C 3 N 4 ), and it is difficult to synthesize ideal and efficient photocatalytic materials simply by ball milling the raw material monomers

Method used

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  • Mechanochemical preparation method for covalent organic framework material and application
  • Mechanochemical preparation method for covalent organic framework material and application
  • Mechanochemical preparation method for covalent organic framework material and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Example 1 : Preparation of covalent organic framework material TpMA of the present invention

[0041] This embodiment is the preparation of covalent organic framework material TpMA, such as figure 1 Shown, the specific preparation method is:

[0042] Put melamine and 2,4,6-triformylphloroglucinol raw materials into a ball mill reaction kettle, mix well, and then add 3mL p-toluenesulfonic acid. Add the zirconia media pellets used for grinding into the reactor, and the total volume of the media pellets and the mixed raw materials shall not exceed 2 / 3 of the total volume of the reactor. Cover the lid of the reaction kettle, fix the ball mill reaction kettle and cover the outer cover of the ball mill. Set the rotational speed of the ball mill to 300 rpm, set the total grinding time to 3 hours and 12 minutes, and the net ball milling time is 3 hours. After ball milling, the samples were washed with dimethylformamide, acetone and ultrapure water, and then dried in an ove...

Embodiment 2

[0043] Example 2 : Structural characterization of the covalent organic framework material TpMA of the present invention

[0044] This example is the structural characterization of the covalent organic framework material TpMA, specifically as follows:

[0045] 1. TEM image

[0046] The morphology and structure of covalent organic framework material TpMA were analyzed by transmission electron microscope Hitachi H-7500: from figure 2 It can be seen that the covalent organic framework material TpMA presents an exfoliated flake-like structure.

[0047] 2. PXRD spectrum

[0048] The X-ray diffraction (XRD) pattern of the covalent organic framework material TpMA was obtained on a PAN-alytical X’Pertdiffractometer, using nickel to filter Cu Kα rays, with a scanning range from 5° to 50° and a scanning speed of 4° / min. Such as image 3 As shown, the covalent organic framework material TpMA has diffraction characteristic peaks at 2θ of 5°, 9.2°, 14.6°, and 26.9°, which are basical...

Embodiment 3

[0055] Example 3 : Catalytic performance test of covalent organic framework material TpMA of the present invention

[0056] In this example, phenol and methyl orange were selected as representatives to test the catalytic performance of the covalent organic framework material TpMA. The test steps are as follows: prepare 50 mL of 10 mg / L phenol and methyl orange dye solutions respectively, put them in a 100 mL beaker, add 30 mg of TpMA photocatalyst sample, and stir for 1 hour in the dark to reach the steady state of adsorption-desorption. Using an Xe lamp as a light source, a 400 nm cut-off glass filter was used to remove wavelengths irrelevant to the experiment, and the solution was irradiated while being magnetically stirred. During the irradiation process, 1.5ml of the solution was taken at regular intervals, and after centrifugation, the supernatant was taken for testing. After the photocatalytic reaction, the TpMA photocatalyst was washed with ultrapure water, dried and...

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Abstract

The invention provides a method for synthesizing an efficient photocatalytic covalent organic framework material by using a mechanochemical method. The method is characterized by comprising the following steps: using the mechanochemical method, using melamine and 2,4,6-triformyl resorcinol as raw materials, distributing according to a certain mole ratio, using a planetary ball-milling device, acquiring sticky slurry at a room temperature through wet-process ball-milling, after washing and drying the sticky slurry, to obtain the stable covalent organic framework material. The method is simple in process, only less solvent is used in a grinding reaction process, the environment is protected, and production cost is reduced. Reaction time is only 1 / 36 of that of a hydrothermal method, a reaction condition is mild, and the method can be applied for large-scale production. In addition, the prepared stripping sheet-like structure powder material is wide in visible light absorption range, highin separation efficiency of a photon-generated carrier, capable of rapidly decomposing toxic organic substances in water, has excellent performance of treating organic wastewater, can be repeatedly used, and has good industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of photocatalytic materials, and relates to a mechanochemical preparation method and application of a covalent organic framework photocatalyst based on melamine and 2,4,6-triformylphloroglucinol. Background technique [0002] With the rapid development of the global economy, the energy shortage and environmental pollution caused by the extensive use of non-renewable energy have become two major worldwide problems that restrict human development and affect social progress. In order to achieve sustainable economic development, finding and developing green, environmentally friendly and sustainable new energy sources has become an important issue that needs to be solved urgently for human survival and development. Among the many existing new energy systems (such as wind energy, tidal energy, geothermal energy and solar energy), solar energy is considered to be the best choice to replace fossil energy in the futu...

Claims

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Application Information

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IPC IPC(8): C07D487/22C08G83/00B01J31/06B01J37/00C02F1/30C02F101/30C02F101/34C02F101/38
CPCB01J31/063B01J37/0036C02F1/30C02F2101/308C02F2101/34C02F2101/345C02F2101/38C02F2101/40C02F2305/10C07D487/22C08G83/008
Inventor 蔡亚岐吕宏洲牛红云
Owner RES CENT FOR ECO ENVIRONMENTAL SCI THE CHINESE ACAD OF SCI
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