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Covalent organic framework and preparation method thereof

A covalent organic framework and aldehyde compound technology, applied in the field of covalent organic framework and its preparation, can solve the problems of high cost, unfriendly environment and high risk

Active Publication Date: 2018-01-05
SHANGHAI INST OF ORGANIC CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to overcome the defects of prior art covalent organic frameworks using organic solvents as the reaction medium, the preparation process is relatively dangerous, the cost is high, the environment is not friendly, and large-scale preparations cannot be carried out. A kind of preparation method of covalent organic framework

Method used

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  • Covalent organic framework and preparation method thereof
  • Covalent organic framework and preparation method thereof
  • Covalent organic framework and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0093]

[0094] Add 2,4,6-triformylphloroglucinol (1.05g, 5.0mmol) and 80% hydrazine hydrate (470uL, 7.5mmol) into water (40mL) and sonicate for 5min, replace the argon three times under dry ice The tube is then sealed. After its temperature rose to room temperature, it was placed in an oven at 120° C. to react for 5 days. After the reaction was completed, it was cooled, filtered, washed with acetone, and dried in a vacuum oven to obtain 1.04 g of covalent organic framework material HCOF-1 as a dark red powder solid, with a yield of 94%.

[0095] from figure 1 It can be found that the infrared spectrum of HCOF-1 ( Figure 1-2 ) and the infrared spectrum of raw material 2,4,6-triformylphloroglucinol ( Picture 1-1 ) is completely different, indicating that a reaction has occurred. The peak around 1590nm is the C=N bond shifting to the short wave due to the hydrogen bond, and superimposed with the C=C double bond peak of another isomer to form a broad peak, indicating the...

Embodiment 2

[0102]

[0103] Add trimellitic trialdehyde (1.0 g, 6.1 mmol) and 80% hydrazine hydrate (580 uL, 9.2 mmol) into water (40 mL) and sonicate for 5 min, add aqueous acetic acid (4 mL, 6 mol / L,) to the above cloudy solution, The tube was sealed after changing the argon gas three times under liquid nitrogen freezing. After its temperature rose to room temperature, it was placed in an oven at 120° C. to react for 5 days. After the reaction was completed, cooled, filtered, washed with acetone, and dried in a vacuum oven to obtain 0.93 g of light yellow fluffy solid covalent organic framework material (expressed as HCOF-2), yield: 86%.

[0104] from figure 2 It can be found that the infrared spectrum of HCOF-2 ( Figure 2-2 ) and the infrared spectrum of the raw material pyromellitic trialdehyde ( diagram 2-1 ) diagrams are completely different, indicating that the reaction has occurred; in the infrared spectrum of HCOF-2, the vibration peak of C=N bond appears at 1628nm, whic...

Embodiment 3

[0110]Add 2,4,6-triformylphloroglucinol (1.05g, 5.0mmol) and 80% hydrazine hydrate (470uL, 7.5mmol) into water (40mL) and sonicate for 5min, pump and ventilate 3 times under refrigeration and seal this tube. After its temperature rose to room temperature, it was placed in an oven at 120°C to react for 3 days. After the reaction was completed, it was cooled, filtered, washed with acetone, and dried in a vacuum oven to obtain 1.0 g of covalent organic framework material HCOF-1 as a dark red powdery solid, with a yield of 91%. The characterization data of HCOF-1 obtained in this embodiment are basically the same as those in Example 1.

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Abstract

The invention discloses a covalent organic framework and a preparation method thereof. The preparation method comprises the following step: performing polymerization reaction on a compound shown as aformula II and hydrazine or a P-phenylenediamine compound shown as a formula IV in water in the presence or the absence of acid. The preparation method of the covalent organic framework utilizes the water as a reactive solvent for the first time, is high in reaction yield, safe, environmentally friendly, cost reduction and suitable for large-scale industrial production. The covalent organic framework prepared by the preparation method disclosed by the invention is larger in specific surface area and wide in application prospect in the fields of gas adsorption and separation, photo-electricityor catalysis and the like.

Description

technical field [0001] The present invention relates to a covalent organic framework and a preparation method thereof. Background technique [0002] Covalent Organic Frameworks (COFs) are a class of crystalline organic porous polymers. In 2005, the Yaghi group reported for the first time that the formation of boronate bonds was used to construct new organic materials with properties such as porosity, high structural regularity and large specific surface area: covalent organic framework ( A.P.; Benin, A.I.; Ockwig, N.W.; O’Keeffe, M.; Matzger, A.J.; Yaghi, O.M. Science 2005, 310, 1166.). Due to their porosity and highly ordered structure, COFs have great application value in the fields of gas storage and separation, catalysis, sensing, and optoelectronic materials, and have received extensive attention in recent years (Ding, S.-Y.; Wang, W. Chem. Soc. Rev. 2013, 42, 548; Zeng, Y.; Zou, R.; Zhao, Y. Adv. Mater. 2016, 28, 2855; Waller, P.J.; Gándara, F.; Yaghi, O.M. Acc. Ch...

Claims

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Application Information

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IPC IPC(8): C08G12/04C08G12/08C08G8/16
Inventor 赵新林沨卢健
Owner SHANGHAI INST OF ORGANIC CHEMISTRY - CHINESE ACAD OF SCI
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