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Method for low-temperature plasma induced synthesis and regulation of covalent organic frame material

A plasma and reactor technology, which is applied in the field of preparation of covalent organic framework materials, can solve the problems of direct synthesis and crystal form regulation that have not been reported, and the long time of COF-1 materials, achieving great academic research value and saving reagents. , the effect of fast response

Active Publication Date: 2019-01-08
SICHUAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The existing synthesis method takes a long time to prepare COF-1 materials, and there is no report on the direct synthesis and crystal form control of AA stacked COF-1

Method used

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  • Method for low-temperature plasma induced synthesis and regulation of covalent organic frame material
  • Method for low-temperature plasma induced synthesis and regulation of covalent organic frame material
  • Method for low-temperature plasma induced synthesis and regulation of covalent organic frame material

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Effect test

Embodiment 1

[0054] Embodiment 1: Preparation of COF-5 material

[0055] Weigh 26mg terephthalic acid (BDBA) and 30mg 2,3,6,7,10,11-hexahydroxytriphenyl (HHTP) in a beaker, add 3mL dimethylformamide and 4mL mesitylene as solvent, Ultrasonic for 3 minutes until evenly dispersed, put the mixed solution into the liquid discharge plasma reactor, connect the inner and outer electrodes (tungsten rod and wound copper wire) of the dielectric barrier discharge reactor to the high-voltage AC power supply respectively, turn on the power supply and adjust The voltage is 32V and the current is 1.1A. At this time, the device emits a blue-violet light and the solution begins to boil. After reacting for 8 minutes, the power was turned off to end the reaction. The product was filtered with suction and washed twice with DMF and three times with acetone, and then dried in a vacuum oven at 80° C. for 12 hours. The gray product (COF-5) was subjected to powder X-ray diffraction (XRD) and Fourier transform infr...

Embodiment 2

[0056] Embodiment 2: Preparation of COF-10 material

[0057] Weigh 50mg biphenyl diboronic acid (BPDA) and 44mg 2,3,6,7,10,11-hexahydroxytriphenyl (HHTP) in a beaker, add 3mL dimethylformamide and 4mL mesitylene as solvent, Ultrasonic for 3 minutes until evenly dispersed, put the mixed solution into the liquid discharge plasma reactor, connect the inner and outer electrodes (tungsten rod and wound copper wire) of the dielectric barrier discharge reactor to the high-voltage AC power supply respectively, turn on the power supply and adjust The voltage is 32V and the current is 1.1A. At this time, the device emits a blue-violet light and the solution begins to boil. After reacting for 10 minutes, the power was turned off to end the reaction. The product was filtered with suction and washed twice with DMF and three times with acetone, and then dried in a vacuum oven at 80° C. for 12 hours. The gray product (COF-10) was subjected to powder X-ray diffraction (XRD) and Fourier trans...

Embodiment 3

[0058] Embodiment 3: preparation NUS-2 material

[0059] Weigh 63 mg of 2,4,6-trihydroxy-1,3,5-benzenetricarbaldehyde (Tp), dissolve it in 7 mL of dimethylformamide, then add 36 μL of hydrazine hydrate, transfer the reaction mixture and react with plasma In the tube, turn on the power and adjust the voltage to 33V, the current to 1.15A, and the response time to 10min. The obtained NUS-2 material was washed three times with DMF and ethanol and dried. The characterization results are shown in the attached Pic 4-1 ,4-2 and Figure 4-3 .

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Abstract

The invention discloses a method for low-temperature plasma induced synthesis and regulation of a covalent organic frame material. According to the method, plasma generated by dielectric barrier discharge is adopted as a synthesis method, a solvent with organic ligand is acted at a specific voltage, current and time, and the covalent organic frame material can be rapidly prepared. In addition, through solvent selection, the crystal form structure of the covalent organic frame material can be controllably adjusted. The method disclosed by the invention is simple to operate, low in energy consumption and good in universality and has wide application prospects since a material of an excellent morphology can be rapidly synthesized, and the crystal form of a two-dimensional material is regulated and controlled for a first time.

Description

technical field [0001] The invention belongs to the technical field of preparation of covalent organic framework materials, and in particular relates to a method for regulating crystal forms and synthesizing various covalent organic framework materials under dielectric barrier discharge plasma conditions. Background technique [0002] Covalent organic frameworks (COFs), as a new type of crystalline porous material covalently bonded by light elements, have been since the Yaghi research group reported the first COFs material (Science, 2005, 310, 1166-1170. ) There have been a large number of research works based on COFs materials. Materials with different structures have different application values. Two-dimensional COFs have high conduction efficiency and large conjugated π-electron systems, and are widely used in sensing, catalysis, and drug loading; three-dimensional COFs have low density, good stability, and relatively low density. With high surface area and excellent ads...

Claims

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Application Information

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IPC IPC(8): C08G83/00
CPCC08G83/008
Inventor 侯贤灯何娟龙舟江雪徐富建曾晓亮
Owner SICHUAN UNIV
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