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Method for preparing covalent organic framework material film through quantitative vacuum evaporation

A covalent organic framework and vacuum evaporation technology, which is applied in vacuum evaporation plating, metal material coating process, ion implantation plating, etc., can solve the problems of low raw material utilization rate, cumbersome steps, poor flexibility, etc., and achieve raw material utilization High efficiency, high preparation efficiency, and cost reduction

Active Publication Date: 2019-12-31
BEIJING NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the solvothermal synthesis method is not conducive to the large-scale synthesis of COFs membranes and the industrialization of the preparation method due to the problems of cumbersome steps, limited types of dispersing solvents, poor flexibility, harsh reaction conditions, and long preparation time.
[0005] In particular, the solvothermal synthesis method needs to immerse the substrate in the monomer solution, and react under high temperature and pressure after sealing, which makes many monomers directly react in the solution to form products, and the nucleation and growth of monomers on the substrate cannot be measured. , the utilization rate of raw materials is low, and the steps of seed crystal coating and secondary growth are generally required
Therefore, it is not easy to quantitatively control industrial production, and it is not easy to prepare ultra-thin films

Method used

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  • Method for preparing covalent organic framework material film through quantitative vacuum evaporation
  • Method for preparing covalent organic framework material film through quantitative vacuum evaporation
  • Method for preparing covalent organic framework material film through quantitative vacuum evaporation

Examples

Experimental program
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Effect test

Embodiment 1

[0055] Example 1: Preparation of COF-LZU1 / PAN film

[0056] A method for preparing a covalent organic framework material thin film by quantitative vacuum evaporation. The PAN base film is soaked in 2mol / L NaOH aqueous solution at 30°C for 1h. Then the diaphragm was taken out and rinsed with deionized water several times until the rinse solution was neutral to convert -CN groups into -COOH groups. Finally, the acidic PAN-based film was air-dried at room temperature. According to the stoichiometric ratio, the two monomers, p-phenylenediamine and trimesaldehyde, were evaporated at 80°C by vacuum evaporation reaction method and reacted for 2 hours, and the COF-LZU1 / PAN film was obtained by repeated alternate evaporation.

[0057] The surface of the prepared COF-LZU1 / PAN film was scanned by SEM, and the obtained scanning electron microscope photos were as follows: figure 1 shown. It can be seen that the present invention obtains a continuous defect-free covalent organic framewor...

Embodiment 2

[0061] Example 2: COF-5 / α-Al 2 o 3 Film preparation

[0062] A method for the preparation of thin films of covalent organic framework materials by quantitative vacuum evaporation, starting with 3-aminopropyltriethoxysilane (APTES) and 4-p-formylphenylboronic acid (FPBA) 2 o 3 Modification of the tube surface. Al first 2 o 3 The tube was soaked in 50mL, 1mol / L hydrochloric acid for 5h, washed 5*25mL with distilled water, and dried at 110°C for 24h. Then, the dried Al 2 o 3 The tube was placed in 35 mL (98.29 mg) of APTES in toluene solution, and the reaction was stirred at 100° C. for 3 h under the protection of argon. Finally, 35 mL (29.6 mg) of 4-formylphenylboronic acid in ethanol was reacted at 55° C. for 1 hour. After cooling to room temperature, wash 5*20mL with ethanol, and dry in vacuum at 60°C for 24h to obtain α-Al with boric acid groups on the surface 2 o 3 Tube. Evaporate terephthalic acid (BDBA) and 2,3,6,7,10,11-hexahydroxytriphenylene (HHTP) by vacuum...

Embodiment 3

[0063] Embodiment 3: the preparation of COF-1 / PVDF film

[0064] A method for quantitative vacuum evaporation to prepare a covalent organic framework material film. The PVDF base film is soaked in deionized water for 12 hours, and then the film is taken out and dried at 25°C. Terephthalic acid (BDBA) was evaporated by vacuum evaporation reaction method and reacted at 120 °C for 6 h. Repeating this alternately, a multi-layer separation membrane can be formed on the surface of the PVDF base membrane. By weighing and calculating the prepared COF-1 / PVDF film, the raw material utilization rate is 95%. Nitrogen adsorption and desorption test results show that the membrane has a large specific surface area and can be widely used in the field of adsorption.

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Abstract

The invention belongs to the technical field of functional materials, and particularly relates to a method for preparing a covalent organic framework material film through quantitative vacuum evaporation. The method comprises the following steps of introducing an anchoring group on the surface of a substrate, then correspondingly placing two or more monomers into an evaporating dish according to areaction stoichiometric ratio, adjusting the temperature of an evaporation source, sequentially carrying out vacuum evaporation, and nucleating monomer vapor on the substrate; and by adjusting the temperature of the substrate, realizing film forming of crystal nucleus of the two or more monomers on on the substrate through diffusion reaction, and finally obtaining the covalent organic framework material film with uniform pore size. Compared with the prior art, according to the method for preparing the covalent organic framework material film through the quantitative vacuum evaporation, the complete nucleation growth of the monomers on the surface of the substrate is realized through precise adjustment of the evaporation temperature, the evaporation source area and the substrate temperature, then the preparation difficulty of the covalent organic framework material film is reduced through industrially produced vacuum evaporation equipment, and the quantitative controllable preparationof the covalent organic framework material film is realized.

Description

technical field [0001] The invention belongs to the technical field of functional materials, and in particular relates to a method for preparing a covalent organic frame material thin film by quantitative vacuum evaporation. Background technique [0002] Thin film materials can be used in separation, optoelectronics, sensing, energy storage and other fields, and have important application value. However, traditional membrane materials are mainly polymers or ceramics, which usually have a wide pore size distribution, and there is a problem of inaccurate separation. Films of new porous materials represented by covalent organic frameworks (COFs) can be used for precision separation, adsorption, sensing, photoelectric conversion, storage, catalysis and other fields. The research on its preparation method, especially the preparation method suitable for industrial promotion has become a research hotspot in this field. [0003] However, COFs materials are usually insoluble and i...

Claims

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Application Information

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IPC IPC(8): C23C14/12C23C14/02C23C14/24
CPCC23C14/02C23C14/12C23C14/24
Inventor 贾志谦郝爽
Owner BEIJING NORMAL UNIVERSITY