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Covalent organic framework and composite material, preparation method and application thereof

A technology of covalent organic framework and composite materials, which is applied in the field of preparation of covalent organic framework and its composite materials, can solve the problems of high energy consumption, high cost, low hydrogen isotope efficiency, etc., and achieve large comparison area and small pore size , Enhance the effect of dynamic sieving effect

Active Publication Date: 2021-05-28
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the technical problems of low efficiency, high energy consumption and high cost of the hydrogen isotope separation method in the prior art, and provide a covalent organic framework and its composite material, preparation method and application

Method used

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  • Covalent organic framework and composite material, preparation method and application thereof
  • Covalent organic framework and composite material, preparation method and application thereof
  • Covalent organic framework and composite material, preparation method and application thereof

Examples

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preparation example Construction

[0054] The preparation method of the covalent organic framework composite material containing the repeating unit shown in formula II of the present invention, the steps are as follows:

[0055] Step 1, under the protection of an inert atmosphere, the Pd(OAC) 2 Soluble in CH 2 Cl 2 In, a clear and transparent reddish-brown solution was obtained;

[0056] Step 2. Under the protection of an inert atmosphere, the covalent organic framework of formula I is placed in CH 2 Cl 2 disperse evenly, and under stirring, dropwise add the clear and transparent reddish-brown solution obtained in Step 1. After the dropwise addition is completed, stir at room temperature for more than 12h, preferably 12-24h, filter under reduced pressure, CH 2 Cl 2 Washing, washing with acetone, and drying in vacuum to obtain a covalent organic framework composite;

[0057] Take Pd(OAC) in step 1 2 For 360mg, the CH in step 1 2 Cl 2 is 50mL, the covalent organic framework in step 2 is 250mg, and the CH...

Embodiment 1

[0070] Accurately weigh tetraaminotetraphenylmethane (66.9mg, 0.176mmol) and 2,5-dihydroxyterephthalaldehyde (58.5mg, 0.352mmol) successively on a balance in a 100mL two-necked round-bottomed flask, every 15min Evacuation and replacement of the gas with argon was repeated three times. Add 8 mL of freshly steamed anhydrous and oxygen-free tetrahydrofuran to it with a long needle, sonicate for 5 minutes, and mix well. Then, under stirring, 1.6 mL of 3 mol / L glacial acetic acid aqueous solution was added at a rate of 1-2 drops per second, protected by argon, and refluxed in an oil bath at 70°C for 72 hours. After the reaction, cool to room temperature. Then use PVDF as the filter membrane to filter under reduced pressure with a membrane filter, and wash the product with 20 mL of freshly distilled anhydrous tetrahydrofuran, repeating three times. Finally, the obtained product was soaked in 20 mL of anhydrous tetrahydrofuran overnight, and filtered again under reduced pressure to...

Embodiment 2

[0078] Accurately weigh 360 mg of Pd(OAC) in the glove box 2 In a 250mL single-necked round bottom flask, add 50mL of freshly distilled anhydrous and oxygen-free CH 2 Cl 2 , sonicate to dissolve completely, and obtain a clear and transparent reddish-brown solution, which is set aside. Weigh 250 mg of the COF-301 powder prepared in Example 1 into a 250 mL two-necked round-bottomed flask, perform vacuum treatment and argon gas replacement every 15 minutes, and repeat the operation three times. Subsequently, 50 mL of freshly distilled anhydrous and oxygen-free CH 2 Cl 2 , protected by argon, stirred at room temperature for 1 h, so that the COF-301 powder was fully dispersed in CH 2 Cl 2 , to obtain COF-301 dispersion. Under stirring, drop the prepared clear and transparent red-brown solution into the above-mentioned COF-301 dispersion at a rate of 1-2 drops per second, and finally stir at room temperature for 24 hours. After the reaction, the solution was filtered under re...

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Abstract

The invention discloses a covalent organic framework and a composite material, a preparation method and application thereof, and belongs to the technical field of covalent organic frameworks. The technical problems of low efficiency, high energy consumption and high cost of a hydrogen isotope separation method in the prior art are solved. A repetitive unit of the covalent organic framework is as shown in a formula I which is described in the specification. The covalent organic framework structure contains an imine bond and a hydroxyl group, and the imine bond and the hydroxyl group have a strong coordination effect with palladium ions, so that the binding force between the palladium ions and the covalent organic framework is stronger, and the covalent organic framework composite material doped with the palladium ions can be prepared; then the palladium nanoparticle doped covalent organic framework composite material is prepared through one-step hydrogen in-situ reduction, the palladium nanoparticles are high in activity and have a certain selective adsorption effect on hydrogen isotopes, and the adsorption effects on the hydrogen isotopes are different in strength, so that the organic framework can be applied to the field of separation of the hydrogen isotopes (H2 / D2); and the separation conditions are mild, the separation efficiency is high, the energy consumption is low, and the operation is simple.

Description

technical field [0001] The invention belongs to the technical field of covalent organic framework, and specifically relates to a covalent organic framework and its composite material, preparation method and application. Background technique [0002] Nanocomposites are based on resin, rubber, ceramics and metal as the continuous phase, and nano-sized metals, semiconductors, rigid particles and other inorganic particles, fibers, carbon nanotubes and other modifiers as the dispersed phase. Methods The modifier is uniformly dispersed in the matrix material to form a composite system containing nanometer-sized materials, which is called nanocomposite material. Nanocomposites are widely used in aerospace, national defense, transportation, sports and other fields due to their excellent comprehensive properties, especially the designability of their properties. However, the composite materials doped with metal nanoparticles in the prior art mainly adopt the method of physically dop...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J20/22B01J20/30B01D59/00
CPCC08G83/008B01J20/226B01D59/00Y02P20/50
Inventor 贲腾付静茹
Owner JILIN UNIV
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