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Super-hydrophobic covalent organic framework material as well as preparation method and application thereof

A covalent organic framework, super-hydrophobic technology, applied in separation methods, textiles and papermaking, liquid separation, etc., can solve the problems that hinder the practical application of oil-water separation, loss of surface super-hydrophobicity, poor durability, etc., and achieve excellent oil-water separation stability The effect of high stability, simple preparation process and good practicability

Active Publication Date: 2021-07-02
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most superhydrophobic materials will involve some application technical problems in the actual separation of oil and water, such as poor durability, especially when they are exposed to extreme conditions such as high temperature, low temperature or corrosive environments, which may lead to permanent loss of surface superhydrophobicity. , the defects of these materials will seriously hinder their practical application in oil-water separation

Method used

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  • Super-hydrophobic covalent organic framework material as well as preparation method and application thereof
  • Super-hydrophobic covalent organic framework material as well as preparation method and application thereof
  • Super-hydrophobic covalent organic framework material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Example 1 Preparation of a superhydrophobic covalent organic framework material LNU-40

[0050] 1. Synthesis of LNU-40

[0051] Add 400mg of tris(4-boronic acid pinesol ester phenyl)amine (0.6418mmol) and 312.89mg of 3,6-dibromocarbazole (0.96274mmol) into 60mL N,N'-dimethylformamide for dissolution, set In a 100mL round-bottomed flask, use liquid nitrogen to freeze and use an oil pump to evacuate the nitrogen for three times. Add 80mg of tetrakis(triphenylphosphine)palladium and 5mL of potassium carbonate solution (2moL / L) to the reaction system quickly, and then repeat the cycle of desorption. The reaction mixture was heated to 130 °C and stirred and refluxed for 48 hours under nitrogen protection.

[0052] 2. Post-processing of LNU-40

[0053] Suction filter the reactant to leave solid insoluble matter, which is washed with tetrahydrofuran, water and acetone solvent several times to remove possible residual unreacted monomer or catalyst residue. The crude product ...

Embodiment 2

[0055] Example 2 Preparation of a superhydrophobic covalent organic framework material LNU-41

[0056] 1. Synthesis of LNU-41

[0057] 400 mg of tris(4-boronic acid pinesol ester phenyl)amine (0.6418 mmol) and 312.89 mg of 2,7-dibromocarbazole (0.96274 mmol) were dissolved in 60 mL of N,N'-dimethylformamide, Place in a 100mL round-bottomed flask, freeze with liquid nitrogen and evacuate nitrogen with an oil pump for three times, add 80mg tetrakis(triphenylphosphine) palladium and 5mL potassium carbonate solution (2moL / L) to the reaction system quickly, and then repeat the cycle After degassing, the reaction mixture was heated to 130°C and stirred at reflux for 48 hours under nitrogen protection.

[0058] 2. Post-processing of LNU-41

[0059] Suction filter the reactant to leave solid insoluble matter, which is washed with tetrahydrofuran, water and acetone solvent several times to remove possible residual unreacted monomer or catalyst residue. The crude product was further ...

Embodiment 3

[0061] Example 3 Preparation of a superhydrophobic covalent organic framework material LNU-42

[0062] 1. Synthesis of LNU-42

[0063] Add 400mg of tris(4-boronic acid pinesol ester phenyl)amine (0.6418mmol) and 386.16mg of 3,6-dibromo-9-phenylcarbazole (0.96274mmol), add 60mL N,N'-di Methylformamide was dissolved, placed in a 100mL round-bottomed flask, frozen with liquid nitrogen and evacuated with an oil pump to vent nitrogen three times, and 80mg of tetrakis(triphenylphosphine)palladium and 5mL of potassium carbonate solution (2moL / L) were quickly added to the reaction system, and then repeated cycle degassing, the reaction mixture was heated to 130 ° C and stirred and refluxed under nitrogen protection conditions for 48 hours.

[0064] 2. Post-processing of LNU-42

[0065] Suction filter the reactant to leave solid insoluble matter, which is washed with tetrahydrofuran, water and acetone solvent several times to remove possible residual unreacted monomer or catalyst res...

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Abstract

The invention belongs to the field of super-hydrophobic materials, and particularly relates to a super-hydrophobic covalent organic framework material and a preparation method and application thereof. The super-hydrophobic covalent organic framework material LNUs is obtained by taking 4-(tetramethyl-1,3,2-dioxaborolan-2-yl)-N,N-bis-[4-(tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl as a construction element and carrying out Suzuki coupling reaction on the 4-(tetramethyl-1,3,2-dioxaborolan-2-yl)-N,N-bis-[4-(tetramethyl-1,3,2-dioxaborolan-2-yl)phenyl and a pi-conjugated dibromo carbazole monomer. The method provided by the invention has the advantages of easily available raw materials and simple preparation process, and can meet actual production requirements. The contact angle of the prepared super-hydrophobic material can reach 150 degrees or above, stable hydrophobic performance can be kept under severe conditions of strong acid, strong alkali, high temperature and the like, mixed liquid of multiple kinds of water and oil (or organic solvents) is separated, and the separation efficiency can reach 90% or above. After 10 times of recycling, the original separation effect can still be maintained, and the super-hydrophobic covalent organic framework material has good practicability in the field of oil-water separation treatment in environmental sewage.

Description

technical field [0001] The invention belongs to the field of superhydrophobic materials, and in particular relates to a superhydrophobic covalent organic framework material and its preparation method and application. Background technique [0002] With the continuous exploitation and production of petroleum, frequent oil spill accidents during transportation and use, and the discharge of oily wastewater in the production of daily necessities seriously threaten human health and the ecological environment. Effective oil-water separation is a key issue that needs to be solved urgently. In order to reduce the adverse effects of oil pollution on the water environment, many methods have been adopted to solve the problem of oil spill and oily wastewater discharge, such as gravity separation, centrifugation, degreasing, flotation, coagulation and in-situ combustion, etc. Applications are time- or energy-intensive and limited by inefficient separations, complex operations, or secondar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G61/12D06M15/37C02F1/40
CPCC08G61/124D06M15/37C02F1/40C08G2261/12C08G2261/135C08G2261/3162C08G2261/3241C08G2261/411D06M2200/12Y02A20/204
Inventor 布乃顺郑桂月夏立新闫卓君许彦梅耿彤飞王朋宇于芷懿
Owner LIAONING UNIVERSITY
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