Conjugated microporous polymer as well as preparation method and application thereof

A technology of conjugated micropores and polymers, applied in the field of chemical analysis, to achieve low detection limit, high specific surface area and chemical stability, and meet the detection requirements

Pending Publication Date: 2022-01-14
SHANDONG ANALYSIS & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to its high specific surface area, thermal stability and chemical stability, conjugated microporous polymers have become a new class of materials t

Method used

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  • Conjugated microporous polymer as well as preparation method and application thereof
  • Conjugated microporous polymer as well as preparation method and application thereof
  • Conjugated microporous polymer as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Synthesis of OH-CMP:

[0051] In a 100mL three-necked flask, sequentially add 1,3,5-tris(4-ethynylphenyl)benzene (0.4mmol, 152mg), tribromophenol (0.4mmol, 132mg), 4.0mL N,N-dimethylmethane amide and 12.0 mL of triethylamine. After three vacuum-N 2 After recycling, tetrakis(triphenylphosphine)palladium catalyst (0.07mmol, 80mg), CuI (0.21mmol, 40mg), 8.0mL N,N-dimethylformamide were added thereto. Then, three more vacuum-N 2 Circulation, the temperature of the oil bath was raised to 40°C, and after keeping for 1 hour, the temperature was adjusted to 100°C, and the reaction was carried out for 72 hours, and a dark brown solid precipitate was obtained at the bottom. After the precipitate was suction-filtered, it was washed three times with water, methanol, and acetonitrile to remove excess impurities; finally, the obtained solid was dried in an oven at 60°C for 24 hours to obtain a dark brown powder.

[0052] Characterization analysis of OH-CMP:

[0053] Such as fig...

Embodiment 2

[0055] Synthesis of OH-CMP:

[0056] In a 100mL three-necked flask, sequentially add 1,3,5-tris(4-ethynylphenyl)benzene (0.4mmol, 152mg), tribromophenol (0.4mmol, 132mg), 4.0mL N,N-dimethylmethane amide and 12.0 mL of triethylamine. After three vacuum-N 2 After recycling, tetrakis(triphenylphosphine)palladium catalyst (0.07mmol, 80mg), CuI (0.21mmol, 40mg), 8.0mL N,N-dimethylformamide were added thereto. Then, three more vacuum-N 2 Circulation, the temperature of the oil bath rose to 42°C, and after keeping for 1.2h, the temperature was adjusted to 105°C, and the reaction was carried out for 75h, and a dark brown solid precipitate was obtained at the bottom. After the precipitate was suction-filtered, it was washed three times with water, methanol, and acetonitrile to remove excess impurities; finally, the obtained solid was dried in an oven at 65°C for 24 hours to obtain a dark brown powder.

Embodiment 3

[0058] Solid phase extraction process:

[0059] The manufacturing steps of the solid-phase extraction column are as follows: accurately weigh the adsorbent OH-CMP (30mg) synthesized in Example 1, fill it into the solid-phase extraction column that has been loaded into the sieve plate, and then cover with a layer of sieve plate, and press lightly. Finally, before extracting the target substance in the sample, wash the solid-phase extraction column with 50mL of acetonitrile and 50mL of pure water to remove excess impurities in the solid-phase extraction column.

[0060] Solid-phase extraction process: The solid-phase extraction method for triazine herbicides is as follows: first, activate the self-made solid-phase extraction column with 6mL acetonitrile and 6mL pure water with pH=4 respectively, and the activation flow rate is 0.5mL / min; Measure 100mL of water sample, connect one end of the polytetrafluoroethylene suction pipe to the inlet end of the solid phase extraction colu...

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Abstract

The invention relates to the technical field of chemical analysis, in particular to a conjugated microporous polymer and a preparation method and application thereof. A repeating unit of the conjugated microporous polymer is shown in the specification, and the conjugated microporous polymer is formed by polymerizing two monomers, namely 1, 3, 5-tri (4-acetylene phenyl) benzene and tribromophenol. The OH-CMP material is of a spherical structure, has an average diameter of 30-50 nm, has high hydrophobicity, has a specific surface area up to 534 m < 2 >. G <-1 >, and has high thermal stability and chemical stability. The OH-CMP has relatively high specific surface area, excellent adsorption capacity and satisfactory repeatability. A novel method for analyzing triazine herbicide pollutants in the environment and food samples by solid-phase extraction-liquid chromatography-tandem mass spectrometry established on the basis of the material is wide in linear range and low in detection limit, and results can meet detection requirements. The polymer has a good application potential in rapid analysis of triazine herbicide pollutants in environment and food.

Description

technical field [0001] The invention relates to the technical field of chemical analysis, in particular to a conjugated microporous polymer and its preparation method and application. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Triazine herbicides are one of the traditional herbicides introduced as early as the 1950s. It is widely used in agricultural production around the world by inhibiting pre-emergence and post-emergence photosynthesis of weeds to increase the yield of crops. However, their continuous abuse and persistent residues have brought great harm to the environment and the entire food chain. Many countries and organizations have clearly stipulated the max...

Claims

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Application Information

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IPC IPC(8): C08G61/02B01D15/08B01J20/26B01J20/28B01J20/285G01N30/02G01N30/06
CPCC08G61/02B01J20/2808B01J20/285B01J20/262B01D15/08G01N30/02G01N30/06G01N2030/062C08G2261/124C08G2261/18C08G2261/312C08G2261/3328C08G2261/352C08G2261/413Y02P10/20
Inventor 赵汝松刘璐涂海辰王晓邢林金明贾永飞季小妹
Owner SHANDONG ANALYSIS & TEST CENT
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