Covalent organic framework material with sulfydryl functionalized beta-ketoenamine structure as well as preparation method and application of covalent organic framework material

A covalent organic framework and functionalization technology, applied in chemical instruments and methods, other chemical processes, chemical/physical processes, etc., can solve problems such as interference and low sensitivity of detection instruments, and achieve the effect of improving the detection limit

Active Publication Date: 2022-01-14
QINGDAO TECHNOLOGICAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the deficiencies in the prior art, the present invention provides a covalent organic framework material with a mercapto-functionalized β-ketoenamine structure, which is applied to quantitative separation When enriching heavy metals (Co2+, Ni2+, Cd2+) in environmental water samples, it can solve the The problems of complex matrix interference and low sensitivity of detection instruments faced in the analysis of trace heavy metals are stable and can be reused

Method used

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  • Covalent organic framework material with sulfydryl functionalized beta-ketoenamine structure as well as preparation method and application of covalent organic framework material
  • Covalent organic framework material with sulfydryl functionalized beta-ketoenamine structure as well as preparation method and application of covalent organic framework material
  • Covalent organic framework material with sulfydryl functionalized beta-ketoenamine structure as well as preparation method and application of covalent organic framework material

Examples

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preparation example Construction

[0037] The second aspect of the present invention provides a method for preparing the covalent organic framework material of the above-mentioned mercapto-functionalized β-ketoenamine structure, comprising the following steps:

[0038] S1. Disperse 1,3,5-triformylphloroglucinol and 2,5-divinyl-p-phenylenediamine in 1,3,5-trimethylbenzene and 1,4-dioxane , slowly drop acetic acid into the dispersion, and mix well;

[0039] S2. The solution obtained in step S1 is subjected to a hydrothermal reaction to obtain a precursor, which is repeatedly washed and dried with acetone;

[0040] S3. Add 1,2-ethanedithiol, azobisisobutyronitrile and trifluorotoluene to the precursor material obtained in step S2 to carry out co-precipitation reaction, collect the precipitate by filtration, and repeatedly wash and dry with acetone.

[0041] Further, in step S1, the mass ratio of 1,3,5-triformylphloroglucinol and 2,5-divinyl-p-phenylenediamine is 21:24, 1,3,5-trimethyl The volume ratio of benzene...

Embodiment 1

[0066] A method for preparing a covalent organic framework material with a mercapto-functionalized β-ketoenamine structure, comprising the following steps:

[0067] S1. Disperse 21 mg of 1,3,5-triformylphloroglucinol and 24 mg of 2,5-divinyl-p-phenylenediamine in 4.5 mL of 1,3,5-trimethylbenzene and In 4.5mL 1,4-dioxane, slowly drop 0.5mL9mol L into the dispersion liquid -1 Acetic acid, stir to make it evenly mixed;

[0068] S2. Transfer the solution obtained in step S1 to a polytetrafluoroethylene-lined stainless steel autoclave, and react at 120°C for 72 hours to prepare the precursor material of the covalent organic framework material, and repeatedly wash the covalent organic framework precursor material with acetone, and dried in a drying oven at 60°C;

[0069] S3. Transfer the covalent organic framework precursor material obtained in step S2 to a branched-necked flask, add 845mg 1,2-ethanedithiol, 10mg azobisisobutyronitrile and 4mL trifluorotoluene, at 80°C under N 2 ...

Embodiment 2

[0072] The covalent organic framework material of the mercapto-functionalized β-ketoenamine structure in Example 1 is used in the separation and enrichment of heavy metals (Co 2+ 、Ni 2+ 、Cd 2+ ), the specific experimental process is as follows figure 2 As shown, the specific steps are as follows:

[0073] (1) The prepared covalent organic framework material with thiol-functionalized β-ketoenamine structure was used to fabricate an online solid-phase extraction column. Use a piece of polytetrafluoroethylene tube as a small column tube for solid phase extraction (L=4cm, I.D.=1.8mm, O.D.=2.6mm), fill it with 5 mg of the prepared covalent organic framework powder material, and seal it with glass wool Both ends of the solid phase extraction cartridge. Utilize the polytetrafluoroethylene tube (I.D.=1.0mm, O.D.=2.0mm) of smaller inner diameter and outer diameter to connect the solid-phase extraction column and the flow injection system made;

[0074] (2) Use the peristaltic pum...

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Abstract

The invention belongs to the technical field of environmental analysis chemistry and new material preparation, and particularly relates to a covalent organic framework material of a sulfydryl functionalized beta-ketoenamine structure as well as a preparation method and application of the covalent organic framework material. When the covalent organic framework material is applied to quantitative separation and enrichment of heavy metals (Co < 2 + >, Ni < 2 + > and Cd < 2 + >) in an environmental water sample, the problems of complex matrix interference and low sensitivity of a detection instrument during analysis of trace heavy metals in the current environmental water sample can be solved, and the covalent organic framework material is stable in property, and can be utilized repeatedly.

Description

technical field [0001] The invention belongs to the technical field of environmental analysis chemistry and new material preparation, and specifically relates to a covalent organic framework material with a mercapto-functionalized β-ketoenamine structure, a preparation method and application thereof. 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] Heavy metals are highly toxic and pass along the food chain, bioaccumulate, and accumulate, posing a serious threat to the environment and human health. Analysis and detection of heavy metal content in environmental samples is of great significance for environmental monitoring and human health risk assessment. However, heavy met...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00B01J20/22B01J20/285B01D15/08B01J20/30
CPCC08G83/008B01J20/226B01J20/285B01D15/08Y02P10/20
Inventor 王莎莎韩小璇田永
Owner QINGDAO TECHNOLOGICAL UNIVERSITY
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