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
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[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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