Preparation method and application of magnetic covalent organic framework compound for adsorbing triphenylmethane dyes

A technology of covalent organic framework and triphenylmethane, which is applied in the fields of alkali metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of complex operation and long reaction time, and achieve simplified synthesis process, short synthesis time and high efficiency. The effect of adsorption performance

Active Publication Date: 2020-07-28
HARBIN INST OF TECH
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Problems solved by technology

[0004] The present invention provides a preparation method and application of a magnetic covalent organic framework compound that adsorbs triphenylmethane dyes i...

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  • Preparation method and application of magnetic covalent organic framework compound for adsorbing triphenylmethane dyes
  • Preparation method and application of magnetic covalent organic framework compound for adsorbing triphenylmethane dyes
  • Preparation method and application of magnetic covalent organic framework compound for adsorbing triphenylmethane dyes

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specific Embodiment approach 1

[0045] Embodiment 1: A method for preparing a magnetic covalent organic framework compound that adsorbs triphenylmethane dyes in this embodiment is carried out in the following steps:

[0046] 1. Superparamagnetic carboxylation of Fe 3 o 4 Magnetic nanoparticles Fe 3 o 4 Preparation of -COOH:

[0047] ①.Weigh 16.5g of FeCl 3 ·6H 2 O and 25g Na 3 Cit·2H 2 O was dissolved in 500mL of ethylene glycol, and ultrasonically treated at 40kHz for 40min to obtain a yellow transparent solution;

[0048] ②. Under the condition that the temperature of the water bath is 50° C. and the stirring speed is 200 rpm, add 30 g of sodium acetate to the yellow transparent solution obtained in step ①, and stir for 30 minutes to obtain a brown transparent solution;

[0049] ③.Transfer the brown transparent solution obtained in step ② into a stainless steel reaction kettle, and react at a temperature of 200°C for 10h;

[0050] ④. Collect the product obtained in step ③ with a magnet, and then w...

specific Embodiment approach 2

[0092] Specific embodiment two: the application of a magnetic covalent organic framework compound that adsorbs triphenylmethane dyes in this embodiment: the Fe prepared in specific embodiment one 3 o 4 -COOH@COF is used as a material for detecting triphenylmethane dyes in the field of aquaculture.

[0093] The application effect of this embodiment is verified by the following tests, and the specific test process is as follows:

[0094] Test a: the Fe prepared by the specific embodiment one 3 o 4 -COOH@COF was applied to the adsorption detection of five triphenylmethane dyes standards of MG, RB, CV, BG and VPBO, and then the detection method of the dye was constructed by HPLC, and the linearity, LOD and RSD of the detection method were evaluated .

[0095] Conclusion: as shown in Table 6, the linear relationship of the 5 dyes is good, and the linear correlation coefficient (R 2 ) are higher than 0.9990. The LOD and LOQ of these dyes were calculated at S / N ratios of 3 and ...

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Abstract

The invention discloses a preparation method and application of a magnetic covalent organic framework compound for adsorbing triphenylmethane dyes. The invention belongs to the field of preparation ofmagnetic covalent organic framework compounds. The invention aims to solve the technical problems of complex operation and long reaction time of the existing method for synthesizing the covalent organic frameworks (COFs). The method comprises the following steps of: 1) preparing carboxylated magnetic nano (Fe3O4-COOH); and 2) synthesizing a magnetic covalent organic framework (Fe3O4-COOH(at)COF)on the surface of the magnetic nano material through a Schiff base reaction. The preparation method is simple, the synthesis time is short, and the synthesis only takes 3 hours at high temperature of120 DEG C. The prepared Fe3O4-COOH (at) COF has magnetic responsiveness, high specific surface area, high thermal stability and high adsorption performance (42.8 mg/g-500mg/g). According to the method, the triphenylmethane cationic dyes can be rapidly extracted from a complex sample within 10 minutes, so that multi-residue detection of the triphenylmethane cationic dyes can be realized, the pretreatment process of the complex sample is simplified, and the separation efficiency is greatly improved.

Description

technical field [0001] The invention belongs to the field of preparation of magnetic covalent organic framework compounds, in particular to a preparation method and application of magnetic covalent organic framework compounds for adsorbing triphenylmethane dyes. Background technique [0002] Triphenylmethane dyes, such as malachite green (MG) and crystal violet (CV), have been widely used in aquaculture because of their excellent efficacy in preventing and treating infectious diseases of fish and other aquatic products. However, in follow-up studies, it was found that MG and CV are carcinogenic and mutagenic, so their use is prohibited. Since 2002, we can find that the MG and CV in the Food and Feed Rapid Alert Report (RARFF) have been significantly reduced, that is, its prohibition effect has been reflected, but there are still a small number of unscrupulous merchants using it. Some researchers proposed to use bright green BG instead of MG, but BG with a structure similar ...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28C02F1/48C02F101/30
CPCB01J20/226B01J20/06B01J20/28009B01J20/28057C02F1/285C02F1/488C02F2101/308
Inventor 杨鑫赵海田刘婧怡
Owner HARBIN INST OF TECH
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