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Nitrogen-rich supercrosslinked porous polymer material, and preparation method and application thereof

A porous polymer, hypercrosslinking technology, applied in chemical instruments and methods, water pollutants, other chemical processes, etc., can solve problems such as illegal use, and achieve the effects of short adsorption time, fast adsorption rate, and easy operation.

Active Publication Date: 2019-08-06
EAST CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although our country has already included malachite green in the list of banned veterinary drugs for food animals, there are still many companies using it illegally for their own self-interest.

Method used

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  • Nitrogen-rich supercrosslinked porous polymer material, and preparation method and application thereof
  • Nitrogen-rich supercrosslinked porous polymer material, and preparation method and application thereof
  • Nitrogen-rich supercrosslinked porous polymer material, and preparation method and application thereof

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Experimental program
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Embodiment 1

[0039] Embodiment 1: A kind of preparation method of nitrogen-rich hypercrosslinked porous polymer material

[0040] Experimental selection of triptycene (A 1 ) and 2,4-diamino-6-phenyl-1,3,5-triazine (A 2 ) as a prefunctionalized monomer. In short, the solid reactant A 1 (0.03mol, 7.63g) and A 2 (0.01 mol, 1.87 g) was dissolved in 15 mL of anhydrous 1,2-dichloroethane. Under nitrogen atmosphere, dimethoxymethane (0.08 mol, 7.06 mL) and anhydrous ferric chloride (0.06 mol, 9.75 g) were added to the above solution using a syringe. The resulting mixture was then heated to 45° C., refluxed at a constant temperature for 5 h, then slowly heated to 80° C., and refluxed at a constant temperature for 19 h. After cooling to room temperature, the crude product was collected by filtration, and the product was washed repeatedly with methanol solution until the filtrate was almost colorless. Finally, the product was dried in a vacuum oven at 60° C. to obtain brown solid triazine hype...

Embodiment 2

[0052] The hypercross-linked porous polymer material N-HCPP (2.5±0.2mg) was added to different concentrations of MG aqueous solution (5mL) and kept shaking at 25°C for 24h. The adsorbed N-HCPP was separated from the solution using a disposable filter device, and the concentration of the filtrate was tested by ultraviolet-visible spectroscopy at a wavelength of 618nm. With the increase of the concentration of MG before adsorption, the adsorption amount of MG by N-HCPP gradually increased until it stabilized at a certain value. At lower concentrations, more adsorption sites are available. As the concentration increased, the MG dye molecules occupied the available sites on the N-HCPP surface after reaching the maximum adsorption capacity. Therefore, after the concentration continued to increase, the adsorption amount tended to balance. Using the Freundlich isotherm model to fit the isotherm experimental data, it can be seen that the linear correlation coefficient R of N-HCPP to...

Embodiment 3

[0054] The hypercrosslinked porous polymer material N-HCPP (2.5 ± 0.2 mg) was added to the MG aqueous solution with an initial concentration of 10 ppm and shaken at regular intervals at 25 °C for different times. The adsorbed N-HCPP was separated from the solution using a disposable filter device, and the concentration of the filtrate was tested by ultraviolet-visible spectroscopy at a wavelength of 618nm. The results showed that the removal rate of MG by N-HCPP was above 60% within 5 minutes. Further, after fitting the experimental data with a pseudo-second-order kinetic model, the linear correlation coefficient R 2 Up to 0.9997, the calculated adsorption rate constant k 2 The value is 0.00497g·mg·min -1 . The results show that the adsorption of N-HCPP to MG conforms to the pseudo-second order kinetics, with Image 6 .

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Abstract

The invention discloses a nitrogen-rich supercrosslinked porous polymer material, and a preparation method and an application thereof. The nitrogen-rich supercrosslinked porous polymer material is synthesized by a one-step Friedel-Crafts alkylation reaction; triptycene and 2,4-diamino-6 phenyl-1,3,5-triazine are used as a nitrogen source and a carbon source of the synthesized product; a result ofX-ray diffraction analysis shows that a significant dispersion peak exists in a range of 10-30 DEG C, the material is an amorphous porous structure, and the BET specific surface area is 57-58 m<2> / g;and the pore sizes are mainly distributed in the range of 10-20 nm. The preparation method and the obtained product have the following advantages: (1) the one-step Friedel-Crafts alkylation process makes the synthesis simple; (2) the porosity is large; and (3) the malachite green (MG) adsorption capacity is large. N-HCPP has a large MG adsorption capacity, and the maximum adsorption capacity reaches 150 mg.g<-1>. Additionally, the prepared N-HCPP has an excellent recycling property, and has great modification and application prospects in the adsorption of the MG in water.

Description

technical field [0001] The invention belongs to the technical field of chemical adsorption materials, and in particular relates to a nitrogen-rich super-crosslinked porous polymer material and a one-step Friedel-Crafts alkylation reaction to synthesize the nitrogen-rich super-crosslinked porous polymer material and its adsorption to malachite green. Background technique [0002] Malachite Green is a widely used fungicide in aquaculture worldwide and is very effective against important protozoan and fungal infections. One of the reasons why it is very popular in the aquaculture industry is that malachite green can prevent the conversion of amino acids in bacterial cells into protein peptides when bacteria divide, which prevents the division of bacteria, thus showing malachite green The second is because aquatic products are prone to deterioration and corruption during long-distance transportation, and malachite green can play a good role in keeping fresh. At the same time, i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/30C02F1/28C02F101/38
CPCB01J20/267C02F1/285C02F2101/38
Inventor 何妍杨俊鑫王小龙平崧古晓斌袁定重罗太安那兵
Owner EAST CHINA UNIV OF TECH