Magnetic COF-TpPa for enriching amide pesticide and preparation method and application of magnetic COF-TpPa

A technology for enriching amides and pesticides, applied in chemical instruments and methods, other chemical processes, water/sludge/sewage treatment, etc., can solve problems such as inability to mass-produce, low yield, and poor stability, and achieve good adsorption. The effect of large specific surface area and strong adsorption capacity

Active Publication Date: 2019-08-23
ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The whole process of solvothermal synthesis of COF is carried out in a closed reaction vessel, and real-time observation and sampling research cannot be carried out, and the yield is generally low
In addition, the solvothermal synthesis process of some COF materials requires operations such as liquid nitrogen flash freezing and flame sealing (such as "Magnetic covalent organic framework material: Synthesis and application as a sorbent for polycyclic aromatic hydrocarbons", Xuexiang Shi, 2018), triazine COFs materials The synthesis needs to be reacted in high-temperature molten zinc chloride, and the reaction conditions are relatively harsh.
Therefore, the COF preparation method has harsh conditions and cannot be mass-produced, which hinders the wide application of COF materials.
In addition, covalent organic frameworks have poor stability and difficult separation, which further limit the application of covalent organic frameworks in the enrichment of amide pesticide residues.

Method used

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  • Magnetic COF-TpPa for enriching amide pesticide and preparation method and application of magnetic COF-TpPa
  • Magnetic COF-TpPa for enriching amide pesticide and preparation method and application of magnetic COF-TpPa
  • Magnetic COF-TpPa for enriching amide pesticide and preparation method and application of magnetic COF-TpPa

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preparation example Construction

[0022] The present invention provides a kind of magnetic COF-TpPa (wherein COF is the abbreviation of covalent organic material, and Tp is the abbreviation of 2,4,6-trihydroxybenzene-1,3,5-triformaldehyde) for enriching amide pesticides The abbreviation of English name TriformylPhloroglucinol, Pa is the abbreviation of the English name p-Phenylenediamine of p-phenylenediamine) preparation method, comprises the steps:

[0023] (1) Mix 2,4,6-trihydroxybenzene-1,3,5-tricarbaldehyde, aminated magnetic beads and ethanol, and perform the first aldehyde-amine condensation reaction to obtain aldehyded magnetic beads;

[0024] (2) Add the solution of p-phenylenediamine to the dispersion of the formylated magnetic beads, then add the solution of 2,4,6-trihydroxybenzene-1,3,5-tricarbaldehyde to carry out the second aldehyde Amine condensation reaction to obtain magnetic COF-TpPa for enrichment of amide pesticides.

[0025] In the invention, 2,4,6-trihydroxybenzene-1,3,5-tricarbaldehyde,...

Embodiment 1

[0054] Mix 0.05g of 2,4,6-trihydroxybenzene-1,3,5-tricarbaldehyde with 50mL of ethanol, and ultrasonically homogenize to obtain a solution of 2,4,6-trihydroxybenzene-1,3,5-tricarbaldehyde ; Mix 0.3g of aminated magnetic beads (particle size: 0.148~0.720μm) with 20mL of ethanol, and ultrasonically homogenize to obtain a dispersion of aminated magnetic beads; mix 2,4,6-trihydroxybenzene-1,3,5 -Mix the triformaldehyde solution and the dispersion of aminated magnetic beads, and react at 40°C for 1 hour; after the reaction, wait until the temperature drops to room temperature, separate the formaldehyde magnetic beads by adding a magnet, and then soak and wash them with ethanol for 3 times (40-50mL each time), supplemented with ultrasound while soaking, the washing solution becomes clear, and formaldehyde magnetic beads are obtained;

[0055] The formylated magnetic beads were mixed with 25mL mixed solvent (1,4-dioxane and trimethylbenzene were obtained by mixing in a ratio of 1:1 b...

Embodiment 2

[0059] Mix 0.05g of 2,4,6-trihydroxybenzene-1,3,5-tricarbaldehyde with 60mL of ethanol, and ultrasonically homogenize to obtain a solution of 2,4,6-trihydroxybenzene-1,3,5-tricarbaldehyde ; Mix 0.4g of aminated magnetic beads (particle size: 0.148~0.720μm) with 25mL of ethanol, and ultrasonically homogenize to obtain a dispersion of aminated magnetic beads; mix 2,4,6-trihydroxybenzene-1,3,5 -Mix the triformaldehyde solution and the dispersion of aminated magnetic beads, and react at 50°C for 1 hour; after the reaction, wait until the temperature drops to room temperature, separate the formaldehyde magnetic beads by adding a magnet, and then soak and wash them with ethanol for 3 times (50mL each time), supplemented with ultrasound while soaking, the washing solution becomes clear, and formaldehyde magnetic beads are obtained;

[0060]The formylated magnetic beads were mixed with 25mL mixed solvent (1,4-dioxane and trimethylbenzene were obtained by mixing in a ratio of 1:1 by vo...

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Abstract

The invention provides magnetic COF-TpPa for enriching amide pesticides and a preparation method and application of the magnetic COF-TpPa and belongs to the technical field of adsorption materials. The preparation method provided by the invention comprises the following steps: (1) mixing 2,4,6-trihydroxy benzene-1,3,5-trioxin, amination magnetic beads and ethanol, and carrying out a first aldehydeamine condensation reaction so as to obtain aldehyde magnetic beads; and (2) putting a solution of p-phenylenediamine into a dispersion liquid of the aldehyde magnetic beads, further adding a solution of 2,4,6-trihydroxy benzene-1,3,5-trioxin, and carrying out a second aldehyde amine condensation reaction, thereby obtaining magnetic COF-TpPa for enriching amide pesticides. The magnetic COF-TpPa which is prepared by using the preparation method provided by the invention has excellent adsorption upon amide pesticides (prochloraz and tolfenpyrad), is good in stability, has superparamagnetism andis easy to separate, in addition, the preparation method is simple to operate, and reaction conditions are gentle and controllable.

Description

technical field [0001] The invention relates to the technical field of adsorption materials, in particular to a magnetic COF-TpPa for enriching amide pesticides and its preparation method and application. Background technique [0002] Covalent Organic Framework (COF) materials are a kind of organic porous materials with ordered structure and controllable functions, which are connected by covalent bonds such as C, H, B, O, N and other light elements. Highly ordered, large specific surface area, good chemical stability and thermal stability, etc., are mainly used in optoelectronics, catalysis, gas adsorption storage, sensing and other fields. However, there are few reports on the application of covalent organic framework materials in the enrichment detection of pesticide residues, and there is no COF that can be used for the enrichment ability of amide pesticide residues. [0003] At present, the common synthesis methods of COF materials include solvothermal synthesis, sonic-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/28B01J20/22B01J20/30C02F1/28C02F101/30C02F101/38
CPCB01J20/28009B01J20/226C02F1/285C02F2101/306C02F2101/38
Inventor 林祥萍齐沛沛王新全王娇狄珊珊王强
Owner ZHEJIANG ACADEMY OF AGRICULTURE SCIENCES
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