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Quaternary ammonium salt type hyperbranched polysulfide modified polymer microspheres and preparation method

A technology of polysulfide and quaternary ammonium salt, which is applied in the field of synthesis of porous polymer pellets, can solve the problems of shortening the service life of fungicides, non-recyclable fungicides, and loss of fungicide molecules, so as to achieve safe service life and increase dosage , The effect of simplifying the production steps

Active Publication Date: 2022-01-28
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the fungicide molecules will be lost due to dissolving in water, which not only shortens the service life of the fungicide, but also causes different degrees of pollution to the water source; after contacting with humans and animals, it will penetrate into the skin of humans and animals, causing certain damage to the health of organisms harm
[0004] That is, the bactericide molecules in the prior art will cause the loss of bactericidal groups on the one hand after being dissolved in water, and on the other hand, the existing bactericides cannot be recycled

Method used

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  • Quaternary ammonium salt type hyperbranched polysulfide modified polymer microspheres and preparation method
  • Quaternary ammonium salt type hyperbranched polysulfide modified polymer microspheres and preparation method
  • Quaternary ammonium salt type hyperbranched polysulfide modified polymer microspheres and preparation method

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Embodiment 1

[0057] A kind of synthetic method of the polymer microsphere of quaternary ammonium salt type hyperbranched polysulfide modification, comprises the following steps:

[0058] S1: Under nitrogen protection conditions, add allyl glycidyl ether (313.5mg, 2.746mmol), cysteamine hydrochloride (312.5mg, 2.750mmol), benzoin dimethyl ether (27.8mg, 0.11mmol) and 2.027g of methanol were added to the rotor and sealed with a rubber stopper, then placed in an ice-water bath at 0°C, and irradiated with ultraviolet light with a wavelength of 365nm for continuous reaction for 10 hours. Precipitate the obtained product in a mixed solution of anhydrous ether and petroleum ether (volume ratio 3:2), and obtain an α-epoxy-ω-ammonium intermediate after drying;

[0059] S2: Add epoxy-based porous polymer microspheres (200mg), the α-epoxy-ω-ammonium-based intermediate (200.3mg) obtained in step S1, 1.53g methanol, a stirring magnet, and rubber Plug and seal, and stir and mix evenly with a magnetic s...

Embodiment 2

[0066] A kind of synthetic method of the polymer microsphere of quaternary ammonium salt type hyperbranched polysulfide modification, comprises the following steps:

[0067] S1: Under nitrogen protection conditions, add allyl glycidyl ether (792.9mg, 6.945mmol), cysteamine hydrochloride (790.5mg, 6.954mmol), 2-hydroxy-2- Methyl-1-phenyl-1-propanone (51.1mg, 0.30mmol) and 7.42g methanol were added to the rotor and sealed with a rubber stopper, then placed in an ice-water bath at 0°C, and irradiated with ultraviolet light with a wavelength of 365nm for continuous reaction 10 hours. Precipitate the obtained product in a mixed solution of anhydrous ether and petroleum ether (volume ratio 3:2), and obtain an α-epoxy-ω-ammonium intermediate after drying;

[0068] S2: Add epoxy-based porous polymer microspheres (7.2mg), the α-epoxy-ω-ammonium-based intermediate (720.6mg) obtained in the S1 step, 7.53g methyl alcohol, and a stirring magnet in a round-bottomed flask, and use The rubb...

Embodiment 3

[0074] A kind of synthetic method of the polymer microsphere of quaternary ammonium salt type hyperbranched polysulfide modification, comprises the following steps:

[0075] S1: Add allyl glycidyl ether (242.0mg, 2.125mmol), cysteamine hydrochloride (241.3mg, 2.123mmol), 2,4,6- Trimethylbenzoyldiphenylphosphine oxide (29.1mg, 0.09mmol) and 5.59g methanol were added to the rotor and sealed with a rubber stopper, then placed in an ice-water bath at 0°C, and irradiated with ultraviolet light with a wavelength of 365nm for continuous reaction 10 hours. Precipitate the obtained product in a mixed solution of anhydrous ether and petroleum ether (volume ratio 3:2), and obtain an α-epoxy-ω-ammonium intermediate after drying;

[0076] S2: Add epoxy-based porous polymer microspheres (40.0mg), the α-epoxy-ω-ammonium-based intermediate (200.6mg) obtained in the S1 step, 3.71g methanol, and a stirring magnet in a round-bottomed flask, and use The rubber stopper was sealed, and the mixtur...

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Abstract

The invention discloses polymer microspheres modified by quaternary ammonium salt type hyperbranched polysulfide and a preparation method. In the present invention, under photoinitiated conditions, polyethylene glycol is used as a porogen, and alkyldithiol, propargyl glycidyl ether and 1,7-octadiyne are used as raw materials, and mercapto-alkyne addition suspension polymerization is used. Methods Prepared epoxy-based microporous polymer beads; then at 0°C, using methanol as a solvent, using ultraviolet light to trigger the reaction of allyl glycidyl ether and cysteamine hydrochloride to synthesize α‑epoxy‑ω ‑ammonium-based intermediate; then, in a solvent and at 60°C, epoxy-based microporous polymer beads, α-epoxy-ω-ammonium-based intermediate and sodium methoxide synthesize hyperbranched polysulfide ammonium in one step Modified polymer microspheres. The obtained product has a good killing effect on Escherichia coli, and the modified polymer microspheres can be recovered and reused through simple filtration.

Description

technical field [0001] The invention relates to a reusable polysulfide bactericide, which belongs to the field of functional polymer materials, and in particular to a synthesis method of porous polymer beads with a surface-grafted hyperbranched polysulfide structure and an application of the bactericide. Background technique [0002] Hyperbranched polymers are a class of macromolecules with a special three-dimensional structure, with small hydrodynamic radius, low viscosity, and reactive functional groups located at the ends of the molecules, so hyperbranched molecules have high reactivity. Compared with the synthesis process of dendrimers, the synthesis process of hyperbranched polymers is simple, does not require complicated purification steps, and can be synthesized in large quantities by "one-pot method". Therefore, hyperbranched polymers have been widely used as pigment dispersants for paints, tougheners for brittle plastics, enhancers for adhesives, slow-release carrie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/02A01N33/12A01P3/00A01P1/00C08G75/045
CPCA01N33/12B01J13/02C08G75/045
Inventor 郑耀臣张谦刘健陈浩高璇巩攀
Owner YANTAI UNIV
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