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Polycation quaternary ammonium salt high polymer material and preparation method thereof

A polymer material and polycation technology, applied in the field of polycation quaternary ammonium salt polymer material and its preparation, can solve problems such as undiscovered, and achieve the effects of stable performance, novel structure and easy processing

Active Publication Date: 2016-04-27
广州永翔科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Based on domestic and foreign literature and patents, we have not found any reports on polycationic quaternary ammonium salt polymer materials based on polyoxetane

Method used

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  • Polycation quaternary ammonium salt high polymer material and preparation method thereof
  • Polycation quaternary ammonium salt high polymer material and preparation method thereof
  • Polycation quaternary ammonium salt high polymer material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] HCl 3 Preparation of Ox monomer:

[0055] Stir 1,3-dichloropropane (10.5g, 93mmol), 3-hydroxymethyloxetane (2.7g, 31mmol), sodium hydroxide (20g, 500mmol) in a two-phase system of n-hexane and water Homogenously, use tetrabutylammonium bromide as a phase transfer catalyst, and react under reflux conditions for 0.5 hours. After the reaction was completed, it was purified by extraction and vacuum distillation to obtain a colorless liquid. Yield: 55%. 1 HNMR (300MHz, CDCl 3 ): δ1.74 (m, 2H, -CH 2 -CH 2 -CH 2 -Cl), δ3.01 (m, 1H, -CH-), δ3.36 (m, 6H, -CH 2 -O-CH 2 -CH 2 -CH 2 -Cl), δ4.34-4.51 (dd, 4H, -CH on the four-membered ring 2 -O-CH 2 -).

[0056] HE 1 Preparation of Ox monomer:

[0057] Ethylene glycol monomethyl ether (12.9g, 170mmol) was reacted with sodium hydride (4g, 170mmol) in anhydrous tetrahydrofuran until no bubbles were generated, and then 3-(p-toluenesulfonate methyl)oxy Heterocyclobutane (41.2 g, 170 mmol) was added dropwise to the reactio...

Embodiment 2

[0063] MeBr 4 Preparation of Ox monomer:

[0064] 1,4-dibromobutane (20g, 93mmol) and 3-methyl-3-hydroxymethyl oxetane (3.1g, 31mmol), sodium hydroxide (20g, 500mmol) in n-hexane and water Stir evenly in the two-phase system, use tetrabutylammonium bromide as a phase transfer catalyst, and react under reflux conditions for 0.5 hours. After the reaction was completed, it was purified by extraction and vacuum distillation to obtain a colorless liquid. Yield: 80%. The NMR spectrum is shown in Fig. 1 HNMR (300MHz, CDCl 3 ): δ1.30 (s, 3H, -CH 3 ), δ1.73 (m, 2H, -CH 2 -CH 2 -Br), δ1.95 (m, 2H, -CH 2 -CH 2 -CH 2 -Br), δ3.47 (m, 6H, -CH 2 -O-CH 2 -CH 2 -CH 2 -CH 2 -Br), δ4.34-4.51 (dd, 4H, -CH on the four-membered ring 2 -O-CH 2 -).

[0065] MeE 2 Preparation of Ox monomer:

[0066] Diethylene glycol monomethyl ether (20g, 170mmol) was reacted with sodium hydride (4g, 170mmol) in anhydrous tetrahydrofuran until no bubbles were produced, and then 3-methyl-3-(p-tolue...

Embodiment 3

[0072] Et 6 Preparation of Ox monomer:

[0073] 1,6-diiodohexane (31.4g, 93mmol) and 3-ethyl-3-hydroxymethyl oxetane (3.6g, 31mmol), sodium hydroxide (20g, 500mmol) in n-hexane and Stir evenly in the water two-phase system, use tetrabutylammonium bromide as a phase transfer catalyst, and react under reflux for 0.5 hours. After the reaction was completed, it was purified by extraction and vacuum distillation to obtain a colorless liquid. Yield: 78%. 1 HNMR (300MHz, CDCl 3 ): δ0.90 (t,3H,-CH 2 -CH 3 ), δ1.20-1.50 (m, 6H, -CH 2 -CH 3 ,-CH 2 -CH 2 -CH 2 -CH 2 -I), δ1.72-1.95 (m, 4H, -O-CH 2 -CH 2 -CH 2 -CH 2 -CH 2 -CH 2 -I), δ3.47 (m, 6H, -CH 2 -O-CH 2 -CH 2 -CH 2 -CH 2 -CH 2 -CH 2 -I), δ4.34-4.51 (dd, 4H, -CH on the four-membered ring 2 -O-CH 2 -).

[0074] Et 4 Preparation of Ox monomer:

[0075]Tetraethylene glycol monomethyl ether (35.4g, 170mmol) was reacted with sodium hydride (4g, 170mmol) in anhydrous tetrahydrofuran until no bubbles were gener...

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Abstract

The invention belongs to the technical field of high polymer materials, and in particular relates to a polycation quaternary ammonium salt high polymer material and a preparation method thereof. The preparation method comprises: firstly, under an inert gas condition, carrying out ring-opening polymerization on an oxetane type monomer, a catalyst and an initiator in an anhydrous solvent, and then carrying out washing, drying, and reduced pressure distillation to remove the solvent, and carrying out refining and purification to obtain a polymer precursor; and under the inert gas condition, carrying out quaterisation on the obtained polymer precursor and excessive tertiary amine in the anhydrous solvent, and then carrying out high-vacuum-degree reduced pressure distillation to remove the solvent and the excessive tertiary amine so as to obtain the polycation quaternary ammonium salt high polymer material. The polycation quaternary ammonium salt high polymer material is novel in structure, has the advantages of board antibacterial spectrum, quickness, high efficiency, stable performance, indiffusion, impermeability, workability and the like, and can be widely applied to the aspects of skin nursing, wound cleaning, and antibacterial sterilization.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a polycation quaternary ammonium salt polymer material and a preparation method thereof. Background technique [0002] With the rapid development of human society and the continuous improvement of living standards, more and more people have found that microbial pathogenic bacteria have become the chief culprit of endangering human health and causing diseases and even death worldwide [1]. Especially in recent years, due to the abuse of antibiotics, antibiotic-resistant superbugs have emerged one after another, which has led to a global antibiotic crisis [2,3]. Therefore, it is imminent to develop new broad-spectrum, efficient, durable and renewable antibacterial agents. [0003] Since Heidelberger discovered the bactericidal effect of quaternary ammonium salts in 1915[4,5], quaternary ammonium salt fungicides have been widely used in materials, cosmetics, te...

Claims

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Application Information

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IPC IPC(8): C07C217/08C07C213/02A61P31/04A61P17/02
CPCC07C41/02C07C213/02C07C217/08C07D205/04C07C43/137C07C43/11
Inventor 赵鹏吴亮亮刘静林超文学军
Owner 广州永翔科技发展有限公司
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