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Pentamine guanidine phosphate oligomer, preparation method thereof and antibacterial polymer prepared from pentamine guanidine phosphate oligomer

A technology of guanidinium pentamethylenediamine phosphate and oligomers, which is applied in the manufacture of rayon, single-component polyamide rayon, textiles and papermaking, etc., and can solve problems such as limited applications

Active Publication Date: 2021-06-15
CATHAY R&D CENT CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Guanidine-based polymers with good antibacterial properties have good water solubility and are convenient to use in water systems, but at the same time limit their application in the field of hydrophobic polymer materials

Method used

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  • Pentamine guanidine phosphate oligomer, preparation method thereof and antibacterial polymer prepared from pentamine guanidine phosphate oligomer
  • Pentamine guanidine phosphate oligomer, preparation method thereof and antibacterial polymer prepared from pentamine guanidine phosphate oligomer
  • Pentamine guanidine phosphate oligomer, preparation method thereof and antibacterial polymer prepared from pentamine guanidine phosphate oligomer

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preparation example Construction

[0029] In one embodiment, the preparation method of guanidinium pentamethylenediamine phosphate oligomer comprises: reacting pentamethylenediamine and guanidine phosphate at 90-140°C for 2-5 hours, then raising the temperature to 170-190°C for 2-15 hours. hours to obtain the first oligomer; then add an organic compound to the first oligomer and continue to react for 1 to 5 hours (for amidation or ring-opening reaction) to obtain pentamethylenediamine phosphate guanidinium oligomer.

[0030] In the preparation of the guanidinium pentamethylenediamine phosphate oligomer according to one embodiment of the present invention, the addition amount of the organic compound is 0.5 to 25 wt % (relative to the mass of the first oligomer), preferably 1 to 15 wt %, for example 1.5 wt % wt%, 2wt%, 3wt%, 5wt%, 6wt%, 6.56wt%, 7.5wt%, 8wt%, 8.09wt%, 10wt%, 12wt%, 15wt%, 20wt%, etc.

[0031] In one embodiment, the molar ratio of pentamethylenediamine to guanidine phosphate is 1:(1˜1.2), such as ...

Embodiment 1

[0054] Preparation of guanidinium pentamethylenediamine phosphate oligomer A1

[0055] Get 102g of pentamethylenediamine and 238g of guanidine phosphate (pentamethylenediamine: guanidine phosphate (mol / mol)=1:1.1) into a 500ml three-necked flask, stir and heat up to 130°C under nitrogen protection, react for 2.5h, and then heat up After 8 hours of reaction at 170°C, 305 g of the first oligomer was obtained. Then, in the first oligomer, add 20g (6.56wt%) pyromellitic anhydride again, keep temperature constant, continue reaction 1h, obtain the pentamethylenediamine phosphate guanidinium oligomer containing terminal anhydride group (several Average molecular weight 2650Da), marked as A1.

[0056] Preparation of antibacterial polyamide B1

[0057] Take 18g of guanidinium pentamethylenediamine phosphate oligomer A1, mix it with 700g of polyamide 66, put it into a twin-screw extruder, melt and blend at 260°C, and the reaction time of the materials in the screw is 3 minutes. Throu...

Embodiment 2

[0059] Preparation of Pentamethylenediamine Phosphate Guanidinium Oligomer A2

[0060] Take 102g of pentamethylenediamine and 255g of guanidine phosphate (pentamethylenediamine: guanidine phosphate (mol / mol)=1:1.05) and add them to a 500ml three-neck flask, stir and heat up to 130°C under nitrogen protection, react for 2.5h, and then heat up After 15 hours of reaction at 180°C, 320 g of the first oligomer was obtained. Then, in the first oligomer, add 4.8g (1.50wt%) ethylene glycol diglycidyl ether and continue to react for 2h, obtain the pentamethylenediamine phosphate guanidinium oligomer (number-average molecular weight 11000Da ), marked as A2.

[0061] Preparation of antibacterial polyamide B2

[0062] Take 10g of guanidinium pentamethylenediamine phosphate oligomer A2, mix it with 1990g of polyamide 56, put it into a twin-screw extruder, melt and blend at 245°C, and the reaction time of the materials in the screw is 5 minutes. Through the reaction between the terminal ...

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Abstract

The invention provides a pentamethylene diamine guanidine phosphate oligomer, a preparation method of the pentamethylene diamine guanidine phosphate oligomer and an antibacterial polymer prepared from the pentamethylene diamine guanidine phosphate oligomer. The pentamethylene diamine guanidine phosphate oligomer has a structure shown in the specification, wherein X is selected from C5-C50 organic groups containing active groups, and the active groups comprise one or more of anhydride groups, isocyanate groups, epoxy groups and oxazoline groups; and Y is hydrogen or X, and n is the number of repetitive units and ranges from 3 to 50. The antibacterial polymer based on pentamethylene diamine guanidine phosphate disclosed by one embodiment of the invention has relatively high antibacterial property and mechanical property, and can be applied to the fields of polyamide fibers, films and plastic products.

Description

technical field [0001] The invention relates to an oligomer of pentamethylenediamine (1,5-pentamethylenediamine) and guanidinium phosphate, specifically a pentamethylenediamine phosphate guanidinium oligomer that can be used for antibacterial polymers, and belongs to the synthesis and application of antibacterial agents technology field. Background technique [0002] Microorganisms widely exist in the natural environment and human environment. They can be used in food processing and brewing, but at the same time, in the world, harmful microorganisms have long endangered human health and life, and also endangered agriculture and animal husbandry. development, resulting in economic losses, and even a heavy blow to human civilization. In recent years, experts and scholars from all walks of life have begun to pay attention to the exploration and development of antibacterial agents and antibacterial materials. How to effectively inhibit the growth and reproduction of harmful mic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/00C08G69/42C08G81/00C08L77/06D01F6/90D01F1/10C08J5/18C08L77/02C08L87/00
CPCC08G73/00C08G69/42C08G81/00D01F6/90D01F1/103C08J5/18C08J2377/06C08J2377/02C08J2487/00Y02A50/30
Inventor 管涌赵元博申屠烜钰王莉莉危大福许祥刘修才
Owner CATHAY R&D CENT CO LTD
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