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Novel organophosphorus flame retardant and preparation method thereof

An organophosphorus and flame retardant technology, applied in the field of flame retardants, can solve the problems of insignificant effect, low operation efficiency, scarcity of flame retardants, etc., and achieve excellent antibacterial durability, great application prospects, and excellent synergistic flame retardancy. Effect

Inactive Publication Date: 2021-06-01
东莞市道尔新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Textiles have flame retardant and antibacterial and antifungal functions at the same time need to add a variety of additives at the same time, the operation efficiency is low, and even the effect is not obvious
[0006] Flame retardants with antibacterial and antifungal functions are very scarce in the market

Method used

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  • Novel organophosphorus flame retardant and preparation method thereof
  • Novel organophosphorus flame retardant and preparation method thereof
  • Novel organophosphorus flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Embodiment 1: A kind of preparation method of novel organophosphorus flame retardant comprises the following steps:

[0035] (1) Add 1 mol of 2-amino-4,6-dichloropyrimidine, 2 mol of allylamine, and 4 mol of triethylamine into a flask containing a mixed solvent of 30 mol of hexane and ethyl acetate (volume ratio 1 / 1) , stirring at room temperature for 24h, after the reaction, add 40mol deionized water to the mixture, separate the liquid, take the organic phase, distill under reduced pressure, and dry in vacuo to obtain the intermediate product I;

[0036] The infrared data of the intermediate product I are as follows: 3121cm -1 : -NH- exists; 3342cm -1 :-NH 2 Spike exists; 1580cm -1 、1490cm -1 、1440cm -1 : presence of pyrimidine ring; 1611cm -1 :-C=C-exists; 706cm -1 :-C-Cl disappears.

[0037] (2) Dissolve 1mol I and 1.2mol DOPO in 50mol 1,4-dioxane and add to the flask, then add 1wt% AIBN and put it in the flask, put it in an oil bath at 80°C for 8h, after the...

Embodiment 2

[0044] Embodiment 2: A kind of preparation method of novel organophosphorus flame retardant comprises the following steps:

[0045] (1) Add 1mol 2-amino-4,6-dichloropyrimidine, 2mol allylamine, and 4mol triethylamine into a flask containing 30mol hexane and ethyl acetate mixed solvent (volume ratio 2 / 1) , stirred at room temperature for 20 h, after the reaction was completed, 40 mol of deionized water was added to the mixture, the liquid was separated, and the organic phase was taken, distilled under reduced pressure, and dried in vacuo to obtain the intermediate product I;

[0046] The infrared data of the intermediate product I are as follows: 3118cm -1 : -NH- exists; 3340cm -1 :-NH 2 Spikes present; 1575cm -1 、1488cm -1 、1439cm -1 : presence of pyrimidine ring; 1610cm -1 :-C=C-exists; 705cm -1 :-C-Cl disappears.

[0047] (2) Dissolve 1 mol I and 1 mol DOPO in 50 mol 1,4-dioxane and add to the flask, then add 2wt% AIBN and put it in the flask, and put it in an oil ba...

Embodiment 3

[0054] Embodiment 3: A kind of preparation method of novel organophosphorus flame retardant comprises the following steps:

[0055] (1) Add 1mol 2-amino-4,6-dichloropyrimidine, 2mol allylamine, and 4mol triethylamine into a flask containing 30mol hexane and ethyl acetate mixed solvent (volume ratio 1 / 2) , stirring at room temperature for 21h, after the reaction, add 40mol deionized water to the mixture, separate the liquid, take the organic phase, distill under reduced pressure, and dry in vacuo to obtain the intermediate product I;

[0056] The infrared data of intermediate product I are as follows: 3120cm -1 : -NH- exists; 3340cm -1 :-NH 2 Spike exists; 1580cm -1 、1490cm -1 、1440cm -1 : presence of pyrimidine ring; 1610cm -1 :-C=C-exists; 706cm -1 :-C-Cl disappears.

[0057] (2) Dissolve 1mol I, 1.1mol DOPO in 50mol 1,4-dioxane and add to the flask, then add 1.5wt% AIBN and put it in the flask, put it in an oil bath at 75°C for 10h, after the reaction, distill under ...

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Abstract

The invention discloses a novel organophosphorus flame retardant and a preparation method thereof, and the preparation method comprises the following steps: by taking 2-amino-4,6-dichloropyrimidine, allylamine, DOPO, a bifunctional epoxy compound and 1-aminohexyl guanidine hydrochloride as raw materials, carrying out substitution, addition, epoxy ring opening and other multi-step reactions to obtain a novel organophosphorus flame retardant material. The novel flame retardant not only effectively solves the problems that an existing common flame retardant has poor flame retardant effect, needs to be added in quantity and has single function, but also has efficient broad-spectrum antibacterial property, and does not influence the mechanical property of the final material. The material is particularly suitable for the fields of indoor decoration materials such as non-woven fabrics and synthetic leather, and is wide in application range.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a novel organophosphorus flame retardant and a preparation method thereof. Background technique [0002] Due to the popularity of polymers such as textiles and synthetic leather, they are also receiving more and more attention in the field of fire safety. Most textiles are too flammable. As one of the most commonly used textile raw materials, cotton fiber has a limiting oxygen index of only 18%, which is extremely flammable and causes fires that endanger human life and property. Therefore, it must be flame-retardant finished to improve its fire resistance. [0003] The most commonly used method is to add a flame retardant with flame retardant function to the polymer system. However, currently commonly used flame retardants are toxic or release toxic gas and smoke during combustion, and a large amount of addition is required to achieve the flame retardant level. [0004...

Claims

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Application Information

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IPC IPC(8): C07F9/6574A01N57/24A01P3/00A01P1/00C08K5/5313C08L75/08C08J9/00C09K21/12
CPCC07F9/657172A01N57/24C08K5/5313C08J9/0038C09K21/12C08J2375/08
Inventor 查皓查家华谢旭鹏
Owner 东莞市道尔新材料科技有限公司
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