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Intumescent flame retardant based on star triazine derivatives and preparation method thereof

A technology of intumescent flame retardants and triazine derivatives, which is applied in the field of intumescent flame retardants and their preparation, can solve the problems of toxicity and weak flame retardant performance, prevent dripping, prevent burning, and solve the problems of high toxicity Effect

Active Publication Date: 2018-06-29
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Boron, phosphorus and nitrogen are all flame retardant elements. Although organic phosphorus flame retardants containing flame retardant phosphorus in the organic molecular structure have good flame retardant properties, they have certain toxicity.
While the organic nitrogen flame retardant containing only one flame retardant element nitrogen in the organic molecular structure is non-toxic, but its flame retardant performance is relatively weak.

Method used

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  • Intumescent flame retardant based on star triazine derivatives and preparation method thereof
  • Intumescent flame retardant based on star triazine derivatives and preparation method thereof
  • Intumescent flame retardant based on star triazine derivatives and preparation method thereof

Examples

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Effect test

Embodiment 1

[0030] A preparation method of an intumescent flame retardant based on a star triazine derivative, comprising the steps of:

[0031] Step 1: Add 13.5ml of ethylene glycol and 140ml of toluene into a three-necked flask, stir and gradually raise the temperature to 48°C, add 7.35g of boric acid, continue to heat up to 73°C, and stir for 50 minutes until the boric acid is completely dissolved; No more increase, continue to react for 1h;

[0032] Step 2: Distill the reaction solution in the first step to remove toluene under reduced pressure, and dry it in vacuum at 70° C. to obtain an intermediate product of a colorless transparent viscous liquid; dissolve 12.29 g of the intermediate product in 60 ml of tetrahydrofuran solution;

[0033] The third step: under the protection of nitrogen, weigh 5.67g of cyanuric chloride and dissolve it in 40ml of tetrahydrofuran solution, then add 4.11g of sodium hydroxide, and at 26°C, add half of the volume of the tetrahydrofuran solution in whic...

Embodiment 2

[0039] A preparation method of an intumescent flame retardant based on a star triazine derivative, comprising the steps of:

[0040] Step 1: Add 27ml of ethylene glycol and 270ml of toluene into the three-necked flask, stir and gradually raise the temperature to 59°C, add 14.76g of boric acid, continue to raise the temperature to 81°C, and stir for 55 minutes until the boric acid is completely dissolved; Increase again, continue to react for 2h;

[0041] Step 2: Distill the reaction solution of the first step to remove toluene under reduced pressure, and dry it in vacuum at 70° C. to obtain an intermediate product of a colorless transparent viscous liquid; dissolve 25.57 g of the intermediate product in 120 ml of tetrahydrofuran solution;

[0042] The third step: under the protection of nitrogen, weigh 11.32g of cyanuric chloride and dissolve it in 80ml of tetrahydrofuran solution, then add 8.56g of sodium hydroxide, at 20°C, add 40% of the volume of the intermediate product tet...

Embodiment 3

[0045] A preparation method of an intumescent flame retardant based on a star triazine derivative, comprising the steps of:

[0046] Step 1: Add 41ml of ethylene glycol and 420ml of toluene into the three-necked flask, stir and gradually raise the temperature to 58°C, add 22.14g of boric acid, continue to raise the temperature to 73°C, and stir for 50 minutes until the boric acid is completely dissolved; Increase again, continue to react for 2h;

[0047] Step 2: Distill the reaction liquid of the first step to remove toluene under reduced pressure, and dry it in vacuum at 70° C. to obtain an intermediate product of a colorless transparent viscous liquid; dissolve 36.89 g of the intermediate product in 180 ml of tetrahydrofuran solution;

[0048] The third step: under the protection of nitrogen, take by weighing 17.32g cyanuric chloride and dissolve in 120ml tetrahydrofuran solution, then add 12.43g sodium hydroxide, at 24 ℃, add 60% of the volume of the tetrahydrofuran solutio...

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Abstract

The invention discloses a star-like triazine derivative-based intumescent flame retardant and a preparation method thereof. The name of star-like triazine derivative is 2,4,6,-tri-{2-([1,3,2] dioxo-boron pentanenitrile ring-2-oxo)-oxethyl}-1,3,5-triazine which is used as the intumescent flame retardant. The preparation method comprises the following steps: mixing methylbenzene and ethylene glycol, heating to 40 to 60 DEG C, adding boric acid, heating, and stirring until the boric acid is dissolved completely; performing stirring and refluxing until the moisture content in a water knockout trap is not increased any more, and preserving the temperature for continuous reaction for 2 to 5 h; performing vacuum distillation on reaction liquid in the first step to remove methylbenzene, and performing vacuum drying to obtain an intermediate product; dissolving the intermediate product into a tetrahydrofuran solution; under the nitrogen protection, dissolving cyanuric chloride into the tetrahydrofuran solution, and then adding sodium hydroxide; adding the tetrahydrofuran solution with the intermediate product step by step, and performing purification to obtain the star-like triazine derivative. The product obtained by the preparation method can be used as a good environment-friendly organic flame retardant.

Description

technical field [0001] The invention relates to the technical field of flame retardant of organic polymer materials, in particular to an intumescent flame retardant based on a star triazine derivative and a preparation method thereof. Background technique [0002] Large and small fires occur almost every day all over the world, mainly caused by the ignition of flammable materials. With the development of modern science and technology, polymer materials play an increasingly important role in the national economy and people's lives. However, general polymer materials are flammable, and the use of flame retardants can reduce the combustion performance of polymer materials, thereby effectively reducing fire losses. Flame retardants can be divided into inorganic flame retardants and organic flame retardants according to their attributes. Inorganic flame retardants have the advantages of low smoke, low toxicity, halogen-free, good stability, and low price. The disadvantages such...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/55C07F5/04C08L63/00
CPCC07F5/04C08K5/55C08L2201/02C08L63/00
Inventor 陈珊珊张铁刘平刘伟时潘永红刘东发徐添贵
Owner SOUTH CHINA UNIV OF TECH
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