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Intumescent flame retardant of borate derivative and preparation method thereof

A technology of intumescent flame retardants and derivatives, applied in the field of intumescent flame retardants, can solve problems such as toxicity and weak flame retardant performance, and achieve the effects of preventing dripping, preventing combustion, and stabilizing the carbon layer

Active Publication Date: 2017-01-11
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 of borate derivative and preparation method thereof
  • Intumescent flame retardant of borate derivative and preparation method thereof
  • Intumescent flame retardant of borate derivative and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The first step: 2.58g phloroglucinol and 9.11gN, N-diisopropylethylamine are dissolved in 40ml tetrahydrofuran solution (mixture 1), 16.79g cyanuric chloride is dissolved in 80ml tetrahydrofuran solution, and Fully stir in an ice-water bath for 31 minutes (mixed solution 2), add mixed solution 1 dropwise to mixed solution 2, stir at 5°C for 3 hours, and filter;

[0030] The second step: use a rotary evaporator to remove tetrahydrofuran in the filtrate of the second step to obtain a white solid, use a mixture of petroleum ether and acetone (3:1 by volume) as a flushing solution, and separate with a chromatographic column to obtain an intermediate product 1;

[0031] Step 3: Add 13.5ml ethylene glycol and 30ml toluene solution into the three-necked flask, stir and gradually raise the temperature to 42°C, add 7.34g boric acid, continue to heat up to 88°C, stir for 47 minutes until the boric acid is completely dissolved; The moisture was no longer increased, and the reacti...

Embodiment 2

[0039] The first step: 5.23g phloroglucinol and 18.37g N,N-diisopropylethylamine are dissolved in 80ml tetrahydrofuran solution (mixture 1), 35.31g cyanuric chloride is dissolved in 80ml tetrahydrofuran solution, And fully stir in the ice-water bath for 31min (mixed solution 2), add the mixed solution 1 dropwise to the mixed solution 2, stir at 5°C for 3h, and filter;

[0040] The second step: use a rotary evaporator to remove tetrahydrofuran in the filtrate of the second step to obtain a white solid, use a mixture of petroleum ether and acetone (3:1 by volume) as a flushing solution, and separate with a chromatographic column to obtain an intermediate product 1;

[0041] Step 3: Add 27ml of ethylene glycol and 60ml of toluene solution into the three-necked flask, stir and gradually heat up to 42°C, add 14.89g of boric acid, continue to heat up to 88°C, and stir for 47 minutes until the boric acid is completely dissolved; Continue to react for 2.5 h without further increase; ...

Embodiment 3

[0045] The first step: 7.76g phloroglucinol and 27.29gN, N-diisopropylethylamine are dissolved in 120ml tetrahydrofuran solution (mixture 1), 49.63g cyanuric chloride is dissolved in 240ml tetrahydrofuran solution, and Fully stir in an ice-water bath for 37 minutes (mixed solution 2), add mixed solution 1 dropwise to mixed solution 2, stir at 3°C ​​for 5 hours, and filter;

[0046] The second step: use a rotary evaporator to remove tetrahydrofuran in the filtrate of the second step to obtain a white solid, use a mixture of petroleum ether and acetone (3:1 by volume) as a flushing solution, and separate with a chromatographic column to obtain an intermediate product 1;

[0047] Step 3: Add 41ml of ethylene glycol and 90ml of toluene (as a water-carrying agent) solution into the three-necked flask, stir and gradually heat up to 47°C, add 22.67g of boric acid, continue to heat up to 70°C, and stir for 55 minutes until the boric acid is completely dissolved ; When the moisture in...

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Abstract

The invention discloses an intumescent flame retardant of a borate derivative and a preparation method thereof. The name of the borate derivative is 1,3,5-tris-{4,6-bis-[([1,3,2] dioxaborolan-2-oxo)-oxethyl]-1,3,5-triazine-2-oxo}benzene. During preparation, phloroglucinol and N-ethyldiisopropylamine are added into a tetrahydrofuran solution and dropwisely added into the tetrahydrofuran solution of cyanuric chloride, and filtering is performed after the reaction; purification is performed to obtain an intermediate product 1; ethylene glycol and methylbenzene are stirred and mixed, boric acid is added, the temperature is increased continuously, stirring and backflow are performed, methylbenzene is removed, vacuum drying is performed, and an intermediate product 2 is obtained; under the nitrogen protection, the intermediate product 2 is dissolved into the tetrahydrofuran solution, then, sodium hydroxide is added, the tetrahydrofuran solution with the intermediate product 1 is added in batches, and a reaction is performed; suction filtration is performed, liquid-phase spinning drying is performed, and separation is performed to obtain the intumescent flame retardant of the borate derivative. The borate derivative can be adopted as the good environment-friendly organic fire retardant.

Description

technical field [0001] The invention relates to an intumescent flame retardant, in particular to an environment-friendly intumescent flame retardant based on star borate derivatives and a preparation method thereof. Background technique [0002] Compared with traditional inorganic metal materials, polymer materials have their own unique advantages, and they play an increasingly important role in the national economy and people's lives. However, most polymer materials are flammable materials, which will pose a huge threat to people's property and life, so flame retardants are very important. 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 as poor capacitance and reduced material performance are limited to a certain extent. Although the traditional organophosp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K7/22C08K5/55C07F5/04C08L63/00
CPCC07F5/04C08K5/55C08K7/22C08L2201/02C08L63/00
Inventor 万之君陈珊珊刘平刘伟时张铁潘永红刘东发徐添贵
Owner SOUTH CHINA UNIV OF TECH
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