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Intumescent flame retardant of star borate derivatives and preparation method thereof

A technology of intumescent flame retardants and borate esters, applied in chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, organic chemistry, etc., can solve the problems of weak flame retardancy and toxicity, and achieve Effects of preventing burning, preventing dripping, and lowering surface temperature

Active Publication Date: 2018-07-20
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 star borate derivatives and preparation method thereof
  • Intumescent flame retardant of star borate derivatives and preparation method thereof
  • Intumescent flame retardant of star borate derivatives and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Step 1: Dissolve 2.58g of phloroglucinol and 9.11g of N,N-diisopropylethylamine in 40ml of tetrahydrofuran solution (mixture 1), dissolve 16.79g of cyanuric chloride in 80ml of tetrahydrofuran solution, and Stir fully in an ice water bath for 31 minutes (mixture 2), add mixture 1 dropwise to mixture 2, stir at 5°C for 3 hours, and filter;

[0031] Step 2: Use a rotary evaporator to remove the tetrahydrofuran in the filtrate of the second step to obtain a white solid. Use a mixture of petroleum ether and acetone (volume ratio of 3:1) as the washing liquid and separate with a chromatographic column to obtain the intermediate product 1;

[0032] The third step: Add 7.5ml ethylene glycol and 20ml toluene (as a water-carrying agent) solution in a three-necked flask, stir and gradually raise the temperature to 42℃, add 7.34g boric acid, continue to raise the temperature to 88℃, and stir for 47 minutes until the boric acid is complete Dissolve; wait for the moisture in the water s...

Embodiment 2

[0040] Step 1: Dissolve 5.23g phloroglucinol and 18.37g N,N-diisopropylethylamine in 80ml tetrahydrofuran solution (mixture 1), dissolve 35.31g cyanuric chloride in 80ml tetrahydrofuran solution, and Stir fully in an ice water bath for 31 minutes (mixture 2), add mixture 1 dropwise to mixture 2, stir at 5°C for 3 hours, and filter;

[0041] Step 2: Use a rotary evaporator to remove the tetrahydrofuran in the filtrate of the second step to obtain a white solid. Use a mixture of petroleum ether and acetone (volume ratio of 3:1) as the washing liquid and separate with a chromatographic column to obtain the intermediate product 1;

[0042] The third step: Add 14ml ethylene glycol and 40ml toluene (as a water-carrying agent) solution in a three-necked flask, stir and gradually raise the temperature to 42℃, add 14.89g boric acid, continue to raise the temperature to 88℃, stir for 47 minutes until the boric acid is completely dissolved ; When the moisture in the water separator no longer...

Embodiment 3

[0046] The first step: Dissolve 7.76g phloroglucinol and 27.29g N,N-diisopropylethylamine in 120ml tetrahydrofuran solution (mixture 1), dissolve 49.63g cyanuric chloride in 240ml tetrahydrofuran solution, and Stir fully in an ice water bath for 37 minutes (mixture 2), add mixture 1 dropwise to mixture 2, stir at 3°C ​​for 5 hours, and filter;

[0047] Step 2: Use a rotary evaporator to remove the tetrahydrofuran in the filtrate of the second step to obtain a white solid. Use a mixture of petroleum ether and acetone (volume ratio of 3:1) as the washing liquid and separate with a chromatographic column to obtain the intermediate product 1;

[0048] The third step: Add 20.5ml ethylene glycol and 60ml toluene (as a water-carrying agent) solution into a three-necked flask, stir and gradually raise the temperature to 47℃, add 22.67g boric acid, continue to raise the temperature to 70℃, and stir for 55 minutes until the boric acid is complete Dissolve; wait for the moisture in the water...

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Abstract

The invention discloses an intumescent flame retardant of a star-shaped boric acid ester derivative and a preparation method of the intumescent flame retardant. The star-shaped boric acid ester derivative is 1,3,5-three-{4,6-two-([1,3,2] dioxaborolane-2-oxo)-1,3,5-triazine-2-oxo} benzene. When the intumescent flame retardant is prepared, phloroglucinol and N, N-diisopropylethylamine are added into tetrahydrofuran solution; mixed solution is dripped into tetrahydrofuran solution of cyanuric chloride, stirred, filtered and separated to obtain intermediate products 1; ethylene glycol and methylbenzene are stirred and mixed, temperature is gradually risen, boric acid is added, the temperature continues to be risen, and backflow and reaction are performed; the methylbenzene is removed, and drying is performed to obtain intermediate products 2; the intermediate products 2 are dissolved in the tetrahydrofuran solution under protection of nitrogen, sodium hydroxide is added, the tetrahydrofuran solution with the intermediate products 1 is added in batches, and continuous reaction is performed for 3-6 hours; purification is performed to obtain target products. The obtained products can serve as excellent environment-friendly organic flame retardants.

Description

Technical field [0001] The invention relates to an environment-friendly flame-retardant polymer material, in particular to an intumescent flame retardant based on a star-shaped borate derivative 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 pose a huge threat to people's property and lives, so flame retardants are very important. Flame retardants can be divided into inorganic flame retardants and organic flame retardants according to their properties. Inorganic flame retardants have the advantages of low smoke, low toxicity, halogen-free, good stability, and low price. Disadvantages such as poor tolerance and reduced material properties are limited to a certain extent. The traditional organophosphorus and or...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F5/04C08K5/55C08L63/02
CPCC07F5/04C08K5/55C08L2201/02C08L63/00
Inventor 曾金明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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