Fire retardant containing boron phenyl phosphonic acid esters and preparation method thereof

A technology of boron phenyl phosphonate and flame retardant, which is applied in the field of boron-containing phenyl phosphonate flame retardant and its preparation, can solve the problems of low flame retardant efficiency, low impact performance of polymer materials, large dosage and the like , to achieve the effect of high flame retardancy and good compatibility

Active Publication Date: 2012-03-21
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This new compound described by this patented technology can be used alone or mixed with other substances like polyamide (PA) or epoxy resin for better heat resistance properties without affecting their overall quality. Its main advantage being that it remains stable even at room temperature but becomes more effective when added into plastics due to its unique chemical composition containing many benzenes instead of just one type called Phosphonium Fluorite. Additionally, certain types of phosporylidylflames have been found to contain specific elemental compositions made from boron oxides combined together through hydrogen bondings between them. These technical improvements make PFAs resistant against fire damage effectively while maintaining excellent mechanical strength over time.

Problems solved by technology

This patents discusses how increasingly important factors like safety standards require flammability resistance on polymer material surfaces such as those made up mainly of bifunctional compounds called diphenolsulfones and triphenyltoluene dimmers. These substances were developed over time due to their ability to absorb energy without generating harmful gas when burned. They could be added to other types of resin compositions to enhance its effectiveness against these threats. Additionally, they may contain chlorine free radicals that pose health concerns because they release noxious fumes even if burnt down. Therefore, there needs an effective method to create flamable and nonflaming products while reducing damage to humans and animals.

Method used

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  • Fire retardant containing boron phenyl phosphonic acid esters and preparation method thereof
  • Fire retardant containing boron phenyl phosphonic acid esters and preparation method thereof
  • Fire retardant containing boron phenyl phosphonic acid esters and preparation method thereof

Examples

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Embodiment 1

[0021] Add 0.30mol o-hydroxybenzyl alcohol and 90ml toluene into a 250ml three-necked flask equipped with a mechanical stirrer and a water separator, heat up to 90°C, add 0.09mol boric acid, then heat the system to a boiling state and react for 50 minutes, then cool , remove unreacted boric acid and o-hydroxybenzyl alcohol by filtration to obtain a hydroxybenzyl borate intermediate; add all the hydroxybenzyl borate intermediates to a spherical Add 0.30 mol of phenylphosphoryl dichloride and 60 ml of toluene to a 250ml four-neck flask connected to nitrogen with a condenser tube and an elbow connection, protect with nitrogen, react at 25°C for 12 hours, and remove excess phenylphosphoryl dichloride under reduced pressure. Chlorine and toluene; replace the decompression device with a reflux device, add 0.30mol phenol, react at 120°C for 2 hours, and then react at 150°C for 4 hours, remove excess phenol under reduced pressure, and place the resulting product in a vacuum oven at 60°...

Embodiment 2

[0025] Add 0.25mol p-hydroxybenzyl alcohol and 150ml xylene into a 500ml three-necked flask equipped with a mechanical stirrer and a water separator, heat up to 80°C, add 0.125mol trimethyl borate, and then heat the system to a boiling state for reaction For 40 minutes, cool, filter and remove boric acid and unreacted hydroxybenzyl alcohol to obtain hydroxybenzyl borate intermediate; add all the hydroxybenzyl borate intermediate to a machine equipped with a mechanical stirrer and connect the hydrogen chloride absorption through an elbow joint. Into a 500ml four-neck flask connected to nitrogen with the spherical condenser and the elbow of the device, add 0.50mol phenylphosphoryl dichloride, 1.46g AlCl 3 And 100ml of xylene, under nitrogen protection, react at 50°C for 8 hours, remove excess phenylphosphoryl dichloride and xylene under reduced pressure; replace the decompression device with a reflux device, add 1.0mol phenol, and react at 130°C After 2 hours and 3 hours at 160°...

Embodiment 3

[0029]Add 0.30mol of m-hydroxybenzyl alcohol and 120ml of 1,4-dioxane into a 500ml three-necked flask equipped with a mechanical stirrer and a water separator, heat up to 85°C and add 0.18mol of triethyl borate, and then the system Heated to boiling state and reacted for 60 minutes, cooled, filtered to remove boric acid and unreacted hydroxybenzyl alcohol to obtain hydroxybenzyl borate intermediate; Add 0.45mol phenylphosphoryl dichloride, 1.32gMgCl 2 And 180ml 1,4-dioxane, nitrogen protection, react at 75°C for 5 hours, remove excess phenylphosphoryl dichloride and 1,4-dioxane under reduced pressure; change the decompression device to reflux device, add 0.8mol phenol, react at 125°C for 4 hours, and then react at 160°C for 2 hours, remove excess phenol under reduced pressure; dissolve the product in tetrahydrofuran, filter to remove MgCl 2 Afterwards, THF was distilled off by heating, and the obtained product was dried in a vacuum oven at 80°C to obtain a boron-containing ph...

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Abstract

The invention discloses a fire retardant containing boron phenyl phosphonic acid esters and a preparation method thereof. The constitutional formula of the fire retardant containing the boron phenyl phosphonic acid esters includes that R is -H, -CH3, -CH2CH3, -CH (CH3)2 or -CH2CH2CH2CH3, and n can be one to five. During preparation, hydroxide radical benzyl alcohol and organic solvent are heated after being mixed, then boron monomers are added into the mixture of the hydroxide radical benzyl alcohol and the organic solvent, the whole system is heated to react under the condition of boiling and then is cooled, and boric acid hydroxide radical benzol methyl ester midbody is prepared. Phenyl phosphorus acyl dichloro and organic solvent are added into the boric acid hydroxide radical benzol methyl ester midbody to react for five to twelve hours, then phenol is added into the boric acid hydroxide radical benzol methyl ester midbody, and the fire retardant containing the boron phenyl phosphonic acid esters is obtained after excessive phenol is removed and the solvent is dried. The fire retardant is solid, cannot move by 'squeezing' and has lower affection on impact performance of high polymer materials.

Description

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Claims

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Application Information

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Owner SOUTH CHINA UNIV OF TECH
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