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 preparation of boron-containing phenyl phosphonate flame retardant, which can solve the problems of low flame retardant efficiency, reduced impact performance of polymer materials, inconvenient processing and use, etc. problem, to achieve the effect of high flame retardancy and good compatibility

Active Publication Date: 2013-04-10
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as pointed out in Japanese patent JP63-227632.1988-9 and Chinese patent 00808793.8, the use of BDP and RDP still has great defects: (1) high viscosity and liquid state at room temperature, which is very inconvenient to process and use; (2) easy to occur Migration to the surface causes the so-called "juicing" phenomenon, which is more likely to occur in places with higher temperatures, (3) causing a significant decrease in the impact properties of polymer materials, (4) containing only one phosphorus flame retardant element, the flame retardant efficiency Low, to achieve a certain level of flame retardant use a large amount

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

Examples

Experimental program
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Effect test

Embodiment 1

[0020] 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

[0024] 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

[0028] 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, add 0.18mol of triethyl borate, and then put 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, 1.32g MgCl 2And 180ml 1,4-dioxane, under 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-conta...

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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

technical field [0001] The invention relates to a novel flame retardant, in particular to a preparation method of a boron-containing phenylphosphonate flame retardant. Background technique [0002] With the densification of urban buildings, the high-rise building and the lightening of building structures, organic synthetic polymer materials are widely used in various fields, but this type has a great potential fire hazard and is easy to cause fire. Due to the occurrence of fires caused by the ignition of polymer materials more and more frequently, people have paid great attention to the flame retardancy of polymer materials. How to improve the flame retardancy of synthetic materials, reduce the burning hazard of combustibles and the toxic gases released during burning, and reduce the loss of people's lives and property has become a research topic for researchers. Researchers have found that adding flame retardants or introducing flame retardant groups into polymer materials...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/55C07F9/40C08L69/00C08L55/02
Inventor 赵建青邓娟刘述梅袁彦超
Owner SOUTH CHINA UNIV OF TECH
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