Phosphorus-containing reaction-type fire retardant as well as synthesis method and application thereof

A technology of reactive flame retardants and synthetic methods, which is applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve problems such as easy decomposition, injury, and life safety threats, and achieve Improved flame retardant performance and improved service life

Inactive Publication Date: 2015-05-06
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most polymer materials have a fatal shortcoming: they are easy to decompose and burn at high temperatures; moreover, the toxic gases and black smoke released by thermal decomposition of polymer materials pose a huge threat to people's lives and safety. harm

Method used

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  • Phosphorus-containing reaction-type fire retardant as well as synthesis method and application thereof
  • Phosphorus-containing reaction-type fire retardant as well as synthesis method and application thereof
  • Phosphorus-containing reaction-type fire retardant as well as synthesis method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Under nitrogen protection, 43.6g of DOPO, 13.4g of m-phthalaldehyde and 60ml of toluene were sequentially added to a 500ml single-necked flask equipped with a condenser tube and a magnetic stirring bar. Stir vigorously, heat to 110°C, keep the toluene in a reflux state, and keep this condition for 5h. Cool to room temperature, filter, collect the precipitate, and continue to wash three times with toluene. Put the product into a vacuum oven to evacuate, heat to 60° C., and hold the pressure for 8 hours; cool to room temperature to obtain 51.3 g of white diDOPO-MDCA product (90% yield).

[0028] The product was determined by NMR 1 H NMR ( figure 1 )and 31 P NMR ( figure 2 ), 1 H NMR (ppm, DMSO-d 6 ), δ=8.29~7.03ppm (20H, Ar-H), 6.47~6.24ppm (2H, =CH-), 5.39~5.05ppm (2H, OH); 31 P NMR (ppm, DMSO-d 6 ), δ=31.02.

Embodiment 2

[0030] Under nitrogen protection, 43.6 g of DOPO, 13.4 g of m-phthalaldehyde and 285 ml of toluene were sequentially added to a 500 ml one-necked flask equipped with a condenser tube and a magnetic stirring bar. Stir vigorously, heat to 130°C, keep the toluene in a reflux state, and keep this condition for 5h. Cool to room temperature, filter, collect the precipitate, and continue to wash three times with toluene. Put the product into a vacuum oven to evacuate, heat to 80° C., and hold the pressure for 8 hours; cool to room temperature to obtain 51.3 g of white diDOPO-MDCA product (90% yield).

Embodiment 3

[0032] Under nitrogen protection, 43.6g of DOPO, 13.4g of m-phthalaldehyde and 200ml of toluene were sequentially added to a 500ml single-necked flask equipped with a condenser tube and a magnetic stirring bar. Stir vigorously, heat to 120°C, keep the toluene in a reflux state, and keep this condition for 5h. Cool to room temperature, filter, collect the precipitate, and continue to wash three times with toluene. Put the product into a vacuum oven to evacuate, heat to 70° C., and hold the pressure for 8 hours; cool to room temperature to obtain 51.3 g of white diDOPO-MDCA product (90% yield).

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Abstract

The invention belongs to the technical field of organic chemical engineering, and particularly relates to a phosphorus-containing reaction-type fire retardant as well as a synthesis method and application thereof. The chemical name of the fire retardant is bis-9,10-dihydro-9-oxa-10-phosphonia-10-phenanthrene oxide-base (diDOPO-MDCA), the compound has two hydroxyl active sites and can be used as the fire retardant for resin reacting with the compound, the element phosphorus is introduced into a molecular structure of a macromolecular material in a form of a covalent bond, the fire resistance of the resin can be improved, and a non-toxic high-efficiency long fire retardant purpose can be realized. The production condition is simple, the product purity and yield are relatively high, and the after-treatment process is simple.

Description

technical field [0001] The invention relates to the field of organic chemical technology, in particular to a phosphorus-containing reactive flame retardant, a synthesis method and an application thereof. Background technique [0002] In the 21st century, polymer materials are widely used in industrial production and people's lives, such as automobiles, electrical equipment, aerospace, high-rise buildings, interior decoration and other fields. However, most polymer materials have a fatal shortcoming: they are easy to decompose and burn at high temperatures; moreover, the toxic gases and black smoke released by thermal decomposition of polymer materials pose a huge threat to people's lives and safety. harm. Therefore, research on polymer flame retardancy has received worldwide attention. [0003] At present, flame retardant research on polymer materials is affected by increasingly stringent environmental protection and flame retardant regulations, and most of them have bid f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5313C07F9/6574C08G59/62C08G18/32
Inventor 谢聪赵龙
Owner SHANGHAI JIAO TONG UNIV
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