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Phosphorus-nitrogen system biology based flame retardant as well as synthesis method and application thereof

A synthesis method and bio-based technology, which can be used in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. Processing and use problems, to achieve good processing performance and dispersibility, reduce the burden on the environment and resources, the synthesis process is simple and low toxicity.

Active Publication Date: 2019-06-21
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003]Although flame retardants and flame retardant materials based on bio-based raw materials have received extensive attention, some preparation methods are relatively complicated, and some products have insufficient performance. In particular, flame retardants prepared from polysaccharide monomers have poor heat resistance, and some are easily soluble in water, which is not conducive to later processing and use

Method used

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  • Phosphorus-nitrogen system biology based flame retardant as well as synthesis method and application thereof
  • Phosphorus-nitrogen system biology based flame retardant as well as synthesis method and application thereof
  • Phosphorus-nitrogen system biology based flame retardant as well as synthesis method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0061] At room temperature, 1 mol of terephthalaldehyde was completely dissolved in 400 mL of ethanol, 2 mol of furfurylamine was added thereto, stirred evenly by magnetic force, and the temperature was raised to 80° C. for 4 h. Keeping the reaction temperature at 80°C, 2.4mol of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide was added into the reaction flask, and the reaction was continued for 8 hours after it was completely dissolved. After the reaction was finished, the solvent was removed by rotary evaporation, washed three times with 2% aqueous sodium hydroxide solution, then washed three times with deionized water, and dried to obtain product 1, whose structural formula is as follows:

[0062]

Embodiment 2

[0064] At room temperature, 1 mol of benzaldehyde was completely dissolved in 200 mL of methanol, 1 mol of furfurylamine was added thereto, stirred evenly by magnetic force, and the temperature was raised to 60° C. to react for 4 h. Add 1.2 mol of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide into the reaction flask, and after completely dissolving, raise the temperature to 80°C and continue the reaction for 12 hours. After the reaction was finished, the solvent was removed by rotary evaporation, washed three times with 2% aqueous sodium hydroxide solution, then washed three times with deionized water, and dried to obtain product 2, whose structural formula is as follows:

[0065]

Embodiment 3

[0067] At room temperature, 1 mol of phenylacetaldehyde was completely dissolved in 200 mL of methanol, 1 mol of furfurylamine was added thereto, stirred evenly by magnetic force, and the temperature was raised to 80° C. to react for 4 h. Add 1 mol of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide into the reaction flask, and after it is completely dissolved, continue to react at 80°C for 8h. After the reaction was finished, the solvent was removed by rotary evaporation, washed three times with 2% aqueous sodium hydroxide solution, then washed three times with deionized water, and dried to obtain product 3, whose structural formula is as follows:

[0068]

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Abstract

The invention discloses a phosphorus-nitrogen system biology based flame retardant as well as a synthesis method and application thereof. The method comprises the following steps: completely dissolving a raw material 1 into an organic solvent at room temperature, adding a raw material 2 into the mixture, uniformly stirring through magnetic force, rising the temperature to 25 to 100 DEG C, and reacting for 2 to 12h; keeping the current reaction temperature, adding a phosphorus-containing material 3 into a reaction flask, ensuring that reaction is continued for 4 to 12 at 25 to 80 DEG C after the phosphorus-containing material 3 is completely dissolved. The flame retardant is simple in synthesis technology, small in pollution, low in toxicity, simple in aftertreatment, and very high in yieldand degree of purity, belongs to a melting point compound, has excellent processing property and excellent flame retardant efficiency, can not only obtain excellent flame retardant effect in epoxy resin, but also be properly applied to polyester compounds (polylactic acid), can obviously improve the UL-94 degree and oxygen index of the polylactic acid, and has little influence on the heat stability and mechanical property of flame retardant composite materials.

Description

technical field [0001] The invention relates to the technical field of flame retardant synthesis and application, in particular to a phosphorus-nitrogen series bio-based flame retardant and its synthesis method and application. Background technique [0002] As the oil crisis and environmental problems continue to intensify, bio-based materials have received more and more attention, and have very important applications in daily life fields such as packaging, transportation, and electronic devices, as well as in special fields such as aerospace and biotechnology. Bio-based materials are polymer materials or small molecular compounds obtained through biotransformation of renewable raw materials, mainly including bio-based platform compounds, bioplastics, functional sugar products, wood-plastic composite materials, etc., which have achieved functions in different fields application. Among them, the application of bio-based materials in the field of flame retardant has become an...

Claims

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Application Information

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IPC IPC(8): C07F9/40C07F9/655C07F9/6574C08K5/5313C08L67/04C08L63/00
Inventor 李娟孙晋皓
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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