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Copolymerized phosphorus-nitrogen macromolecular intumescent flame retardant modified layered nano zirconium phosphate as well as preparation method and application thereof

An intumescent flame retardant, layered nanotechnology, applied in the field of zirconium phosphate, can solve the problems of ineffective regulation, high content of hindered amine groups, limited flame retardant efficiency, etc., to improve catalytic carbonization performance, overcome easy migration , the effect of excellent flame retardant performance and thermal stability

Active Publication Date: 2021-03-12
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high content of hindered amine groups in the synthesized one-component macromolecule intumescent flame retardant, which cannot be effectively regulated, the excessive hindered amines will promote the chain degradation of PP and accelerate the melting and burning. , limiting the further improvement of flame retardant efficiency

Method used

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  • Copolymerized phosphorus-nitrogen macromolecular intumescent flame retardant modified layered nano zirconium phosphate as well as preparation method and application thereof
  • Copolymerized phosphorus-nitrogen macromolecular intumescent flame retardant modified layered nano zirconium phosphate as well as preparation method and application thereof
  • Copolymerized phosphorus-nitrogen macromolecular intumescent flame retardant modified layered nano zirconium phosphate as well as preparation method and application thereof

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Experimental program
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Effect test

Embodiment 1

[0035] Preparation method of layered nanophosphate phosphosphate in a copolymerized phosphorus-nitrogen moxic expansion flame retardant, including the following steps:

[0036] 1) Synthesis of copolymerized phosphorus-nitrogen moxic expansion flame retardants: Under 5 ° C, 36.90 g of three-mouth flask, 35.82 g of PEPA, 0.75 g T152 and 250 mL of acetonitrile were added to 350R. The MIN speed was stirred at 15 min; 20.20 g of triethylamine was slowly added dropwise, and the dropwax time was 1.5 h. After the drop was completed, the reaction was continued for 4 h; then, 12.00 g of ethylenediamine was continued after the temperature was raised to 55 ° C. 20.20 g of a mixture of triethylamine, a dropwate of 1.5 h, and the reaction was continued after 6 h after completion of the drop. Finally, heated to 95 ° C, and 20.20 g of triethylamine reflux reaction was added 6 h. After completion of the reaction, the mixture was filtered, washed, dried to obtain a nitrogen-phosphorus macromolecula...

Embodiment 2

[0041] Preparation method of layered nanophosphate phosphosphate in a copolymerized phosphorus-nitrogen moxic expansion flame retardant, including the following steps:

[0042] 1) Copolymerized nitrogen-phosphorus moxic expansion flame retardant synthesis: Under 0 ° C, 36.90 g of TME cyanin, 35.64 g PEPA, 1.50 g T152 and 250 mL of toluene were added to 500 ml of toluene. The MIN speed was stirred at 10 min; 23.70 g of pyridine was slowly added dropwise, and the drip time was 2 h. After the drop was completed, the reaction was continued for 5 h; then, 14.40 g of ethylenediamine and 15.82 g of pyridine were continued after the temperature increased to 60 ° C. The mixture was mixed with a dropwise time of 2 h, and the reaction was continued for 8 h after completion of the drop. Finally, the temperature was warmed to 100 ° C, and 23.70 g of a pyridine reflux reaction was added dropwise for 9 h. After completion of the reaction, the mixture was filtered, washed, dried to obtain a nitro...

Embodiment 3

[0046] Preparation method of layered nanophosphate phosphosphate in a copolymerized phosphorus-nitrogen moxic expansion flame retardant, including the following steps:

[0047] 1) Synthesis of copolymerized phosphorus-nitrogen moxic expansion flame retardants: Under 10 ° C, 36.90 g of TME cyanide, 35.29 g of PEPA, 2.97 g T152 and 250ml 1, 4- Dioxin ring, mechanically stirred at 200R / min speed to make it dispersed uniform; slowly drop 24.24 g of triethylamine, the dropwate is 2 h, and the reaction is continuously reacted after 3 hours after the drop; then, the temperature increases to 40 ° C continued A mixture of 12.00 g of ethylenediamine and 24.24 g of triethylamine were added dropwise, and the dropwate was 2 h, and the reaction was continued for 8 h after drying. Finally, the temperature was warmed to 100 ° C, and 24.24 g of triethylamine reflux reaction was added to 9 h. After completion of the reaction, the mixture was filtered, washed, dried to obtain an macromolecularly e...

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Abstract

The invention discloses copolymerized phosphorus-nitrogen macromolecular intumescent flame retardant modified layered nano zirconium phosphate as well as apreparation method and application thereof. The preparation method comprises the steps of adding a hindered amine monomer, bicyclic caged phosphate and cyanuric chloride into an organic solvent, carrying out nucleophilic substitution reaction, dropwise adding ethylenediamine, sequentially reacting at the temperature 40-60 DEG C and the temperature of 90-120 DEG C, filtering, and washing to obtain a hindered amine content-adjustable copolymerized phosphorus-nitrogen macromolecular intumescent flame retardant; and then, adding the copolymerized phosphorus-nitrogen macromolecular intumescent flame retardant into a stripping type nano zirconium phosphate dispersion solution to react, filtering, washing and drying to obtain the copolymerized phosphorus-nitrogen macromolecular intumescent flame retardant modified layered nano zirconium phosphate. Compared with the prior art, the content of hindered amine can be regulated and controlled through copolymerization, the efficient synergistic effect of flame retardant free radical quenchingand a catalytic charring mechanism can be achieved, and PP can be endowed with excellent flame retardant property and thermal stability only by adding a small amount of hindered amine.

Description

Technical field [0001] The present invention relates to zirconium phosphate, and more particularly to a lay-form nanosphate phosphate-nitrogen-nitrotic expansion-type flame retardant modified, a preparation method and application thereof, belonging to a halogen-free flame retardant, and is a preparation and application of a halogen-free flame retardant. Background technique [0002] The expansion flame retardant (IFR) is a new environmentally friendly halogen-free flame retardant, which has been developed rapidly in recent years. The conventional IFR is usually compounded by two or more small molecular compounds, and it is difficult to uniformly disperse in the polymer matrix during processing, resulting in difficulty in which the components are difficult to play, so that the flame retardant efficiency is lowered; These small molecule compounds are polar polarity, poorly compatible with polypropylene (PP), and add a large amount of mechanical properties and processability of the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L85/02C08K9/04C08K7/00C08K3/32C08L23/12
CPCC08K9/08C08K7/00C08K3/32C08L23/12C08K2003/328C08K2003/323C08K2201/011C08L2201/02C08L2201/22C08L85/02
Inventor 赖学军李佳欣曾幸荣李红强陈奕燊
Owner SOUTH CHINA UNIV OF TECH
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