Copolymerized phosphorus-nitrogen macromolecular expansion flame retardant modified layered nano zirconium phosphate and its preparation method and application

An intumescent flame retardant and layered nanotechnology, applied in the field of zirconium phosphate, can solve the problems of limited flame retardant efficiency, high content of hindered amine groups, and inability to effectively control, and achieve excellent flame retardant performance and thermal stability. Overcoming the effect of easy migration

Active Publication Date: 2022-03-29
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 expansion flame retardant modified layered nano zirconium phosphate and its preparation method and application
  • Copolymerized phosphorus-nitrogen macromolecular expansion flame retardant modified layered nano zirconium phosphate and its preparation method and application
  • Copolymerized phosphorus-nitrogen macromolecular expansion flame retardant modified layered nano zirconium phosphate and its preparation method and application

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Effect test

Embodiment 1

[0035] The preparation method of the layered nano zirconium phosphate modified by the copolymerization type phosphorus-nitrogen macromolecule expansion type flame retardant comprises the following steps:

[0036] 1) Synthesis of copolymerized phosphorus-nitrogen macromolecular intumescent flame retardant: at 5°C, add 36.90g of cyanuric chloride, 35.82g of PEPA, 0.75g of T152 and 250mL of acetonitrile into a 500mL four-neck flask, Stir mechanically for 15 minutes at a speed of 1 / min; slowly add 20.20 g of triethylamine dropwise for 1.5 hours, and continue to react for 4 hours after the dropwise addition is completed; then, continue to dropwise add 12.00 g of ethylenediamine and The mixed solution of 20.20g triethylamine, the dropwise addition time is 1.5h, after the dropwise addition is completed, continue to react for 6h. Finally, the temperature was raised to 95°C, and 20.20 g of triethylamine was added dropwise for reflux reaction for 6 h. After the reaction is finished, th...

Embodiment 2

[0041] The preparation method of the layered nano zirconium phosphate modified by the copolymerization type phosphorus-nitrogen macromolecule expansion type flame retardant comprises the following steps:

[0042] 1) Synthesis of copolymerized nitrogen-phosphorus macromolecular intumescent flame retardant: Add 36.90g of cyanuric chloride, 35.64g of PEPA, 1.50g of T152 and 250mL of toluene into a 500mL four-necked flask at 0°C, Stir mechanically at a speed of 10min / min; slowly add 23.70g of pyridine dropwise for 2h, and continue to react for 5h after the dropwise addition is completed; then, continue to dropwise add 14.40g of ethylenediamine and 15.82g of pyridine after the temperature rises to 60°C The mixed solution, the dropwise addition time is 2h, and the reaction is continued for 8h after the dropwise addition is completed. Finally, the temperature was raised to 100°C, and 23.70 g of pyridine was added dropwise for reflux reaction for 9 hours. After the reaction is finish...

Embodiment 3

[0046] The preparation method of the layered nano zirconium phosphate modified by the copolymerization type phosphorus-nitrogen macromolecule expansion type flame retardant comprises the following steps:

[0047] 1) Synthesis of copolymerized phosphorus-nitrogen macromolecular intumescent flame retardant: Add 36.90g of cyanuric chloride, 35.29g of PEPA, 2.97g of T152 and 250mL of 1,4- Dioxane, stir mechanically at 200r / min to disperse evenly; slowly add 24.24g of triethylamine dropwise for 2h, and continue to react for 3h after the drop; then, continue to A mixture of 12.00 g of ethylenediamine and 24.24 g of triethylamine was added dropwise for 2 hours, and the reaction was continued for 8 hours after the drop was completed. Finally, the temperature was raised to 100°C, and 24.24 g of triethylamine was added dropwise for reflux reaction for 9 h. After the reaction, the mixed liquid is filtered, washed and dried to obtain a macromolecular intumescent flame retardant with adju...

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Abstract

The invention discloses a layered nano-zirconium phosphate modified by a copolymerized phosphorus-nitrogen macromolecular expansion flame retardant, a preparation method and an application thereof. The preparation method is to add hindered amine monomer, bicyclic cage-shaped phosphate and cyanuric chloride into an organic solvent, undergo nucleophilic substitution reaction, add ethylenediamine dropwise, and successively add ethylenediamine under the conditions of 40-60°C and 90-120°C. reacted, filtered and washed to obtain a copolymerized phosphorus-nitrogen macromolecular intumescent flame retardant with adjustable hindered amine content. Subsequently, it is added into the exfoliated nano-zirconium phosphate dispersion liquid for reaction, and the layered nano-zirconium phosphate modified by the copolymerized phosphorus-nitrogen macromolecular expansion flame retardant is obtained through filtering, washing and drying. Compared with the existing technology, the content of hindered amines in the present invention can be regulated by the copolymerization reaction, which can exert the efficient synergistic effect of flame retardant free radical quenching and catalytic char formation mechanism, and only need to add a small amount to give PP Excellent flame retardancy and thermal stability.

Description

technical field [0001] The invention relates to zirconium phosphate, in particular to a layered nano-zirconium phosphate modified by a copolymerized phosphorus-nitrogen macromolecular expansion flame retardant, a preparation method and application thereof, and belongs to the field of preparation and application of halogen-free flame retardants. Background technique [0002] Intumescent flame retardant (IFR), as a new type of environmentally friendly halogen-free flame retardant, has been developed rapidly in recent years. Traditional IFR is usually composed of two or more small molecular compounds, which are difficult to uniformly disperse in the polymer matrix during processing, making it difficult for each component to play a synergistic role, reducing its flame retardant efficiency; in addition, These small molecular compounds are highly polar and have poor compatibility with polypropylene (PP). Adding a large amount will deteriorate the mechanical properties and processi...

Claims

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Application Information

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Patent Type & Authority Patents(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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