Phosphonitrile fire retardant and preparation method and application thereof

A phosphazene flame retardant and technology for flame retardants are used in the preparation of halogen-free flame retardant composite materials, phosphazene flame retardants and their preparation fields, and can solve the problems of deteriorating mechanical properties of composite materials, narrow melting range and the like, To solve the problem of poor mechanical properties of materials, narrow melting range and good compatibility

Inactive Publication Date: 2015-01-21
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a phosphazene flame retardant and its preparation method and application, so as to solve the difficulty in preparing aliphatic amine-substituted phosphazene flame retardants with narrow melting range, high purity, high yield and good processability in the prior art. Flame retardants, and adding them as flame retardants to plastic base materials, especially EVA polymer base materials, can achieve excellent flame retardant effects while not deteriorating the mechanical properties of composite materials

Method used

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  • Phosphonitrile fire retardant and preparation method and application thereof
  • Phosphonitrile fire retardant and preparation method and application thereof
  • Phosphonitrile fire retardant and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0043] (1) Dissolve 3.00g (0.0086 mol) of hexachlorocyclotriphosphazene and 8.73g (0.086mol) of triethylamine in an inclined three-necked round-bottomed flask (with a condensing device) filled with 100ml of dioxane, and pass Into N 2 protection, put the round-bottomed flask into an oil bath at 80°C, and stir magnetically for 10 minutes to dissolve and mix evenly to obtain a uniform mixture; The dioxane solution of diamine was added dropwise while stirring, and the drop was completed after 2 hours. After the dropwise addition was completed, the reaction was refluxed at 80° C. for 12 hours to obtain a reaction solution;

[0044] (2) Cool the reaction solution to room temperature, let it stand until the layers are separated, filter under reduced pressure to obtain a white precipitate, first rinse with dioxane, then rinse with a large amount of deionized water, and finally put the precipitate into a vacuum oven at 80°C for drying Oven-dried for 12 h, the product hexa-dodecylamino...

Embodiment 2

[0052] (1) Dissolve 3.00g (0.0086 mol) of hexachlorocyclotriphosphazene and 8.73g (0.086mol) of triethylamine in an inclined three-necked round-bottomed flask (with a condensing device) filled with 100ml of dioxane, and pass Into N 2 protection, put the round-bottomed flask into an oil bath at 50°C, and stir magnetically for 8 minutes to dissolve and mix evenly to obtain a uniform mixture; at this time, add 50ml containing 9.546g (0.0516mol) The dioxane solution of diamine was added dropwise while stirring, and the drop was completed after 2 hours. After the dropwise addition was completed, it was refluxed at 80°C for 10 hours to obtain a reaction solution;

[0053] (2) Cool the reaction solution to room temperature, let it stand until the layers are separated, filter under reduced pressure to obtain a white precipitate, first rinse with dioxane, then rinse with a large amount of deionized water, and finally put the precipitate into a vacuum oven at 80°C for drying After oven...

Embodiment 3

[0056] (1) Dissolve 3.00g (0.0086 mol) of hexachlorocyclotriphosphazene in an inclined three-necked round-bottomed flask (with a condensing device) filled with 100ml of dioxane, and inject N 2 protection, put the round-bottomed flask into an oil bath at 80°C, and stir magnetically for 8 minutes to dissolve and mix evenly to obtain a uniform mixture; Diamine and 8.73g (0.086mol) of triethylamine in dioxane solution were added dropwise while stirring, and the drop was completed after 1 hour. After the drop was completed, the solution was refluxed at 75°C for 12 hours to obtain a reaction solution;

[0057] (2) Cool the reaction solution to room temperature, let it stand until the layers are separated, filter under reduced pressure to obtain a white precipitate, first rinse with dioxane, then rinse with a large amount of deionized water, and finally put the precipitate into a vacuum oven at 80°C for drying After oven drying for 12 h, the product hexa-dodecylamino-cyclotriphosphaz...

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Abstract

The invention discloses a chemical structure of a phosphonitrile fire retardant, and discloses a preparation method of the phosphonitrile fire retardant. The method comprises the following steps: (a) dissolving phosphonitrilic chloride trimer and an acid-binding agent into an organic solvent, introducing N2 for protecting, stirring evenly to obtain a mixed solution, dropwise adding n-octylamine or lauryl amine to the mixed solution when stirring, carrying out reflux reaction at 50-80 DEG C for 9-12 hours after dropwise adding is ended, so as to obtain reaction liquid; and (b) cooling the reaction liquid, standing and separating a target product, and drying to obtain a phosphonitrile fire retardant. Meanwhile, the invention also discloses a composite material which is prepared from the prepared fire retardant added to EVA and is excellent in flame retardant property and mechanical performance. According to the novel phosphonitrile fire retardant developed by the method, the preparation method is simple and easy to operate; the prepared aliphatic amine-substituted phosphonitrile compound is narrow in melting range, high in purity and good in processability; and the composite material prepared by compounding with EVA can be widely used as a cable raw material.

Description

technical field [0001] The invention relates to a flame retardant and its preparation method and application, in particular to a phosphazene flame retardant, its preparation method and the application of adding it in EVA polymer base material to prepare halogen-free flame retardant composite material. Background technique [0002] Phosphazene and its derivatives are a kind of halogen-free, environment-friendly nitrogen-phosphorus flame retardants. Due to their high thermal stability, only P and N two flame retardant elements, high flame retardant efficiency and low toxicity And a series of advantages, the researchers have launched a wide range of research and application. At present, the types of cyclophosphazene flame retardants added to plastic polymers mainly include: ① hydroxyl cyclotriphosphazene flame retardants, ② amino cyclotriphosphazene flame retardants, ③ cyclotriphosphazene flame retardants containing double bonds Fuel. Among them, the amino group-containing cy...

Claims

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Application Information

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IPC IPC(8): C08K5/5399C08L23/08C08K3/22C08K5/527C07F9/6593
Inventor 王春征武翠翠屈红强刘晓威徐建中
Owner HEBEI UNIVERSITY
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