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Bicyclic phosphate-based triazine derivative flame retardant and preparation method thereof

A technology of bicyclic phosphate triazine and derivatives, applied in the field of bicyclic phosphate triazine derivative flame retardants and their preparation, can solve the problem of material mechanical and mechanical properties decline, uneven distribution of components, flame retardants Easy to absorb moisture and other problems, to achieve the effect of improving defects, easy availability of raw materials, and good migration resistance

Active Publication Date: 2010-12-22
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] At present, compound intumescent flame retardants are mostly composed of three components including carbon source, acid source, and foaming source. This mixture will inevitably lead to uneven distribution of components in the material, and the mechanical properties of the material , The mechanical properties are obviously reduced, and the flame retardant is easy to absorb moisture, easy to migrate and seep out, etc.

Method used

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  • Bicyclic phosphate-based triazine derivative flame retardant and preparation method thereof
  • Bicyclic phosphate-based triazine derivative flame retardant and preparation method thereof
  • Bicyclic phosphate-based triazine derivative flame retardant and preparation method thereof

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Effect test

Embodiment 1

[0035] Under the protection of high-purity nitrogen (purity ≥ 99.9%), put 1.84g (10mmol) cyanuric chloride into the reactor, add 50mL N, N-dimethylacetamide, stir for 10 minutes to disperse the cyanuric chloride evenly , then add 6.10mL (35mmol) N, N-diisopropylethylamine and 5.40g (30mmol) PEPA, continue to stir for a period of time to make the reactant disperse evenly, after reacting at 40°C for 8 hours, raise the reaction temperature to 60°C ℃, after stirring and reacting for 10 hours, raise the reaction temperature to 110℃, and after stirring and reacting for 12 hours, stop the reaction. After drying for 48 hours, a triazine derivative flame retardant having a bicyclic phosphate group was obtained with a yield of 93.7%.

[0036] The above-mentioned prepared bicyclic phosphate group triazine derivative flame retardant is carried out infrared test, and the test instrument is NICOLET 6700; Potassium bromide compression tablet sample preparation; its infrared spectrum is as f...

Embodiment 2

[0040] Under the protection of high-purity nitrogen (purity ≥ 99.9%), put 1.84g (10mmol) cyanuric chloride into the reactor, add 50mL of dioxane, stir for 20 minutes to disperse the cyanuric chloride evenly, add 5.78mL (40mmol) triethylamine and 5.40g (30mmol) PEPA, continue to stir for a period of time to make the reactant disperse evenly, after reacting at 40°C for 12 hours, raise the reaction temperature to 60°C, stir and react for 12 hours, then increase the reaction temperature Temperature to 85°C, stirring reaction for 24 hours, stop the reaction, precipitate the reaction product with 1500mL acetone after cooling, wash with a large amount of acetone after suction filtration, and vacuum dry at 80°C for 48 hours to obtain a bicyclic phosphate ester structure bicyclic Phosphate-based triazine derivative flame retardant with a yield of 95.2%.

[0041] The above-mentioned prepared bicyclic phosphate-based triazine derivative flame retardant is subjected to infrared testing, t...

Embodiment 3

[0044] Under the protection of high-purity nitrogen (purity ≥ 99.9%), put 1.84g (10mmol) cyanuric chloride into the reactor, add 50mL of 1-methyl 2-pyrrolidone, stir for 10-30 minutes to disperse the cyanuric chloride evenly , add 6.10mL (35mmol) N, N-diisopropylethylamine and 5.40g (30mmol) PEPA, continue to stir for a period of time to disperse the reactants evenly, after reacting at 40°C for 8 hours, raise the reaction temperature to 60°C , after stirring for 8 hours, raise the reaction temperature to 120°C, and stop the reaction after stirring for 12 hours. After cooling, use 1000mL ethanol to precipitate the reaction product, wash it with a large amount of acetone after suction filtration, and dry it in vacuum at 80°C. After 48 hours, a bicyclic phosphate-based triazine derivative flame retardant was obtained with a yield of 94.1%.

[0045] The above-mentioned prepared bicyclic phosphate-based triazine derivative flame retardant is subjected to infrared testing, the test ...

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Abstract

The invention discloses a bicyclic phosphate-based triazine derivative flame retardant and a preparation method thereof. The flame retardant is prepared by the condensation polymerization of cyanuric chloride and 1-oxide-4-hydroxymethyl-2,6,7-trioxa-1-phosphabicyclo [2,2,2] octane. The preparation method has the advantages of easy acquisition of raw materials and simple operation. The prepared flame retardant contains a carbon source, an acid source and a foaming source, greatly exerts the advantages of the PEPA and the triazine structure in flame retardant applications, is favorable for exerting the synergistic flame retardant action of nitrogen and phosphorus, and can effectively improve the defects of the traditional compound flame retardant. The bicyclic phosphate-based triazine derivative flame retardant has large molecular weight, has the advantages of high heat stability, good migration resistance and the like, and can be used as a single intumescent flame retardant (IFR) or can be compounded with other components to form an IFR system to be applied to material flame retardant modification.

Description

technical field [0001] The invention relates to the technical field of flame retardant development, in particular to a bicyclic phosphate-based triazine derivative flame retardant and a preparation method thereof. Background technique [0002] With the rapid development of polymer materials, people have higher requirements for the flame retardant properties of materials. Generally, adding flame retardants to materials can significantly improve the flame retardant properties of materials. Halogenated flame retardants were mostly used in the early days, which have the characteristics of less addition, obvious flame retardant effect, many varieties, and high cost performance. At the same time, it causes "secondary disasters", so it is gradually eliminated. In recent years, all countries are seeking to develop high-efficiency multifunctional composite flame retardants and environmentally friendly flame retardants. Among them, intumescent flame retardants are one of the types of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K21/12C07F9/6574
Inventor 陶慷李娟严庆薛立新朱红芳朱琦良
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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