Preparation method of POSS-DOPO-triazine derivative flame retardant with self-assembled enhancement effect and application thereof

A triazine derivative and enhancement technology, applied in the field of flame retardants, can solve the problems of reducing the mechanical properties of the matrix, large additions, poor compatibility, etc., and achieve increased stability, increased heat insulation, and flame retardant good effect

Active Publication Date: 2018-04-03
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] At present, there are various phosphorus-based, nitrogen-based and silicon-based flame retardants, but the flame retardants of each element have some defects, such as a large amount added to the polymer, poor compatibility, and reduced matrix mechanical properties and other issues

Method used

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  • Preparation method of POSS-DOPO-triazine derivative flame retardant with self-assembled enhancement effect and application thereof
  • Preparation method of POSS-DOPO-triazine derivative flame retardant with self-assembled enhancement effect and application thereof
  • Preparation method of POSS-DOPO-triazine derivative flame retardant with self-assembled enhancement effect and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] (1) Synthesis of intermediate products

[0041] Add 1.84g (0.01mol) of cyanuric chloride and 50mL of tetrahydrofuran into a 250mL three-necked round-bottomed flask, then add 4.372g (0.005mol) of POSS-NH 2 Dissolve in 50mL of tetrahydrofuran, dissolve and stir at -5~0°C respectively to obtain the first solution and the second solution, add the second solution dropwise to the first solution, stir at low temperature, slowly rise to room temperature, and add the second solution at the same time An acid-binding agent 10% NaHCO 3 solution, keep the pH value at neutral, and react for 6 hours. After the reaction, the solvent is concentrated by rotary evaporation, washed with distilled water to remove the first acid-binding agent salts, and further precipitated with acetonitrile to obtain an intermediate product with a yield of about 83%. (2) Preparation of POSS-DOPO-triazine derivative flame retardant

[0042]The dioxane of 100mL and the dimethyl sulfoxide of 100mL were mixed...

Embodiment 2

[0047] (1) Synthesis of intermediate products

[0048] Add 1.84g (0.01mol) of cyanuric chloride and 50mL of tetrahydrofuran into a 250mL three-necked round-bottomed flask, then add 4.372g (0.005mol) of POSS-NH 2 Dissolve in 50mL of tetrahydrofuran, dissolve and stir at -5 ~ 0°C respectively to obtain the first solution and the second solution, add the second solution dropwise to the first solution, stir at low temperature, slowly rise to room temperature, and add First Acid Binder 10% NaHCO 3 Solution, keep the pH value as neutral, and react for 6h. After the reaction, the solvent was concentrated by rotary evaporation, the first acid-binding agent salt was removed by washing with distilled water, and the intermediate product was obtained by further precipitation with acetonitrile, and the yield was about 83%.

[0049] (2) Preparation of POSS-DOPO-triazine derivative flame retardant

[0050] The dioxane of 100mL and the dimethyl sulfoxide of 100mL were mixed to obtain the s...

Embodiment 3

[0055] (1) Synthesis of intermediate products

[0056] Add 1.84g (0.01mol) of cyanuric chloride and 50mL of tetrahydrofuran into a 250mL three-necked round-bottomed flask, then add 4.372g (0.005mol) of POSS-NH 2 Dissolve in 50mL of tetrahydrofuran, dissolve and stir at -5 ~ 0°C respectively to obtain the first solution and the second solution, add the second solution dropwise to the first solution, stir at low temperature, slowly rise to room temperature, and add First Acid Binder 10% NaHCO 3 Solution, keep the pH value as neutral, and react for 6h. After the reaction, the solvent was concentrated by rotary evaporation, the first acid-binding agent salt was removed by washing with distilled water, and the intermediate product was obtained by further precipitation with acetonitrile, and the yield was about 83%.

[0057] (2) Preparation of POSS-DOPO-triazine derivative flame retardant

[0058] The dioxane of 100mL and the dimethyl sulfoxide of 100mL were mixed to obtain the s...

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Abstract

The invention discloses a preparation method of a POSS-DOPO-triazine derivative flame retardant with a self-assembled enhancement effect and application thereof. The flame retardant has the followingmolecular structural formula as shown in the specification, wherein R and R1 are as shown in the specification. The heat stability and flame retardant property of an epoxy resin matrix are improved onthe basis of ensuring mechanical property of the matrix, and the flame retardant has the advantages of being excellent in flame-retardant effect, wide in application range and the like.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and in particular relates to a preparation method and application of a POSS-DOPO-triazine derivative flame retardant with self-assembly enhancing effect. Background technique [0002] Epoxy resin has good physical and chemical properties, heat resistance, solvent resistance, excellent electrical insulation and mechanical properties, so it is widely used in electronic instruments, adhesives, construction and so on. With the increasing attention of epoxy resin, the requirements for its safety are gradually increasing. Epoxy resin is a three-dimensional network structure with high internal stress and surface energy, and is flammable. Therefore, it is necessary to ensure its mechanical properties on the basis of its flame retardancy modification. [0003] Phosphorus, nitrogen, and silicon are all effective flame retardant elements. Among them, organophosphorus can promote the carbonization...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/395C08L63/00C08L83/08
CPCC08G77/045C08L63/00C08L2201/02C08L2201/08C08L83/08
Inventor 戴李宗吴海洋李云同陈国荣曾碧榕袁丛辉许一婷罗伟昂
Owner XIAMEN UNIV
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