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2,4,6-diethyl triphosphate hydroxymethylphenoxy-1,3,5-triazine flame retardant and preparation method

A technology of diethyl triphosphate hydroxymethylphenoxy and trialdehyde phenoxy, which is applied in the field of flame retardancy, can solve the problems of deteriorating the basic physical properties of materials, affecting the durability of material flame retardancy, and uneven dispersion, achieving Strong practicability, high thermal stability, simple and easy-to-operate preparation process

Active Publication Date: 2018-01-02
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, when this kind of flame retardant is used in thermosetting polymer materials such as polyurethane and epoxy resin, it will cause obvious problems such as uneven dispersion and easy migration.
These problems will not only deteriorate the basic physical properties of the material, but also affect the flame retardant durability of the material

Method used

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  • 2,4,6-diethyl triphosphate hydroxymethylphenoxy-1,3,5-triazine flame retardant and preparation method
  • 2,4,6-diethyl triphosphate hydroxymethylphenoxy-1,3,5-triazine flame retardant and preparation method
  • 2,4,6-diethyl triphosphate hydroxymethylphenoxy-1,3,5-triazine flame retardant and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a 500mL dry three-neck flask equipped with a mechanical stirrer, a constant pressure dropping funnel and a condensing reflux device, add 31.8g of potassium carbonate, 36.6g of p-hydroxybenzaldehyde and 250mL of refined tetrahydrofuran in sequence, and stir at room temperature for 1h under nitrogen protection Make it dissolve; Then take by weighing 18.45g cyanuric chloride (the molar ratio of cyanuric chloride and p-Hydroxybenzaldehyde is 1:3) and dissolve in 100mL refined tetrahydrofuran, slowly add it dropwise in the above-mentioned reaction system, Adding time is 1h; after 0.5h, slowly heat up to 60°C, reflux and stir for 24h, after the reaction is completed, change it to a distillation device, distill off the solvent under reduced pressure, pour it into a large amount of deionized water, and immediately precipitate a white precipitate; again Filter and wash the product repeatedly with deionized water for 3 times; vacuum-dry at 50°C for 12 hours to obtain a white po...

Embodiment 2

[0030] In a 500mL dry three-neck flask equipped with a mechanical stirrer, a constant pressure dropping funnel and a condensing reflux device, add 31.8g of potassium carbonate, 36.6g of p-hydroxybenzaldehyde and 250mL of refined tetrahydrofuran in sequence, and stir at room temperature for 1h under nitrogen protection Make it dissolve; Then take by weighing 18.45g cyanuric chloride (the molar ratio of cyanuric chloride and p-Hydroxybenzaldehyde is 1:4) and dissolve in 100mL refined tetrahydrofuran, slowly add it dropwise in the above-mentioned reaction system, Adding time is 1h; after 0.5h, slowly heat up to 60°C, reflux and stir for 24h, after the reaction is completed, change it to a distillation device, distill off the solvent under reduced pressure, pour it into a large amount of deionized water, and immediately precipitate a white precipitate; again Filter and wash the product repeatedly with deionized water for 3 times; vacuum-dry at 50°C for 12 hours to obtain a white po...

Embodiment 3

[0033] In a 500mL dry three-neck flask equipped with a mechanical stirrer, a constant pressure dropping funnel and a condensing reflux device, add 31.8g of potassium carbonate, 36.6g of p-hydroxybenzaldehyde and 250mL of refined tetrahydrofuran in sequence, and stir at room temperature for 1h under nitrogen protection Make it dissolve; Then take by weighing 18.45g cyanuric chloride (the molar ratio of cyanuric chloride and p-Hydroxybenzaldehyde is 1:3) and dissolve in 100mL refined tetrahydrofuran, slowly add it dropwise in the above-mentioned reaction system, Adding time is 1h; after 0.5h, slowly raise the temperature to 80°C, reflux and stir for 24h, after the reaction is completed, change it to a distillation device, distill off the solvent under reduced pressure, pour it into a large amount of deionized water, and immediately precipitate a white precipitate; again Filter and wash the product repeatedly with deionized water for 3 times; vacuum-dry at 50°C for 12 hours to obt...

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Abstract

The invention discloses a 2,4,6-triphosphate diethyl hydroxymethylphenoxy-1,3,5-triazine flame retardant and a preparation method thereof, belonging to the technical field of flame retardancy. Add cyanuric chloride, p-hydroxybenzaldehyde, and a catalyst to an organic solvent, heat to reflux for reaction, and then undergo a post-processing step to obtain a white solid powder 2,4,6-trialdehyde-phenoxy-1,3,5 ‑triazine; then 2,4,6‑3 formylphenoxy‑1,3,5‑triazine, diethyl phosphite, and triethylamine are heated and refluxed in an organic solvent, and the reaction product is decompressed After distilling off the organic solvent and triethylamine, a 2,4,6-diethyl triphosphate hydroxymethylphenoxy-1,3,5-triazine flame retardant is obtained. The preparation process of the 2,4,6-triphosphate diethyl hydroxymethylphenoxy-1,3,5-triazine involved in the present invention is simple and easy to operate, has high yield, strong practicability, environmental protection and pollution-free, and can large-scale industrial production.

Description

technical field [0001] The invention relates to a synthesis method of a flame retardant 2,4,6-diethyl triphosphate hydroxymethylphenoxy-1,3,5-triazine, in particular to a reactive flame retardant containing nitrogen and phosphorus The invention relates to a preparation method of a synergistic flame retardant element compound, which belongs to the field of flame retardant technology. Background technique [0002] Intumescent flame retardant (IFR) is a composite flame retardant mainly composed of nitrogen and phosphorus. It has the characteristics of high efficiency and low toxicity. It can prevent oxygen from entering the combustion area, and can also prevent the gaseous or liquid products generated by degradation from overflowing the surface of the material, thereby preventing further combustion of the material. This kind of flame retardant not only has high flame retardant efficiency but also has the characteristics of high efficiency, low toxicity and environmental protec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/523C07F9/6521C08L75/08C08G18/48C08J9/04
Inventor 李锦春马彬彬杨荣张鑫胡文田
Owner CHANGZHOU UNIV
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