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Halogen-free phosphazene expanding-type flame retardant and preparation method thereof

An intumescent flame retardant, halogen-free phosphazene technology, applied in the field of flame retardants, can solve the problems of uncontrollable reaction process, complicated product purification process, unfavorable industrial production, etc., and achieves high synthesis efficiency, improved thermal stability, Add less effect

Inactive Publication Date: 2018-08-31
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the reaction process of this product, substitution reactions between various products are prone to occur, and dendritic by-products of different lengths are generated, resulting in too many by-products and the uncontrollable reaction process. The product purification process is complicated, which is not conducive to industrial production.

Method used

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  • Halogen-free phosphazene expanding-type flame retardant and preparation method thereof
  • Halogen-free phosphazene expanding-type flame retardant and preparation method thereof
  • Halogen-free phosphazene expanding-type flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 8.84ml triethylamine and 6.25g neopentyl glycol and 40ml tetrahydrofuran solvent in the 250ml three-neck flask equipped with reflux condenser, constant pressure titration funnel, thermometer and magnetic stirrer, simultaneously 6.95g hexachlorocyclotriphosphazene Dissolve in 20ml tetrahydrofuran and transfer to a constant pressure titration funnel, raise the temperature to 50°C under the protection of nitrogen, start to slowly add the hexachlorocyclotriphosphazene solution dropwise, after the drop, raise the temperature to 60°C for reflux for 7 hours, and stop the reaction. After cooling, it was filtered, and the filtrate was distilled under reduced pressure, recrystallized from ethyl acetate, and dried under vacuum at 65°C for 2 hours to obtain a white solid product. Yield 78.3%.

Embodiment 2

[0030] Add 8.84ml triethylamine and 6.25g neopentyl glycol and 40ml tetrahydrofuran solvent in the 250ml three-neck flask equipped with reflux condenser, constant pressure titration funnel, thermometer and magnetic stirrer, simultaneously 6.95g hexachlorocyclotriphosphazene Dissolve in 20ml tetrahydrofuran and transfer to a constant pressure titration funnel, raise the temperature to 50°C under the protection of nitrogen, start to slowly add the hexachlorocyclotriphosphazene solution dropwise, after the drop, raise the temperature to 70°C and reflux for 5 hours to stop the reaction. After cooling, it was filtered, and the filtrate was distilled under reduced pressure, recrystallized from ethyl acetate, and dried under vacuum at 65°C for 2 hours to obtain a white solid product. Yield 81.4%.

[0031] The infrared characterization figure of the product obtained in this embodiment is as follows figure 1 As shown, wherein: 2974cm-1 is the C-H vibration absorption peak of the methy...

Embodiment 3

[0034] Add 8.84ml triethylamine and 6.25g neopentyl glycol and 40ml tetrahydrofuran solvent in the 250ml three-neck flask equipped with reflux condenser, constant pressure titration funnel, thermometer and magnetic stirrer, simultaneously 6.95g hexachlorocyclotriphosphazene Dissolve in 20ml tetrahydrofuran and transfer to a constant pressure titration funnel, raise the temperature to 50°C under the protection of nitrogen, start to slowly add the hexachlorocyclotriphosphazene solution dropwise, after the drop, raise the temperature to 70°C and reflux for 7 hours to stop the reaction. After cooling, it was filtered, and the filtrate was distilled under reduced pressure, recrystallized from ethyl acetate, and dried under vacuum at 65°C for 2 hours to obtain a white solid product. Yield 86.9%.

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Abstract

The invention discloses a halogen-free phosphazene expanding-type flame retardant and a preparation method thereof. The method comprises the following steps: dissolving an acid binding agent and neopentyl glycol in a solvent, and carrying out heating to 20-60 DEG C under the protection of inert gas; slowly dropwise adding a phosphonitrilic chloride trimer solution, finishing the adding in 0.5-1 hours, carrying out heating to 40-120 DEG C, carrying out a reflux reaction for 4-24 hours, carrying out cooling, then carrying out filtering, reduced pressure distillation and recrystallizing, and carrying out vacuum drying at 65-90 DEG C to obtain a white solid which is the target product. The flame retardant provided by the invention has an initial decomposition temperature of 300 DEG C and has good compatibility when blended with a polymer, and the flame retardant is not dissolved in water and has excellent transference resistance. The flame retardant is prepared by adopting a one-step method, the reaction raw materials are simple and easy to obtain, the process is simple, by-products are few, the synthesis efficiency is high, the solvent can be recycled and reused after the reduced pressure distillation, and the preparation method is easy to industrialize. The flame retardant has the characteristics that no halogen exists in the molecular structure, no toxic gas is generated in a combustion process, and the flame retardant provided by the invention has a low smoke amount, greenness and no environmental pollution compared with a conventional flame retardant.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and in particular relates to a halogen-free nitrogen and phosphorus flame retardant and a preparation method thereof. Background technique [0002] With the rapid development of polymer materials, the flame retardancy of polymer materials has also received close attention. At present, the most widely used flame retardants in the market are halogen flame retardants. Halogen flame retardants have the advantages of low price and high flame retardant efficiency. It will cause secondary damage to the affected people in the fire, and will also cause pollution and damage to the environment. With the enhancement of people's awareness of environmental protection, traditional halogenated flame retardants are gradually eliminated by the market, and research on new flame retardants with high efficiency, environmental protection and low toxicity has become an inevitable trend in the development of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/5399C08L67/02C07F9/6581
Inventor 刘生鹏殷祥许莉莉丁一刚熊芸孙国锋吴晓宇
Owner WUHAN INSTITUTE OF TECHNOLOGY
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