Imidazole polypyrophosphate flame retardant and preparation method thereof

The technology of imidazole phosphate and imidazolium phosphate is applied in the field of phosphorus nitrogen flame retardants, which can solve problems such as easy combustion, and achieve the effects of improving flame retardant efficiency, simple and practical preparation method, and high thermal stability.

Active Publication Date: 2020-04-21
JIANGSU JICUI ADVANCED POLYMER MATERIAL RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Polymer materials are widely used in various fields, but they are extremely flammable

Method used

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  • Imidazole polypyrophosphate flame retardant and preparation method thereof
  • Imidazole polypyrophosphate flame retardant and preparation method thereof
  • Imidazole polypyrophosphate flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Add 10 kg of 85% phosphoric acid solution into the reactor, the rotating speed is increased to 60rmp, and the temperature is increased to 100°C. Add a saturated aqueous solution of imidazole in a spray mode, wherein the imidazole content is 12.25 kg. After reacting for 1 hour, the water was distilled off under reduced pressure to obtain 20.5 kg of imidazolium phosphate as a white solid. Add imidazolium phosphate into the vacuum kneader, increase the speed to 50 rpm, replace with nitrogen for more than three times, raise the temperature to 280°C, and react for 3 hours to obtain imidazole pyropolymerized phosphate.

Embodiment 2

[0042] Add 10 kg of 85% phosphoric acid solution into the reactor, the rotating speed is increased to 60rmp, and the temperature is increased to 100°C. Add a saturated aqueous solution of imidazole in a spraying manner, wherein the content of imidazole is 12.25 kg, and adjust the pH of the solution to 5-6 to stop adding the saturated aqueous solution of imidazole. After reacting for 1 hour, the water was distilled off under reduced pressure to obtain 22.7 kg of imidazolium phosphate as a white solid. Add imidazolium phosphate into the vacuum kneader, increase the speed to 50 rpm, replace with nitrogen for more than three times, raise the temperature to 280°C, and react for 3 hours to obtain imidazole pyropolymerized phosphate.

Embodiment 3

[0044] Add 10 kg of 85% phosphoric acid solution into the reactor, the rotating speed is increased to 60rmp, and the temperature is increased to 100°C. Add a saturated aqueous solution of imidazole in a spraying manner, wherein the content of imidazole is 12.25 kg, and adjust the pH of the solution to 5-6 to stop adding the saturated aqueous solution of imidazole. After reacting for 1 hour, the water was distilled off under reduced pressure to obtain 23.1 kg of imidazolium phosphate as a white solid. Add imidazolium phosphate into the vacuum kneader, increase the rotation speed to 50 rpm, replace with nitrogen for more than three times, raise the temperature to 300°C, and react for 1.5 hours to obtain imidazole pyropolymerized phosphate.

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Abstract

The invention discloses an imidazole polypyrophosphate flame retardant and a preparation method thereof. Phosphoric acid and imidazole or derivatives thereof are mixed and reacted in a reaction deviceto obtain imidazole phosphate; and the imidazole phosphate is subjected to a dehydration reaction in an inert atmosphere or a high-boiling-point solvent at a reaction temperature of 250-300 DEG C toprepare the imidazole polypyrophosphate. The imidazole polypyrophosphate is a novel phosphorus-nitrogen synergistic environment-friendly flame retardant. An imidazole ring is a nitrogen source provider, and a condensed ring structure of the imidazole ring can effectively induce carbon formation and improve the flame retardant efficiency. The imidazole polypyrophosphate is high in cost performance,and the preparation method is simple, convenient and practical and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of phosphorus-nitrogen flame retardants, and particularly designs an imidazole pyrophosphate flame retardant and a preparation method thereof. Background technique [0002] Polymer materials are widely used in various fields, but they are extremely flammable. Flame retardants can effectively inhibit the flammability of polymer materials and reduce the risk of fire. Early halogen-containing flame retardants were widely used, but with the improvement of environmental protection requirements, the amount of halogen-free flame retardants has increased year by year and has become a development trend of flame retardants. Phosphorus-nitrogen flame retardants have excellent performance among halogen-free flame retardants due to the phosphorus-nitrogen synergistic effect. However, there are few types of phosphorus nitrogen flame retardants currently on the market, mainly ammonium polyphosphate and melamine polyphosphate. Co...

Claims

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Application Information

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IPC IPC(8): C08K3/32C08K5/3445C08L77/06C08L23/06C08K13/04C08K7/14C08K13/06C08K9/08C07D233/58C07D233/84
CPCC08L77/06C07D233/58C07D233/84C08L2201/02C08J5/08C08J5/10C08K2003/321C08L2201/22C08L23/26C08K9/08C08K7/14C08K5/3445C08K3/32Y02P20/52
Inventor 闻辉刘渊吴建国陈荣
Owner JIANGSU JICUI ADVANCED POLYMER MATERIAL RES INST CO LTD
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