Preparation technology of phosphorus nitrogen series expansion type fire retardant

An intumescent flame retardant and preparation technology, which is applied in the direction of fireproof coatings, etc., can solve the problems of poor compatibility of polyolefins, high hygroscopicity, synthesis yield and environmental protection, etc.

Inactive Publication Date: 2006-08-30
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The present invention provides a synthesis route of phosphorus-nitrogen series intumescent flame retardant, which overcomes the disadvantages of improving synthesis yield and environmental protect

Method used

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  • Preparation technology of phosphorus nitrogen series expansion type fire retardant
  • Preparation technology of phosphorus nitrogen series expansion type fire retardant

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Add 68g of pentaerythritol and 250ml of phosphorus oxychloride into a 500ml three-neck flask, place in an oil bath at 110°C, stir vigorously for 24 hours, and absorb the hydrogen chloride gas produced by the reaction with NaOH aqueous solution. After the reaction was completed, it was cooled with an ice-water bath, filtered under reduced pressure, washed with dichloromethane, and the filtrate was vacuum-dried at room temperature (20° C.) for 6 hours to obtain a white solid powder (yield 76%). Take 29.7g of the white solid powder and dissolve it in a three-neck flask filled with 250ml of water, place it in a water bath at 90°C, stir and react for 0.5 hours, then add 100ml of 2mol / L NaOH aqueous solution dropwise, the dropping time is 1 hour, add dropwise Continue to react for 10 minutes after completion. Then add 25.2 g of melamine, add 1 g of sodium stearate after reacting for 1 hour, and continue to stir and reflux for 1 hour. After the reaction, cool with an ice-wate...

Embodiment 2

[0028] Add 68g of pentaerythritol and 250ml of phosphorus oxychloride into a 500ml three-neck flask, place in an oil bath at 110°C, stir vigorously for 24 hours, and absorb the hydrogen chloride gas produced by the reaction with NaOH aqueous solution. After the reaction was completed, it was cooled with an ice-water bath, filtered under reduced pressure, washed with dichloromethane, and the filtrate was vacuum-dried at room temperature (20° C.) for 6 hours to obtain a white solid powder (yield 76%). Take 29.7g of the white solid powder and dissolve it in a three-necked flask filled with 250ml of water, place it in a water bath at 90°C, stir and react for 0.5 hours, then add 2mol / L NaHCO dropwise 3 The aqueous solution was 100ml, and the dropwise addition time was 1 hour, and the reaction was continued for 10 minutes after the dropwise addition was completed. Then add 25.2 g of melamine, add 1 g of sodium stearate after reacting for 1 hour, and continue to stir and reflux for 1...

Embodiment 3

[0030] Add 68g of pentaerythritol and 250ml of phosphorus oxychloride into a 500ml three-neck flask, place in an oil bath at 110°C, stir vigorously for 24 hours, and absorb the hydrogen chloride gas produced by the reaction with NaOH aqueous solution. After the reaction was completed, it was cooled with an ice-water bath, filtered under reduced pressure, washed with dichloromethane, and the filtrate was vacuum-dried at room temperature (20° C.) for 6 hours to obtain a white solid powder (yield 76%). Take 29.7g of the white solid powder and dissolve it in a three-neck flask filled with 250ml of water, place it in a water bath at 90°C, stir and react for 0.5 hours, then add 100ml of 2mol / L NaOH aqueous solution dropwise, the dropping time is 1 hour, add dropwise Continue to react for 10 minutes after completion. Next, 25.2 g of melamine was added, and after 1 hour of reaction, 1 g of sodium dodecylbenzenesulfonate was added, and the stirring and reflux reaction was continued for...

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Abstract

The present invention discloses a preparation process of phosphonitrogen series expanded fire-retarding agent and fire-retarding agent prepared according to said preparation process. Said preparation process includes the following steps: making polybasic alcohol be reacted with phosphorus oxychloride, making the obtained product undergo the processes of hydrolysis and solution pH value regulation, then making said product be reacted with cyanurotriamide, the described polybasic alcohol includes pentaerythritol and dipentaerythritol, then using surfactant to make surface modification treatment so as to obtain the invented fire-retarding agent.

Description

technical field [0001] The invention relates to a preparation process of a flame retardant, in particular to a preparation process of a phosphorus-nitrogen series intumescent flame retardant and the phosphorus-nitrogen series intumescent flame retardant prepared according to the process. Background technique [0002] Intumescent flame retardant (IFR) is a flame retardant with phosphorus, nitrogen, and carbon as the main core elements. It can be combined with a flammable polymer to prepare a new type of flame retardant material. When the material is heated and burned, a uniform carbon foam layer will be formed on the surface. The carbon foam layer is dense and contains non-combustible gas, which has the functions of blocking heat and oxygen transfer and suppressing smoke, and can effectively prevent melting. drop. No toxic fumes are produced during the flame retardant process, and it is a new type of environmentally friendly flame retardant that can replace halogenated flame...

Claims

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Application Information

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IPC IPC(8): C09K21/12C08K5/5399
Inventor 杨辉周箭方晨鹏谢飞慕长江
Owner ZHEJIANG UNIV
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