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Reaction type P-N containing intumescent fire retardant and synthetic method thereof

An intumescent flame retardant and a synthesis method technology, applied in the field of flame retardants, can solve the problems of high synthesis temperature, low thermal stability and low carbon-forming properties, and achieve simple equipment, good carbon-forming properties and simple synthesis process. Effect

Inactive Publication Date: 2013-09-04
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The present invention provides a reactive P-N-containing intumescent flame retardant and its synthesis method in order to solve the problems of low thermal stability, low carbon formation and high synthesis temperature in the existing intumescent flame retardants.

Method used

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  • Reaction type P-N containing intumescent fire retardant and synthetic method thereof
  • Reaction type P-N containing intumescent fire retardant and synthetic method thereof
  • Reaction type P-N containing intumescent fire retardant and synthetic method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] The first step is to dissolve 9.23g (0.05mol) cyanuric chloride in 50mL acetone, pour this solution into 110mL distilled water, stir, keep the temperature at 0-3°C, add 2mol / L HCl aqueous solution to adjust the pH value to 1-2, slowly add 8.8g (0.05mol) sodium p-aminobenzenesulfonate dropwise, add dropwise 0.05mol sodium carbonate aqueous solution, adjust the pH value to 7-8, react for about 6h, filter with suction, and wash the obtained solid with acetone 2 times and dried to obtain 14 g of white solid, namely intermediate I (yield 81.4%).

[0028] In the second step, take 3.44g (10mmol) of intermediate I, dissolve it in 60mL of distilled water, add 50mL of acetone, slowly add 1.26g (12mmol) of diethanolamine (dissolved in 20mL of water) at room temperature, and heat to 45 ℃, add sodium carbonate to neutralize the generated hydrogen chloride, adjust the pH value to 8-9, then react for about 7 hours, remove the solvent, wash the obtained solid twice with ethanol and ace...

Embodiment 2

[0038] In the first step, take 9.23g (0.05mol) of cyanuric chloride and dissolve it in 50mL of acetone, pour this solution into 110mL of distilled water (about 100g of crushed ice), stir, keep the temperature at 3-5°C, and add 2mol / L of HCl aqueous solution, adjust the pH value to 1-2, slowly add 8.8g (0.05mol) sodium p-aminobenzenesulfonate dropwise, add dropwise 0.05mol sodium carbonate aqueous solution, adjust the pH value to 7-8, react for about 6h, pump After filtration, the resulting solid was washed 2-3 times with acetone, and dried to obtain 14 g of a white solid, which was Intermediate I (yield 81.4%).

[0039] In the second step, take 3.44g (10mmol) of intermediate I, dissolve it in 60mL of distilled water, add 50mL of acetone, slowly add 1.1g (10mmol) of diethanolamine (dissolved in 20mL of water) at room temperature, and heat to 40 ℃, add sodium carbonate to neutralize the generated hydrogen chloride, adjust the pH value to 8-9, then react for about 7 hours, remov...

Embodiment 3

[0042] In the first step, take 5.53g (0.03mol) of cyanuric chloride and dissolve it in 50mL of acetone, pour this solution into 110mL of distilled water (about 100g of crushed ice), stir, keep the temperature at 0-5°C, and slowly add 5.85g (0.03mol) of sodium p-aminobenzenesulfonate, add dropwise sodium carbonate aqueous solution, adjust the pH value to 7-8, react for about 5.5h, filter with suction, wash the obtained solid with acetone 2-3 times, dry to obtain a white solid , which is intermediate I8.5g, (82.4% yield).

[0043] In the second step, take 3.44g (10mmol) of intermediate I, dissolve it in 60mL of distilled water, add 50mL of acetone, slowly add 1.26g (12mmol) of diethanolamine (dissolved in 20mL of water) at room temperature, and heat to 45 ℃, add sodium carbonate to neutralize the generated hydrogen chloride, adjust the pH value to 8-9, then react for about 6 hours, remove the solvent, wash the obtained solid twice with ethanol and acetone, and dry to obtain 3.65...

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Abstract

The invention discloses a reaction type P-N containing intumescent fire retardant and a synthetic method thereof and solves the problems of low thermal stability, low carbon-forming property and high preparation temperature of the prior art. The synthetic method comprises the following steps of: (1) adding cyanuric chloride, sodium sulfanilate and acid binding agent sodium carbonate, a molar ratio of which is 1:1:1, to a solution of water and acetone, a volume ratio of which is 11:5, reacting for 5-6H at the temperature of 0-5 DEG C, and generating a midbody I; (2) adding the midbody I, diethanol amine and the acid binding agent sodium carbonate, a molar ratio of which is 1:1.2:1, to a solution of water and acetone, a volume ratio of which is 6:5, reacting for 6h at the temperature of 35-55 DEG C, and generating a midbody II; (3) taking 5mmol of the midbody II, stirring and dissolving the midbody II in 60mL of methylene chloride, then adding 0.77g of phosphorus oxychloride at a room temperature, reacting for 1h, adding 1g of triethylamine in twice, and reacting for 6-7h at the temperature of 25-45 DEG C, thereby obtaining the reaction type P-N containing intumescent fire retardant. The reaction type P-N containing intumescent fire retardant integrates a carbon source, an acid source and a gas source and has higher thermal stability, better carbon-forming performance and good flame retardant effect; and the synthetic process is simple and is low in cost.

Description

technical field [0001] The invention relates to a flame retardant, in particular to a reactive P-N-containing intumescent flame retardant and a synthesis method thereof. Background technique [0002] With the continuous development and progress of science and technology, and the continuous improvement of people's living standards, chemical fibers, plastics, rubber and other polymer materials have been widely used in various fields such as production, life, national defense construction and scientific research, and play an increasingly important role. more important role. However, these materials also have a common feature, that is, flammable or combustible, which is particularly easy to cause fire accidents. This potential flammability has seriously affected people's life and property safety. With the increasing awareness of environmental protection, people not only require flame retardants to have good flame retardancy, but also require the ability to suppress smoke and re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6584C09K21/12
Inventor 刘亚青赵培华张美孙付宇赵贵哲
Owner ZHONGBEI UNIV