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Method for preparing reactive phosphorus-nitrogen series intumescent flame retardant

An intumescent flame retardant, phosphorus-nitrogen-based technology, used in the field of flame retardant preparation, can solve the problems of poor compatibility with polymers, exudation, easy migration, etc., and achieves low equipment requirements and environmental pollution. Small, good thermal stability

Inactive Publication Date: 2012-05-09
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the invention is to solve the disadvantages of poor compatibility between existing intumescent flame retardants and polymers, which are prone to migration and exudation, and to provide a preparation method for reactive phosphorus-nitrogen series intumescent flame retardants, so that It is chemically bonded with the polymer, so as to achieve the dual purpose of non-migration and flame retardancy of the flame retardant

Method used

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  • Method for preparing reactive phosphorus-nitrogen series intumescent flame retardant
  • Method for preparing reactive phosphorus-nitrogen series intumescent flame retardant
  • Method for preparing reactive phosphorus-nitrogen series intumescent flame retardant

Examples

Experimental program
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Effect test

Embodiment 1

[0020] In a 1000ml three-necked flask equipped with a stirrer, a constant pressure funnel and a reflux condenser, dissolve 19.0g (0.1mol) of cyanuric chloride in 160ml of acetone, and add 5.8 g (0.1mol) allyl alcohol, then add 45g of 10% NaOH solution with a mass concentration, and react for 1.0 hour under stirring and at a temperature of -5°C to 0°C to obtain colorless 2-allyloxy-4,6- Dichloro-1,3,5-triazine intermediate (I) solution. Add 25.0g (0.2mol) methylamine aqueous solution dropwise to the intermediate product (I) solution, and add dropwise 90g of 10% NaOH solution with a mass concentration of 90g, react under stirring and 20°C for 2.0 hours, and then at 55°C React for 1.0 hour under cooling, spin off the solvent, filter with suction, wash, and dry to obtain white flaky solid 2-allyloxy-4,6-dimethylamino-1,3,5-triazine intermediate The product (II) was 17.6 g, and the yield was 90.1%.

[0021] In a 1000ml three-neck flask equipped with a stirrer, a constant pressure...

Embodiment 2

[0026] In a 1000ml three-neck flask equipped with a stirrer, a constant pressure funnel and a reflux condenser, dissolve 19.0g (0.1mol) of cyanuric chloride in 160ml of acetone, and drop 5.8g (0.1mol) allyl alcohol, then add 45g of 10% NaOH solution with a mass concentration, and react for 0.5 hours under stirring and at a temperature of 0°C to 5°C to obtain colorless 2-allyloxy-4,6-dichloro -1,3,5-Triazine intermediate product (I) solution. Add dropwise 25.0g (0.2mol) methylamine aqueous solution to the intermediate product (I) solution, and dropwise add 90g of a mass concentration of 10% NaOH solution, react under stirring and 25°C for 1.5 hours, and then under 60°C React for 1.0 hour under cooling, spin off the solvent, filter with suction, wash, and dry to obtain white flaky solid 2-allyloxy-4,6-dimethylamino-1,3,5-triazine intermediate The product (II) was 17.0 g, and the yield was 87.3%.

[0027]In a 1000ml three-neck flask equipped with a stirrer, a constant pressure ...

Embodiment 3

[0029] In a 1000ml three-neck flask equipped with a stirrer, a constant pressure funnel and a reflux condenser, dissolve 28.1g (0.15mol) of cyanuric chloride in 240ml of acetone, and drop 8.7g (0.1mol) allyl alcohol, then add 60g of 10% NaOH solution with a mass concentration, and react for 1.0 hour under stirring and at a temperature of -5°C to 0°C to obtain colorless 2-allyloxy-4,6-di Chloro-1,3,5-triazine intermediate (I) solution. Add dropwise 37.2g (0.15mol) of methylamine aqueous solution to the intermediate product (I) solution, and dropwise add 120g of 10% NaOH solution with a mass concentration of 120g, react under stirring and 25°C for 1.5 hours, and then under 60°C React for 0.5 hours under cooling, evaporate the solvent by rotary evaporation, suction filter, wash, and dry to obtain white flaky solid 2-allyloxy-4,6-dimethylamino-1,3,5-triazine intermediate The product (II) was 27.1 g, and the yield was 92.5%.

[0030] In a 2000ml three-neck flask equipped with a s...

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Abstract

The invention discloses a method for preparing a reactive phosphorus-nitrogen series intumescent flame retardant, which comprises the steps of: preparing an intermediate product (I), i.e. 2-alkenylalkoxy-4,6-dichloro-1,3,5-triazine, through the reaction of cyanuric chloride and alkyl enol; preparing an intermediate product (II), i.e. 2-alkenylalkoxy-4,6-dialkyl amido-1,3,5-triazine, through the reaction of the intermediate product (I) and alkyl hartshorn; and preparing a 2-alkenylalkoxy-4,6-dialkyl amido-1,3,5-triazine (poly)phosphate of the flame retardant through the reaction of the intermediate product (II) and (poly)phosphoric acid. Under the initiation action of peroxide, an alkenylalkoxy double-bonded group in the flame retardant can be chemically bonded with a polymer. The invention has no transfer, no effusion, no halogen and environmental protection and integrates an acid source, a carbon source, a gas source and a reactive group into a whole. During combustion, the surface of a high polymer can form a uniform carbonaceous foamlayer which has the functions of heat insulation, oxygen insulation, smoke suppression and flame retarding.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant, in particular to a preparation method of a reactive phosphorus-nitrogen series expansion type flame retardant. Background technique [0002] The intumescent flame retardant is mainly composed of three parts: acid source (dehydrating agent), carbon source (carbon forming agent) and gas source (nitrogen source, expansion agent). When burning, the intumescent flame retardant produces a uniform porous expanded carbon layer on the surface of the polymer, which prevents the transfer of heat and the diffusion of oxygen, effectively delays the thermal degradation of the polymer, reduces the release of combustible gas and smoke, and prevents the polymer from burning The resulting molten drop behavior, so as to achieve the purpose of interrupting the polymer combustion. [0003] Intumescent flame retardants are usually divided into two types: mixed type and single-component type. The mixed typ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K5/52
Inventor 陈朝晖张丽芳樊晓娜林新花孙仙平
Owner SOUTH CHINA UNIV OF TECH
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