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A kind of supercritical method prepares nano-phosphorus-nitrogen intumescent flame retardant method

A supercritical, flame retardant technology, applied in the production of bulk chemicals, organic chemistry, etc., can solve the problems of large particle size, low flame retardant efficiency, and large impact on the mechanical properties of polymer matrix.

Active Publication Date: 2017-07-18
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to provide a nano-phosphorus nitrogen flame retardant prepared by supercritical carbon dioxide in view of the shortcomings of the existing phosphorus nitrogen flame retardants, such as large particle size, low flame retardant efficiency, and great influence on the mechanical properties of the polymer matrix. agent method

Method used

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  • A kind of supercritical method prepares nano-phosphorus-nitrogen intumescent flame retardant method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Accurately weigh a certain amount of melamine, phosphoric acid and surfactant according to the formula (the mass ratio of melamine and phosphoric acid is 1:1, and the quality of surfactant is 2% of the total mass of melamine and phosphoric acid), and add it to a certain amount of distilled water ( The amount of distilled water is 10% of the total mass of melamine and phosphoric acid), stirred to make it fully dissolved and prepared into a solution. Put the above solution into a supercritical reaction kettle, open the carbon dioxide steel cylinder, the carbon dioxide gas is cooled into a liquid by a refrigerator, and then pressurized by a high-pressure pump into the reaction kettle. Control a certain pressure (30MPa) and temperature (353K), and keep the pressure for a certain period of time (40min); open the pressure relief port to reduce the pressure in the supercritical reactor to normal pressure, and you can get nanometer particles with a number average particle size o...

Embodiment 2

[0025] Accurately weigh a certain amount of melamine, phosphoric acid and surfactant according to the formula (the mass ratio of melamine and phosphoric acid is 1.5:1, and the quality of surfactant is 0.5% of the total mass of melamine and phosphoric acid), and add it to a certain amount of distilled water ( The amount of distilled water is 50% of the total mass of melamine and phosphoric acid), stirred to make it fully dissolved and prepared into a solution. Put the above solution into a supercritical reaction kettle, open the carbon dioxide steel cylinder, the carbon dioxide gas is cooled into a liquid by a refrigerator, and then pressurized by a high-pressure pump into the reaction kettle. Control a certain pressure (40MPa) and temperature (363K), and keep the pressure for a certain period of time (20min); open the pressure relief port to reduce the pressure in the supercritical reactor to normal pressure, and you can get nanometer particles with a number average particle si...

Embodiment 3

[0027] Accurately weigh a certain amount of melamine, phosphoric acid and surfactant according to the formula (the mass ratio of melamine and phosphoric acid is 1:1.2, and the quality of surfactant is 1% of the total mass of melamine and phosphoric acid), and add it to a certain amount of distilled water ( The amount of distilled water is 20% of the total mass of melamine and phosphoric acid), stirred to make it fully dissolved and prepared into a solution. Put the above solution into a supercritical reaction kettle, open the carbon dioxide steel cylinder, the carbon dioxide gas is cooled into a liquid by a refrigerator, and then pressurized by a high-pressure pump into the reaction kettle. Control a certain pressure (35MPa) and temperature (363K), and keep the pressure for a certain period of time (60min); open the pressure relief port to reduce the pressure in the supercritical reactor to normal pressure, and you can get nanometer particles with a number average particle size...

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Abstract

The invention discloses a method for preparing nano phosphorus-nitrogen inrumescent flame retardant melamine phosphate (MP) by means of a supercritical method. The method comprises the steps that phospholipid melamine, phosphoric acid, surface active agents and the like are weighed, and are dissolved in a little distilled water; the dissolved solution is added to a supercritical reaction kettle, temperature and pressure are controlled, and the pressure is kept for certain time; the nano phosphorus-nitrogen inrumescent flame retardant melamine phosphate (MP) is obtained by releasing the pressure. The characteristics that supercritical carbon dioxide fluid is high in solvent resistance and environmentally friendly and can be easily separated from products after preparation is finished are utilized, and the nano phosphorus-nitrogen inrumescent flame retardant is prepared. In the preparation process of the method, toxic organic solvent is not used, and pollution to environment is avoided. The prepared phosphorus-nitrogen inrumescent flame retardant is small in particle size and easy to disperse, the problem that nano particles are poor in dispersity in polymer matrixes is solved, and therefore high fire resistance is achieved. The process is simple, and cost is low.

Description

technical field [0001] The invention belongs to the field of flame retardant preparation, and in particular relates to a method for preparing a nano-scale phosphorus-nitrogen expansion type flame retardant by using supercritical carbon dioxide. [0002] technical background [0003] Intumescent flame retardant (IFR) is an environmentally friendly green composite flame retardant mainly composed of nitrogen and phosphorus. It does not contain halogen and does not use antimony oxide as a synergist. The foam expands to form a carbon foam layer, which has the functions of heat insulation, oxygen insulation, smoke suppression, and anti-drip. It has excellent flame retardant performance, low smoke, low toxicity, and no corrosive gas generation. Toxic and environmentally friendly flame retardants. After the 1990s, the research on intumescent flame retardants gradually became active, and it was recognized as one of the effective ways to realize the non-halogenation of flame retardant...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/56
CPCC07D251/56Y02P20/54
Inventor 何丹农徐少洪张春明王艳丽冉伟陈超金彩虹
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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