Phosphosilicate containing fire retardant and its prepn process

A technology of flame retardant and silicate, which is applied in the field of phosphorus-containing silicate flame retardant and its preparation, can solve the problems of thermal stability and migration affecting material performance and surface finish, and achieve the purpose of inhibiting thermal oxidation degradation Reaction, less corrosive gas, effect of preventing mass loss

Inactive Publication Date: 2005-12-14
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When most phosphorus-containing flame retardants are used together with halogen-containing compounds, the flame-retardant effect can be greatly improved, but because halogen flame retardants generate more smoke and corrosive gases during combustion, they have been affected by dioxins. Problems, and gradually replaced by halogen-free flame retardants
The organophosphorus flame retardants widely used in polymer materials are phosphates and phosphonates, but their thermal stability and migration problems often affect the performance and surface finish of materials

Method used

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  • Phosphosilicate containing fire retardant and its prepn process
  • Phosphosilicate containing fire retardant and its prepn process
  • Phosphosilicate containing fire retardant and its prepn process

Examples

Experimental program
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Effect test

Embodiment 1

[0018] First, 10.0g (0.05mol) of 1-oxo-1-phospha-2,6,7-trioxabicyclo[2.2.2]-4-chloromethyloctane was stirred and dissolved in 50ml of Dimethylformamide, then add 12.5g (0.05mol) of pentacoordinate silicon potassium compound, stir vigorously, then raise the temperature to 65°C for constant temperature reaction; when the pH is 7, stop the reaction, cool down to room temperature, suction filter, remove The salt generated therein is added to the filtrate with 100ml of reverse phase precipitation reagent acetone to produce a large amount of white precipitated matter, which is filtered, and the white matter is placed in a vacuum drying oven and dried at a constant temperature of 70°C for 24 hours to obtain the white granular matter which is the present invention. The yield of the phosphorus-containing silicate flame retardant is 80%. The analysis test results are as follows:

[0019] Fourier infrared: 3384cm -1 、2956cm -1 、1465cm -1 、1229cm -1 、1094cm -1 、1045cm -1 、952cm -1...

Embodiment 2

[0023] First, 2.0g (0.01mol) of 1-oxo-1-phospha-2,6,7-trioxabicyclo[2.2.2]-4-chloromethyloctane was stirred and dissolved in 5ml of Dimethylacetamide, then add 5g (0.02mol) of pentacoordinate silicon potassium compound, stir vigorously, and then raise the temperature to 60°C for constant temperature reaction; when the pH is 7, stop the reaction, cool down to room temperature, and remove it by suction filtration. Generated salt, then add 25ml of reverse-phase precipitation reagent acetone to the filtrate, produce a large amount of white precipitated matter, filter, put the white matter in a vacuum drying oven for 30 hours at a constant temperature of 60°C, and obtain the white granular matter that is the product of the present invention. A phosphorus-containing silicate flame retardant is described with a yield of 76%.

Embodiment 3

[0025] First, 2.0g (0.01mol) of 1-oxo-1-phospha-2,6,7-trioxabicyclo[2.2.2]-4-chloromethyloctane was stirred and dissolved in 15ml of Dimethyl sulfoxide, then add 3.75g (0.015mol) of pentacoordinate silicon potassium compound, stir vigorously, then raise the temperature to 70°C for constant temperature reaction; when the pH is 7, stop the reaction, cool down to room temperature, suction filter, remove The salt generated therein is added to the filtrate with 30ml of reverse-phase precipitation reagent acetone to produce a large amount of white precipitated matter, which is filtered, and the white matter is placed in a vacuum drying oven and dried at a constant temperature of 80°C for 18 hours to obtain white granular matter which is the present invention. The yield of the phosphorus-containing silicate flame retardant is 82%.

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Abstract

The present invention discloses one kind of phosphosilicate containing fire retardant with shown structure expression and its preparation process. The preparation process includes following steps: dissolving 1-oxy-1-phospha-2, 6, 7-trioxa doublecycle[2.2.2]-4-chloromethyl octane in some solvent, adding penta-complex silicon potassium compound and heating to 60-70 deg.c for constant temperature reaction until pH value reaches 7; lowering the temperature to room temperature, suction filtering, adding reverse precipitant to produce white precipitate, filtering, and drying the precipitate at 60-80 deg.c for 18-30 hr to obtain the phosphosilicate containing fire retardant. The fire retardant is well compatible with material, has no influence on the use performance, color, surface smoothness, etc of the product, has high fire retarding efficiency, no toxicity, no bad smell, and no toxic matter and smoke released while burning.

Description

technical field [0001] The invention relates to the technical field of flame retardant synthesis, in particular to a phosphorus-containing silicate flame retardant and a preparation method thereof. Background technique [0002] In the production and application of flame retardants, while exploring and synthesizing new high-efficiency flame retardants, people also compound flame retardants with better flame retardant effects. That is to use the interaction between flame retardants in order to improve the performance of flame retardants and achieve the so-called "synergistic effect" of flame retardants. When most phosphorus-containing flame retardants are used together with halogen-containing compounds, the flame-retardant effect can be greatly improved, but because halogen flame retardants generate more smoke and corrosive gases during combustion, they have been affected by dioxins. Problems, and gradually replaced by halogen-free flame retardants. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K21/12
Inventor 刘安华张利利温永向曾幸荣
Owner SOUTH CHINA UNIV OF TECH
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