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Synthesis method of organosilicone modified superfine aluminum hypophosphite

A technology of aluminum hypophosphite and synthesis method, which is applied in the preparation of inorganic flame retardant materials and in the field of inorganic chemistry, can solve the problems of large smoke generation, poor thermal stability, and large hygroscopicity, so as to reduce the dosage and improve the mechanical mechanics Performance, the effect of mild reaction conditions

Inactive Publication Date: 2016-08-17
SHIFANG TAIFENG NEW FLAME RETARDANT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The flame retardant of traditional engineering plastics such as PBT and PA usually adopts halogen flame retardant system, but because the flame retardant materials of halogen compounds may produce PBDD (polybrominated dibenzodioxin) and PBDF (polybrominated substituted dibenzofuran) and other toxic substances, and usually have a large amount of smoke. In developed countries such as Europe and the United States, they are gradually being replaced by halogen-free flame retardants. Problems such as high hygroscopicity and poor thermal stability have not been widely used in flame retardant plastics

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Prepare 600g of 30% sodium hypophosphite aqueous solution and 500g of 50% aluminum sulfate aqueous solution. Set the sodium hypophosphite solution as the bottom solution. After the temperature of the bottom solution rises to 85 degrees, add 2g of dispersant and continue to stir. Heating, when the temperature rises to 95 degrees, gradually add aluminum sulfate solution to the sodium hypophosphite solution at a stirring speed of 100r / min and a dripping rate of 20g / min. After the addition is completed, continue to keep the material temperature at 95 degrees and react for 30 minutes. Then, add dropwise an organic silicon solution with a mass fraction of 30% for 0.5h alcoholysis, continue to stir for 0.5h, then cool to room temperature, wash several times and use 5% BaCl 2 Solution inspection, after the filtrate did not produce white precipitate, dried to obtain organic silicon modified ultrafine aluminum hypophosphite product, the yield was 98%, the average particle size was 4...

Embodiment 2

[0021] Prepare 600g of 35% sodium hypophosphite aqueous solution and 500g of 55% aluminum sulfate aqueous solution. Set the sodium hypophosphite solution as the bottom solution. After the temperature of the bottom solution rises to 90 degrees, add 2g of dispersant and continue stirring. Heating, when the temperature rises to 95 degrees, gradually add aluminum sulfate solution to the sodium hypophosphite solution at a stirring speed of 200r / min and a dripping rate of 10g / min. After the addition is completed, continue to keep the material temperature at 95 degrees for 30 minutes. Then add dropwise an organic silicon solution with a mass fraction of 50% alcoholysis for 1 hour, continue to stir for 0.5 hours, then cool to room temperature, wash several times and use 5% BaCl 2 Solution inspection, after the filtrate did not produce white precipitate, dried to obtain the organic silicon modified ultrafine aluminum hypophosphite product, the yield was 99%, and the average particle size ...

Embodiment 3

[0023] Prepare 600g of 40% sodium hypophosphite aqueous solution and 500g of 60% aluminum sulfate aqueous solution. Set the sodium hypophosphite solution as the bottom solution. After the temperature of the bottom solution rises to 90 degrees, add 3g of dispersant and continue to stir. Heating, when the temperature rises to 95 degrees, gradually add aluminum sulfate solution to the sodium hypophosphite solution at a stirring speed of 400r / min and a dripping rate of 5g / min. After the addition is completed, continue to keep the material temperature at 95 degrees and react for 10 minutes. Then add dropwise an organosilicon solution with a mass fraction of 50% for alcoholysis for 0.5 h, continue to stir for 1 h, then cool to room temperature, wash several times and use 5% BaCl 2 Solution inspection, after the filtrate did not produce white precipitate, dried to obtain organosilicon modified ultrafine aluminum hypophosphite product, the yield was 97%, and the average particle size was...

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Abstract

The invention discloses a method for synthesizing organosilicon-modified ultrafine aluminum hypophosphite, which comprises the following steps: 1) preparing sodium hypophosphite aqueous solution; 2) preparing aluminum sulfate aqueous solution; 3) preparing organosilicon-modified ultrafine aluminum hypophosphite : First add a dispersant to the sodium hypophosphite solution, then slowly add the aluminum sulfate aqueous solution to the sodium hypophosphite solution dropwise, and continue to stir for 0 to 3 hours; After stirring for 0-1h, cool to room temperature, wash and test the filtrate with a certain concentration of barium chloride solution, and wait for no white precipitate to appear in the filtrate, then place it in an oven for drying to obtain organosilicon-modified ultrafine aluminum hypophosphite product . The present invention uses organic silicon as a modifier to make organic silicon modified aluminum hypophosphite and high molecular compound more tightly combined, improve the interfacial binding force between the flame retardant and high molecular material, the reaction conditions are mild, and the yield is high , which is more suitable for industrialization.

Description

Technical field [0001] The invention belongs to the field of preparation of inorganic flame-retardant materials, relates to the field of inorganic chemistry, and specifically relates to a method for synthesizing superfine aluminum hypophosphite modified with organic silicon. Background technique [0002] Traditional engineering plastics, such as PBT and PA, usually use halogen-based flame-retardant systems. However, flame-retardant materials made of halogen-containing compounds may produce PBDD (polybrominated dibenzodioxin) and PBDF (polybrominated dioxins) when they burn. Substitute dibenzofuran) and other toxic substances, which usually emit a large amount of smoke, are gradually being replaced by halogen-free flame retardants in developed countries such as Europe and the United States. The IFR intumescent flame retardant system, which has been given high expectations, is also due to its existence The problems of high hygroscopicity and poor thermal stability have not been wid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/40C09C3/12
CPCC09C1/40C09C3/12
Inventor 黄剑陈荣义袁明强练杰
Owner SHIFANG TAIFENG NEW FLAME RETARDANT
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