A core-shell type silicon-containing synergistic flame retardant and preparation method thereof

A technology of synergistic flame retardants and flame retardants, applied in the field of flame retardants, can solve the problems of high production costs, limited coating effect, and staying in the laboratory stage, etc., to achieve improved processing performance, good recycling effect, The effect of meeting strict requirements

Active Publication Date: 2012-02-01
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the production cost of this kind of flame retardant is high, most of them stay in the laboratory stage, and some of them are used in special occasions
U.S. Patent US6,444,315 and Japanese Patent JP-A3,131,508 selected alkoxy silicone-containing halogen-free flame retardants and ammonium cyanurate flame retardants made of oxalic acid, phthalic acid, and isocyanic acid. Microencapsulation, its encapsulation method may be directly dripped, sprayed, injected or suspended in the presence of organic solvents under heating conditions, but alkyl siloxy silicone oils cannot interact well with flame retardants, and encapsulation limited role

Method used

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  • A core-shell type silicon-containing synergistic flame retardant and preparation method thereof
  • A core-shell type silicon-containing synergistic flame retardant and preparation method thereof
  • A core-shell type silicon-containing synergistic flame retardant and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0026] Add 50ml of deionized water and 150ml of ethanol to a reaction kettle equipped with a stirring and reflux device. After stirring evenly, add 50g of ammonium polyphosphate and 1g of OP-10, heat to 45°C while stirring, and add concentrated ammonia water to adjust the pH value to 9. ~11, then slowly add 5g of organosilicon oxide compound dropwise at a rate of 3ml / min, stir for 150min, then lower the reaction kettle to room temperature, filter, wash, and dry the filter cake at 120°C and 30mmHg to obtain 51.4 g of the core-shell silicon-containing synergistic flame retardant product of the present invention with good fluidity.

[0027] If other conditions remain unchanged, the flame retardant ammonium polyphosphate in this embodiment is replaced by antimony trioxide, aluminum hydroxide, magnesium hydroxide, aluminum oxalate, calcium aluminate, calcium carbonate, hydroxide Inorganic flame retardants including calcium, zinc borate, borax, expanded graphite or red phosphorus; ...

Embodiment 2

[0029] Add 50ml of deionized water and 150ml of ethanol to a reaction kettle equipped with a stirring and reflux device. After stirring evenly, add 50g of ammonium polyphosphate and 1g of OP-10, heat to 45°C while stirring, add concentrated ammonia water, and adjust the pH value at 9 to 11, then slowly add 7.5g of organosilicon oxide compound dropwise at a rate of 5ml / min, the dropwise addition is completed within 25 minutes, and the reaction is stirred for 180 minutes, then the reactor is lowered to room temperature, filtered, washed, and the filter cake is Dry at 120°C and 30mmHg to obtain 52.6g of the core-shell silicon-containing synergistic flame retardant product of the present invention with good fluidity.

Embodiment 3

[0031] Add 50ml of deionized water and 150ml of ethanol to a reaction kettle equipped with a stirring and reflux device. After stirring evenly, add 50g of ammonium polyphosphate and 1g of OP-10, heat to 45°C while stirring, add concentrated ammonia water, and adjust the pH value at 9 to 11, then slowly add 10 g of organosilicon oxide compound dropwise at a rate of 3 ml / min, stir for reaction, after reacting for 330 minutes, cool, filter, wash, and dry the filter cake at 120°C and 30 mmHg to obtain 53.3 g of free The core-shell silicon-containing synergistic flame retardant product of the invention has good fluidity.

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Abstract

The invention discloses a core-shell type silicon-containing synergistic flame retardant and a preparation method thereof, which is characterized in that 50ml of deionized water and 150ml of ethanol are added into a reaction kettle equipped with a stirring and reflux device, and after stirring evenly, 50g of Ammonium polyphosphate and 1g OP-10, heated to 45°C under stirring, added concentrated ammonia water to adjust the pH value to 9-11, then slowly added 5g organic silicon oxide compound dropwise at a speed of 3ml / min, stirred for 150min, and then The reaction kettle was lowered to room temperature, filtered, washed, and the filter cake was dried at 120°C and 30mmHg. The average particle size of the obtained product does not increase significantly, the free flow of particles is good, the shell is dense and uniform, the water property is greatly reduced, and the high temperature water resistance is significantly improved. It can be used as a polymer material such as polyolefin, polyurethane, rubber, and foam. Flame retardant, it can also be used for flame retardant of paper, wood, fabric, etc.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and in particular relates to a core-shell silicon-containing synergistic flame retardant and a preparation method thereof. Background technique [0002] As people pay more and more attention to environmental protection and personal health, the European Union issued the "Directive on the Prohibition of the Use of Certain Hazardous Substances in Electrical and Electronic Equipment" ("ROHS Directive"), which makes manufacturers of flame-retardant materials in various countries begin to use caution The attitude towards the application of brominated flame retardants in polymers has led to the emergence of non-halogenated flame retardants, especially phosphorus-based flame retardants, which are constantly moving from the laboratory to the market. On pages 13-20 and 48-53 of the book "Basics and Applications of Halogen-Free Flame-Retardant Polymers" (Wang Jianqi, Science Press, 2005.6), it is p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09K21/00C08K9/10
Inventor 胡源倪健雄宋磊
Owner UNIV OF SCI & TECH OF CHINA
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