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Supermolecular flame retardant based on ionic bonds and preparation method thereof

An ionic bond and supramolecular technology, applied in the field of new structural flame retardants, can solve the problems of not well-solved flame retardant efficiency and limited improvement, and achieve easy implementation, increase compatibility, and improve heat resistance. Effect

Active Publication Date: 2016-05-11
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the improvement range is limited, and its flame retardant efficiency has not yet been well resolved.

Method used

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  • Supermolecular flame retardant based on ionic bonds and preparation method thereof
  • Supermolecular flame retardant based on ionic bonds and preparation method thereof
  • Supermolecular flame retardant based on ionic bonds and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Take 3.5g (0.0103mol) of polyphosphoric acid and disperse it in 80ml of absolute ethanol, heat it in an oil bath at 70°C and stir under reflux, and blow nitrogen into it to prepare a solution E with a dispersion concentration of 0.1287mol / L. Dissolve 9g (0.0832mol) of p-phenylenediamine in 150ml of absolute ethanol, adjust the pH value to about 6.5 with formic acid, and dissolve it under heating at 60°C to prepare an acidified concentration of 0.5547mol / L p-phenylenediamine Solution D. Take 50ml of solution D and add it dropwise to E, and drop it into the flask at a rate of 1-2 drops per second to form a precipitate. After a reaction time of 3 hours, add 2g of octadecylamine (0.0074mol) to it. After reflux for 2 hours, remove the solvent by filtration, wash with ethanol three times, dry the product in a blast oven at 70°C for 1 hour, transfer to a vacuum oven at 50°C for 5 hours, and grind it into powder to obtain the product after drying. The resulting structure is as...

Embodiment 2

[0060] Take the dicationic imidazolium chloride salt: Dissolve in absolute ethanol solution, fully dissolve it under heating conditions and prepare a 1.25mol / L solution for later use. Take 100ml of absolute ethanol in a 500ml three-necked flask, and add 3.8g (0.0112mol) of polyphosphoric acid into it, and mechanically stir for 1 hour under the condition of heating an oil bath at 70°C. At the same time, nitrogen protection is introduced and an exhaust gas treatment device is connected after the condenser. Take 25ml (0.0313mol) of the prepared imidazolium chloride salt solution in a constant pressure dropping funnel, and drop it into the flask at a rate of 1-2 drops per second. After a reaction time of 2 h, 2 g (0.0074 mol) of octadecylamine was added thereto. After refluxing for 2 hours, remove the solvent by filtration, wash with ethanol three times, dry the product in a blast oven at 80°C for 1 hour, transfer to a vacuum oven at 60°C for 5 hours, and grind it into powder t...

Embodiment 3

[0062] Take the dicationic imidazolium chloride salt: Dissolve in absolute ethanol solution, fully dissolve it under heating conditions and prepare a 1.25mol / L solution for later use. Take 100ml of absolute ethanol in a 500ml three-neck flask, and add 5g (0.0148mol) of polyphosphoric acid into it, and heat it in an oil bath at 70°C for 1 hour under mechanical stirring. At the same time, nitrogen protection is introduced and an exhaust gas treatment device is connected after the condenser. Take 30ml (0.0375mol) of the prepared imidazolium chloride salt solution in a constant pressure dropping funnel, drop it into the flask at a rate of 1-2 drops per second, and add 4g (0.018mol) KH550 into it after a reaction time of 2 hours. After refluxing for 2 hours, remove the solvent by filtration, wash with ethanol three times, dry the product in a blast oven at 80°C for 1 hour, transfer to a vacuum oven at 60°C for 5 hours, and grind it into powder to obtain the product after drying. ...

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Abstract

The invention discloses a supermolecular flame retardant based on ionic bonds and a preparation method thereof. An inner layer of the flame retardant is supermolecules B-A formed through ionic bond assembling of anions and cations, a shell layer is a dense or crosslinked-structural protection layer formed through ionic bonds or chemical bonds, and the inner layer and the outer layer are connected through ionic bonds or chemical bonds. The method comprises that a cationic raw material solution is dropwise added to an anionic raw material solution, a reaction is carried out for 1-5 h, and then surface treatment is carried out by a monofunctional modification method or a chemical crosslinking method. Through the way of ionic assembly, a three-dimensional structure is formed, and the stability of the flame retardant is enhanced to a certain extent; and a layer of stable protection layer is formed through the chemical method, so heat resistance and water resistance of the flame retardant can be effectively improved, the flame retardant can have good compatibility with a matrix and can be applied in plastics, rubber, adhesives, paints and other fields.

Description

technical field [0001] The invention relates to a novel structural flame retardant, in particular to an ion bond-based supramolecular structure flame retardant and a preparation method thereof. Background technique [0002] Polymer materials are widely used in all aspects of the national economy and human life. However, due to its own structure, most of them are flammable, so giving them a flame-retardant function is the key to their safe use. Traditional halogenated flame retardants have good flame retardant effects and occupy a large share in the flame retardant market. However, when the halogen-based flame retardants are burned, they are easy to release toxic smoke and gas, which will cause secondary damage. Therefore, it is of great significance to find more green and environmentally friendly flame retardant solutions. [0003] Intumescent flame retardant (IFR) is a green and environmentally friendly flame retardant, which has the characteristics of halogen-free, low ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/06C08K9/04C08K5/3445C08K5/3432C08K5/3415C08K5/3462C08K5/17C08K5/18
CPCC08K5/17C08K5/18C08K5/3415C08K5/3432C08K5/3445C08K5/3462C08K9/04C08K9/06
Inventor 李娟马东
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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