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Single-component intumescent flame retardant with free radical quenching function, preparation method and applications thereof

An intumescent flame retardant, one-component technology, used in the preparation and application of polymer halogen-free flame retardants, can solve the problems of poor matrix compatibility, large hygroscopicity, loss, etc., and achieve good compatibility, Effect of improving dispersibility and improving flame retardant efficiency

Active Publication Date: 2020-02-11
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a single-component intumescent flame retardant with free radical quenching function to address the shortcomings of the existing intumescent flame retardants, which can effectively overcome the existing multi-component intumescent flame retardants. The agent has disadvantages such as high hygroscopicity, poor compatibility with the matrix, and easy migration to the surface of the polymer and loss; at the same time, it is endowed with a free radical quenching function, so that the free radical quenching function and the expansion of charcoal are efficiently coupled to play a highly efficient flame retardant effect

Method used

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  • Single-component intumescent flame retardant with free radical quenching function, preparation method and applications thereof
  • Single-component intumescent flame retardant with free radical quenching function, preparation method and applications thereof
  • Single-component intumescent flame retardant with free radical quenching function, preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] (1) Preparation of macromolecule char-forming agent containing hindered amine structure

[0045] At 0°C, add 250mL of acetone and 18.8g (0.1mol) of cyanuric chloride into a 500mL four-neck flask, and stir at a uniform speed for 30 minutes; dissolve 22.3g (0.1mol) of 3-aminopropyltriethoxysilane In 10mL acetone, 0.076g (0.0001mol) 2,4-bis-[N-n-butyl-N-(1-cyclohexyloxy-2,2,6,6-tetramethyl-4-piperidinyl )amino]-6-(2-hydroxyethylamino)-1,3,5-triazine was dissolved in 10mL of acetone, and the two solutions were slowly added to the flask within 1h, and at the same time, 20mL of 5mol / L Sodium hydroxide aqueous solution, continue to react for 3 hours after dripping; then raise the temperature to 45°C, dissolve 3.1g (0.05mol) ethylenediamine and 4.0g (0.1mol) sodium hydroxide in 20mL deionized water to form a mixed solution, Slowly drop it into the flask within 1 hour, and then continue to react for 3 hours; after the reaction, filter the solution, wash the filter cake with dei...

Embodiment 2

[0051] (1) Preparation of macromolecule char-forming agent containing hindered amine structure

[0052] At 25°C, add 250mL of acetone and 18.8g (0.1mol) of cyanuric chloride to a 500mL four-neck flask, and stir at a uniform speed for 40 minutes; 38.2g (0.2mol) of γ-aminopropylmethyldiethoxy Dissolve silane in 10mL acetone, 0.076g (0.0001mol) 2,4-bis-[N-n-butyl-N-(1-cyclohexyloxy-2,2,6,6-tetramethyl-4-piper Pyridyl)amino]-6-(2-hydroxyethylamino)-1,3,5-triazine was dissolved in 10mL of acetone, and the two solutions were slowly added to the flask within 1h, and at the same time, 40mL of 5mol / L of sodium hydroxide aqueous solution, continue to react for 3 hours after dripping; then raise the temperature to 65°C, dissolve 3.1g (0.05mol) of ethylenediamine and 4.0g (0.1mol) of sodium hydroxide in 20mL of deionized water, and make a mixture The solution is slowly dropped into the flask within 1 hour, and the reaction is continued for 3 hours after the drop is completed; after the ...

Embodiment 3

[0058] (1) Preparation of macromolecule char-forming agent containing hindered amine structure

[0059] At 25°C, add 250mL of acetone and 18.8g (0.1mol) of cyanuric chloride into a 500mL four-neck flask, stir at a constant speed for 30min; dissolve 22.3g (0.1mol) of 3-aminopropyltriethoxysilane In 10mL acetone, 1.52g (0.002mol) 2,4-bis-[N-n-butyl-N-(1-cyclohexyloxy-2,2,6,6-tetramethyl-4-piperidinyl )amino]-6-(2-hydroxyethylamino)-1,3,5-triazine was dissolved in 10mL of acetone, and the two solutions were slowly added to the flask within 1h, and at the same time, 20mL of 5mol / L Sodium hydroxide aqueous solution, continue to react for 1h after dripping; then raise the temperature to 65°C, dissolve 3.1g (0.05mol) ethylenediamine and 4.0g (0.1mol) sodium hydroxide in 20mL deionized water to form a mixed solution, Slowly drop it into the flask within 1 hour, and then continue to react for 1 hour; after the reaction, filter the solution, wash the filter cake with deionized water an...

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Abstract

The invention discloses a single-component intumescent flame retardant with free radical quenching function, a preparation method and applications thereof. The preparation method comprises: carrying out a reaction by using cyanuric chloride, alkoxy silane, a hindered amine monomer and a diamine monomer as raw materials sequentially at 0-25 DEG C and 45-65 DEG C to obtain an intermediate product; and carrying out ion exchange and nucleophilic substitution reaction on the intermediate product, a nitrogen-phosphorus flame retardant and a diamine monomer at 80-120 DEG C to prepare the single-component intumescent flame retardant with free radical quenching function, wherein the single-component intumescent flame retardant is used in polypropylene fire retardation. Compared with the flame retardant in the prior art, the single-component intumescent flame retardant of the invention has the easily controlled phosphorus-nitrogen ration, easily achieves the efficient coupling of free radical quenching and intumescent charring, has high flame-retardant efficiency, can achieve efficient flame-retardant effect only at a small adding amount, further has outstanding water resistance, and is widely applied to the fields of electronic and electrical appliances, architectural decoration, automobile parts and the like.

Description

technical field [0001] The invention relates to the field of preparation and application of a polymer halogen-free flame retardant, in particular to a one-component intumescent flame retardant with free radical quenching function and its preparation method and application. Background technique [0002] Polypropylene (PP) is prone to cracking at high temperature to produce R and H, or is oxidized to produce RO and HO. Combustible gases such as ketones and aldehydes, when mixed with oxygen, will burn violently and release a lot of heat when they encounter an open flame, which will further aggravate the degradation and combustion of PP. [0003] Hindered amines have excellent free radical scavenging functions, and are often used as light stabilizers in polyolefin films and polymer coatings. In recent years, it has been found that they can also play a good role in flame retardancy in polymers. Using 2,2,6,6-tetramethylpiperidinamine and phenylphosphonic dichloride as raw materi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/06C08L23/12C08L79/04C08K3/32
CPCC08G73/0638C08G73/065C08K2003/323C08L23/12C08L2201/02C08L79/04C08K3/32
Inventor 赖学军曾运生李佳欣曾幸荣李红强江昌乘陈宇轩
Owner SOUTH CHINA UNIV OF TECH
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