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Ultraviolet light-cured phosphorus-nitrogen-containing halogen-free flame retardant and preparation method thereof

A technology of ultraviolet light and flame retardants, applied in the field of flame retardants, can solve the problems of low flame retardant efficiency and complicated preparation steps, and achieve the effects of high production efficiency, good fire protection and good compatibility

Active Publication Date: 2012-05-23
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But its disadvantage is that the flame retardant efficiency is not high, and the preparation steps are complicated

Method used

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  • Ultraviolet light-cured phosphorus-nitrogen-containing halogen-free flame retardant and preparation method thereof
  • Ultraviolet light-cured phosphorus-nitrogen-containing halogen-free flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 1. Preparation of UV-curable phosphorus-nitrogen-containing halogen-free flame retardant

[0021] In a 250ml three-neck flask equipped with mechanical stirring and a constant pressure dropping funnel, add 21.1g (0.1mol) phenyl phosphate dichloride and 80ml tetrahydrofuran, stir in an ice bath, and after 10 minutes, add 21.2g (0.21mol) Triethylamine, and a mixed solution of 11.6 g (0.1 mol) of hydroxyethyl acrylate and 20 ml of tetrahydrofuran was slowly added dropwise within 2 hours under continuous stirring, and the reaction was continued for 4 hours. Then 4.307 g (0.05 mol) of piperazine was dissolved in 80 ml of tetrahydrofuran, and slowly dropped into the above reaction system under constant stirring, and reacted for 8 hours. Suction filtration under reduced pressure to remove the triethylamine salt, and distillation under reduced pressure to remove the solvent, and the obtained brown-yellow viscous transparent liquid is the product of the present invention. The yi...

Embodiment 2

[0030] In a 250ml three-necked flask equipped with mechanical stirring and a constant pressure dropping funnel, add 21.1g (0.1mol) phenyl phosphate dichloride and 80ml methylene chloride, stir in an ice bath, and after 10 minutes, add 21.2g (0.21 mol) triethylamine, then slowly dropwise added a mixed solution of 11.6 g (0.1 mol) of hydroxyethyl acrylate and 20 ml of dichloromethane in 2 hours under continuous stirring, and continued to react for 4 hours. Then 4.307 g (0.05 mol) of piperazine was dissolved in 60 ml of dichloromethane, and slowly dropped into the above reaction system under constant stirring, and reacted for 8 hours. Suction filtration under reduced pressure to remove the triethylamine salt, distillation under reduced pressure to remove the solvent, and the viscous transparent liquid obtained is the product of the present invention. The yield was 88%.

[0031] The obtained product was analyzed by nuclear magnetic resonance spectrum. The peak position of the che...

Embodiment 3

[0034] In a 250ml three-neck flask equipped with mechanical stirring and a constant pressure dropping funnel, add 21.1g (0.1mol) phenyl phosphate dichloride and 80ml tetrahydrofuran, stir in an ice bath, and after 10 minutes, add 21.2g (0.21mol) Triethylamine, and a mixed solution of 11.6 g (0.1 mol) of hydroxyethyl acrylate and 20 ml of tetrahydrofuran was slowly added dropwise within 2 hours under continuous stirring, and the reaction was continued for 4 hours. Then, 5.407 g (0.05 mol) of m-phenylenediamine was dissolved in 80 ml of tetrahydrofuran, and slowly dropped into the above reaction system under constant stirring, and reacted for 8 hours. Suction filtration under reduced pressure to remove the pyridinium salt, and distillation under reduced pressure to remove the solvent, and the obtained brown viscous transparent liquid is the product of the present invention. The yield was 85%.

[0035] The obtained product was analyzed by nuclear magnetic resonance spectrum. The...

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Abstract

The invention discloses an ultraviolet light-cured phosphorus-nitrogen-containing halogen-free flame retardant and a preparation method thereof. The preparation method is characterized in that: phenyl dichlorophosphate serving as a reaction matrix is reacted with polyalcohol or polyphenol partially acidified by acrylicacid or methacrylic acid; the product of the reaction is reacted with a nitrogen-containing compound with two reactive amino groups to form a yellow, sticky, transparent, liquid and phosphorus-nitrogen-containing substance which is ultraviolet light-cured monomer of which the molecule has an active double bound and phosphorus-nitrogen flame retardant elements; and the ultraviolet light-cured monomer serving as a reactive flame retardant is added into an ultraviolet light-cured resin substrate to form a transparent coating with high flame retarding efficiency through quick curing in ultraviolet light. The ultraviolet light-cured flame-retardant coating generates 34.0 percent of residue under an air condition at 60 DEG C, and 26.3 percent under a nitrogen condition. The maximum release rate of the ultraviolet light-cured flame-retardant coating is 146.6 W / g. The ultraviolet light-cured halogen-free phosphorus-nitrogen-containing flame retardant can be used for inflaming retarding in wood, textile, plastics, metal or circuit boards.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and in particular relates to an ultraviolet-curable phosphorus-nitrogen-containing halogen-free flame retardant and a preparation method thereof. Background technique [0002] Resins cured by ultraviolet light crosslinking have been more and more widely used in the coating industry, graphic arts industry and microelectronics industry, etc., and it has gradually replaced traditional thermally induced polymerization coatings and adhesives. But similar to conventional synthetic resins, the major drawback of existing UV-curable resins is their flammability. The existing conventional flame retardants are generally low-molecular-weight organic or inorganic additives, which are usually added in a large amount and need to be blended with the base material during construction. Due to their poor compatibility with macromolecules, the blending effect Not ideal; blending not only brings a lot of la...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6509C07F9/24C09K21/12C09D4/02C09D5/18
Inventor 胡源陈丽娟宋磊台启龙邢伟义
Owner UNIV OF SCI & TECH OF CHINA
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