Phosphorous and nitrogenous UV-cured flame retardant and preparation method thereof

A phosphite and flame retardant technology, which is applied in the field of UV-curable nitrogen-phosphorus flame retardants and their preparation, can solve the problems of low flame retardant efficiency, complicated preparation steps, etc., and achieves high production efficiency and curbs Effect of flame retardant migration and high flame retardancy

Inactive Publication Date: 2013-12-11
合肥安聚达新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above-mentioned flame retardant adopts the currently relatively environmentally friendly halogen-free flame retardant method, and introduces flame retardant elements such as phosphorus to perform flame retardant, the preparation steps are complicated and the flame retardant efficiency is not high.

Method used

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  • Phosphorous and nitrogenous UV-cured flame retardant and preparation method thereof
  • Phosphorous and nitrogenous UV-cured flame retardant and preparation method thereof
  • Phosphorous and nitrogenous UV-cured flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] In a 500ml three-neck flask equipped with mechanical stirring and a constant pressure dropping funnel, add 0.3mol (24.3g) of 37%-40% formaldehyde aqueous solution; after stirring at 40°C for 1 hour, slowly drop 0.3mol (31.5g) of Diethanolamine, heat preservation reaction for 2 hours; the reaction solution was distilled under reduced pressure at 0.094MPa to obtain the intermediate; after the intermediate temperature was raised to 60°C, 0.3mol (41.4g) diethyl phosphite was added dropwise, and the heat preservation reaction was carried out for 3 hours. A yellow transparent liquid was obtained. Then take 10.21g (0.04mol) of the yellow liquid and 125ml of chloroform into a 250ml three-necked flask, control the temperature at -5-10°C, add 12.14g (0.12mol) of triethylamine and stir for 1 hour, then add 10.86g (0.12mol) of acryloyl chloride, after 4 hours of reaction, the temperature was raised to room temperature (25°C), and the reaction was continued for 12 hours; Washed wit...

Embodiment 2

[0036] In a 500ml three-neck flask equipped with mechanical stirring and a constant pressure dropping funnel, add 0.3mol (24.3g) of 37%-40% formaldehyde aqueous solution; after stirring for 1 hour at 40°C, slowly drop 0.3mol (39.9g) of Diisopropanolamine, heat preservation reaction for 2 hours; the reaction solution was distilled under reduced pressure at 0.094MPa to obtain the intermediate; after the intermediate temperature was raised to 60°C, 0.3mol (41.4g) diethyl phosphite was added dropwise, and the heat preservation reaction After 3 hours, a yellow transparent liquid was obtained. Then take 11.3g (0.04mol) of the yellow liquid and 125ml of chloroform into a 250ml three-necked flask, control the temperature at -5-10°C, add 12.14g (0.12mol) of triethylamine and stir for 1 hour, then add 10.86g (0.12mol) of acryloyl chloride, after 4 hours of reaction, the temperature was raised to room temperature (25°C), and the reaction was continued for 12 hours; Washed with salt wate...

Embodiment 3

[0040] In a 500ml three-neck flask equipped with mechanical stirring and a constant pressure dropping funnel, add 0.3mol (35.7g) of 37%-40% acetaldehyde aqueous solution; after stirring at 40°C for 1 hour, slowly drop in 0.3mol (39.9g) Melted 3,3'-dihydroxydiphenylamine, heat preservation reaction for 2 hours; the reaction solution was distilled under reduced pressure at 0.094MPa to obtain the intermediate; after the intermediate was heated to 60°C, 0.3mol (41.4g) of diphosphite was added dropwise Ethyl ester was incubated for 3 hours to obtain a yellow transparent liquid. Then take 14.0g (0.04mol) of the yellow liquid and 125ml of chloroform into a 250ml three-necked flask, control the temperature at -5-10°C, add 12.14g (0.12mol) of triethylamine and stir for 1 hour, then add 10.86g (0.12mol) of acryloyl chloride, after 4 hours of reaction, the temperature was raised to room temperature (25°C), and the reaction was continued for 12 hours; Washed with salt water, and dried wi...

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PUM

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Abstract

The invention discloses a phosphorous and nitrogenous UV-cured flame retardant and a preparation method thereof. According to the invention, phosphorus and nitrogen compound precursor with high phosphorus content is synthesized by using raw materials of alcamines compound, aldehydes compound, and dialkyl phosphite through Kabachnik-Fields reaction; a light-cured monomer containing phosphorus and nitrogen elements is prepared through substitution/esterification reaction of the precursor with (methyl) acryloyl chloride or (methyl) propenoic acid by utilizing active hydroxy of the precursor; the monomer is used as reaction type flame retardant to be applied to light-cured resin matrix, and can curve rapidly with matrix under UV lighting to form a flame-retarded light-cured material which not only has good flame retardant property, but also can reduce the transfer and loss of the flame retardant in the using process. Compared with a conventional additive flame retardant, the compatibility of the flame retardant and the macromolecule matrix is also increased, and the duration of the flame retardant property of the material can be guaranteed.

Description

technical field [0001] The invention belongs to the technical field of flame retardant design and preparation, and in particular relates to an ultraviolet light-curable nitrogen-containing phosphorus flame retardant and a preparation method thereof; when applied to a light-curable resin matrix, it has a good flame-retardant effect on materials. Background technique [0002] Ultraviolet (UV) curing resin has been widely used in chemical industry, machinery, electronics, light industry, communication and other fields in recent years because of its advantages of low energy consumption, less pollution, fast curing rate, low cost and high chemical stability. Especially in terms of coatings and adhesives, UV curable resins are gradually replacing traditional thermosetting resins, and the market prospect is great. However, like many polymer resins, UV curable resins are also derived from petrochemicals and contain a large amount of carbon and hydrogen elements, so they are highly f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/40C08F283/10C08F230/02
Inventor 江赛华时虎
Owner 合肥安聚达新材料科技有限公司
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