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Reactive halogen-free flame retardant and preparation method thereof

A reactive, flame retardant technology, applied in the field of flame retardants, can solve the problems of material physical, mechanical and processing properties being greatly affected, and achieve the effect of easy operation and simple process

Inactive Publication Date: 2012-02-15
KAIFENG LONGYU CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the current reports are additive types. When applied to polymer materials, although they can play an effective flame retardant effect, they have a greater impact on the physical, mechanical and processing properties of the material.
However, the reactive flame retardant (monomer) integrating "three sources" has not been reported in the literature.

Method used

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  • Reactive halogen-free flame retardant and preparation method thereof
  • Reactive halogen-free flame retardant and preparation method thereof
  • Reactive halogen-free flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In a 250 mL three-necked flask equipped with stirring, reflux condenser and thermometer, 12.9 g (0.10 mol) of aminoethyl methacrylate, 12.0 g (0.12 mol) of triethylamine, 0.1 g of hydroquinone and 80 mL of tetrahydrofuran, stirred at room temperature for 0.5 h, then added 18.5 g (0.10 mol) of cyclic neopentyl glycol phosphoryl chloride and 0.7 g of 4-(N,N-dimethylamino)pyridine, adjusted the temperature to about 50 °C, The stirring reaction was continued for 4.5 h. The insoluble matter was removed by filtration under reduced pressure, the filtrate was distilled under reduced pressure and tetrahydrofuran was recovered, the sticky matter in the bottle was adjusted to neutrality with 5% dilute hydrochloric acid, washed with 2×50 mL water, and recrystallized with ethyl acetate / petroleum ether to obtain White to light red needle-like crystals, after drying, 22.3 g of the product was obtained, with a yield of 80.5%. The melting point of the product is 77.5-78.5°C, and its in...

Embodiment 2

[0033] In a 250 mL three-neck flask equipped with stirring, reflux condenser and thermometer, add 16.6 g (0.10 mol) of aminoethyl methacrylate hydrochloride, 19.0 g (0.24 mol) of pyridine, and 0.2 g of hydroquinone , 75 mL of ethyl acetate, stirred at room temperature for 0.5 h, then added 15.9 g (0.08 mol) of cyclic neopentyl glycol phosphorus oxychloride and 0.8 g of anhydrous magnesium chloride, adjusted the temperature to about 60 °C, and continued to stir for 10 h. Post-processing and structural characterization are the same as in Example 1. 21.5 g of the product was obtained, and the yield was 77.6%.

Embodiment 3

[0035] In a 250 mL three-necked flask equipped with stirring, reflux condenser and thermometer, add 11.5 g (0.10 mol) of aminoethyl acrylate, 11.0 g (0.11 mol) of triethylamine, 0.2 g of hydroquinone, and 50 mL of chloroform , stirred at room temperature for 0.5 h, then added 18.4 g (0.10 mol) of cyclic neopentyl glycol phosphorus oxychloride and 1.0 g of anhydrous magnesium chloride, adjusted the temperature to about 65 °C, and continued to stir for 15 h. After filtration, the filtrate was distilled and the solvent was recovered. The sticky matter in the bottle was fully washed with 2×50 mL of water, recrystallized with ethanol / water, and dried to obtain 20.6 g of the product, with a yield of 78.3%.

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PUM

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Abstract

The invention relates to a reactive halogen-free flame retardant and a preparation method thereof, belonging to the technical field of flame retardant. The reactive halogen-free flame retardant is represented by the following formula, wherein, R1 and R2 represent respectively independent H, C1-C6 alkyl or phenyl, R3 represents H,C1-C6 alkyl or phenyl, and R4 represents H or C1-C6 alkyl. The reactive halogen-free flame retardant is a flame retardant with a combination of the sour resource, the char resource and the gas resource of an intumescent flame retardant, and comprises polymerisable methacrylate groups. The preparation method has the advantages of simple process, safety, easy operation, and basic no pollution to the environment, and the yield can reach more than 80%. Hydrogen chloride gas generated in the reaction process after being absorbed by bind acid agent has no corrosion to the device. The prepared product is acicular crystals from white to light red, has synergistic effects resulting from nitrogen and phosphorus elements, and has the advantages of no halogen, low toxicity, no pollution and the like.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, in particular to a reactive halogen-free flame retardant and a preparation method thereof. Background technique [0002] The application of polymer materials in people's daily life is becoming more and more important, but the fires caused by their flammability not only cause huge economic losses and casualties, but also directly affect economic development and social stability. By adding flame retardants to polymer materials, the risk of fire caused by material combustion can be greatly reduced. [0003] According to the processing method, flame retardants can be divided into additive type and reactive type. Additive flame retardants currently occupy a dominant position in the flame retardant market. They have the advantages of low price and simple operation, but they have poor compatibility with polymer materials, and are prone to problems such as blooming and sweating, which makes the...

Claims

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Application Information

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IPC IPC(8): C08K5/5399C07F9/6574C08F20/36
Inventor 徐元清刘常进郭红丽高存生田一政赵利军余洋李武斌郭学群曹志奎
Owner KAIFENG LONGYU CHEM
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