Fire retardant containing styrene structure and phosphorus and nitrogen elements and synthetic method thereof

A synthesis method and styrene technology, applied in the field of flame retardants, can solve problems such as affecting the compatibility of flame retardant monomers, deteriorating material physical properties, deteriorating material mechanics and impact resistance physical properties, etc., and achieving excellent flame retardant properties. The effect of performance, novel molecular structure, and easy industrial production

Inactive Publication Date: 2014-01-29
JIANGSU YOKE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that since the flame retardant is added in the form of physical blending, it will often deteriorate the physical properties of the material, such as mechanics and impact resistance.
The disadvantage is that most of the produced products have certain water solubility, which not only affects the compatibility of the flame retardant monomer and the flame retardant substrate, but also easily dissolves the flame retardant in the cooling water during the extrusion process, which greatly deteriorates the material. physical properties

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Embodiment 1, in the flask equipped with stirring, condensation, drying device, add sodium hydroxide 0.17g and pyridine 0.48g successively, carbon tetrachloride 7.48g, 4-amino styrene 0.37g, open stirring device, ice Cool the salt bath to 0°C, slowly add a mixture of 0.64 g of dibutyl phosphite and 4.40 g of carbon tetrachloride dropwise from the dropping funnel, and drop it in about 2 hours. Keep the reaction at 0°C for 37 hours to complete the reaction, filter off the generated solid, spin off the reaction solvent, and separate the product by column chromatography (ethyl acetate:petroleum ether=5:2) to obtain a sample of 0.92g. The yield is 97.8%.

Embodiment 2

[0020] Embodiment 2, in the flask equipped with condensation, stirring, drying device, add potassium carbonate 0.70g and triethanolamine 0.76g successively, carbon tetrachloride 8.28g, 4-aminostyrene 0.61g, open stirring device, ice Cool the salt bath to 4°C, slowly add a mixture of 1.38g of dihexyl phosphite and 3.67g of carbon tetrachloride dropwise from the dropping funnel, and drop it in about 2 hours. Keep the reaction at 4-9°C for 40 hours to complete the reaction, filter off the formed solid, spin off the reaction solvent, and separate the product by column chromatography (ethyl acetate:petroleum ether=3:1) to obtain a sample of 1.79g. Yield 96.2%.

Embodiment 3

[0021] Example 3, in a flask equipped with a stirring, drying, and condensing device, sequentially add 0.50 g of sodium benzoate, 0.66 g of aniline, 6.25 g of carbon tetrachloride, and 0.43 g of 4-aminostyrene, start the stirring device, and add ice-water The bath was cooled to 0°C, and the mixture of 0.50 g of diethyl phosphite and 4.51 g of carbon tetrachloride was slowly added dropwise from the dropping funnel, and the drop was completed in about 2.5 hours. Keep the reaction at 0-5°C for 40 hours to complete the reaction, filter off the formed solid, spin off the reaction solvent, and separate the product by column chromatography (ethyl acetate:petroleum ether=3:1) to obtain a sample of 0.88g. The yield is 95.1%.

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PUM

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Abstract

The invention discloses a fire retardant containing a styrene structure and phosphorus and nitrogen elements. The fire retardant is obtained by reacting dialkyl phosphite with 4-aminostyrene and carbon tetrachloride in the presence of a catalyst, wherein the catalyst is a compound of an organic base and an inorganic base; the organic base catalyst is pyridine, triethylamine, diethylamine, triethanolamine, diethanolamine, aniline, tetrabutyl ammonium hydroxide or tetraethyl ammonium hydroxide, while the inorganic base catalyst is sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate, sodium bicarbonate, potassium bicarbonate, sodium benzoate or potassium benzoate; the mol ratio of the organic base to 4-aminostyrene is (3-1): 1 and the mol ratio of the inorganic base to 4-aminostyrene is (1.1-1): 1. Due to the existence of the styrene structure in the molecule, the fire retardant monomer is easy to have a polymerization reaction with active double bonds such as styrene and ethylene; in the meantime, due to the existence of phosphorus and nitrogen fire-retarding elements, the material is provided with fire resistance; carbon tetrachloride is used as a solvent in the synthesis process, so that the reaction is convenient to operate and high in yield; industrial production of the fire retardant is easy to realize.

Description

technical field [0001] The invention relates to a flame retardant, in particular to a flame retardant containing styrene structure and phosphorus and nitrogen elements and a synthesis method thereof. technical background [0002] With the increasing application of polymer materials, the fire safety of materials is gradually attracting people's attention. The traditional fire retardant treatment is to add a certain amount of flame retardant during the polymer blending process to achieve the purpose of material flame retardant. This method is simple to operate and convenient to produce. The disadvantage is that because the flame retardant is added in the form of physical blending, it often deteriorates the mechanical properties and impact resistance of the material and other physical properties. [0003] In recent years, the research on bulk copolymerized flame retardant materials has been increasing. The method is to use the activity of the flame retardant monomer itself to...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/24C08F212/08C08F210/02C08F230/02
Inventor 沈琦杨建伟陈俊蔡伦
Owner JIANGSU YOKE TECH
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