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Reaction type phosphorus-nitrogen fire retardant and synthesizing method thereof

A reactive flame retardant, phosphorus nitrogen flame retardant technology, applied in chemical instruments and methods, adhesive additives, non-polymer adhesive additives, etc., can solve poor dispersion, easy water absorption, and poor persistence of flame retardant effect and other problems, to achieve the effects of long-lasting flame retardant efficiency, simple preparation process, and little impact on performance

Inactive Publication Date: 2012-10-31
GUANGDONG JUSHI CHEM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the disadvantages of the commonly used phosphorus-nitrogen added flame retardants such as poor dispersion, easy water absorption, easy migration and precipitation, poor persistence of flame retardant effect, and great influence on the mechanical properties of polymer matrix materials. In order to solve the problems of cumbersome synthesis process of phosphorus-nitrogen reactive flame retardants and other problems, a reactive phosphorus-nitrogen flame retardant and its synthesis method with simple synthesis method and easy post-treatment are provided.

Method used

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  • Reaction type phosphorus-nitrogen fire retardant and synthesizing method thereof
  • Reaction type phosphorus-nitrogen fire retardant and synthesizing method thereof
  • Reaction type phosphorus-nitrogen fire retardant and synthesizing method thereof

Examples

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Effect test

Embodiment 1

[0024] 6.01g (0.1mol) ethylenediamine, 15.2g (0.15mol) triethylamine and 80mL tetrahydrofuran were added to a 250mL four-necked flask and placed in an oil bath. Dry nitrogen was introduced at room temperature and the rate was 300 rpm. Stir continuously for 20 minutes at a rotation speed of 2 minutes; 22g (0.1mol) of diphenylphosphorus chloride was dissolved in 20mL of tetrahydrofuran, and then slowly dropped into the four-necked flask with a constant pressure dropping funnel. The dropping time was 2 hours. After the dropwise addition of phenylphosphonium chloride was completed, the temperature of the oil bath was increased to 75°C, and the reaction was continued with nitrogen for 6 hours. The obtained reaction product was filtered to obtain a filter cake, which was washed three times with deionized water, filtered, and filtered. The solid was dried at 120° C. for 5 hours and then ground and crushed to obtain 23.1 g of white product with a yield of 95%. The purity of the product ...

Embodiment 2

[0028] In a 500mL four-necked flask equipped with mechanical stirring and reflux condenser, 21.6g (0.2mol) o-phenylenediamine and 16.8g (0.3mol) potassium hydroxide were dissolved in 100mL petroleum ether, and nitrogen was introduced at room temperature. And continue to stir at 400 rpm for 30 minutes; 19.49g (0.1mol) phenylphosphoryl dichloride was dissolved in 50mL petroleum ether, and then slowly dropped into the four-necked flask with a constant pressure dropping funnel. The addition time is 2 hours. After the dropwise addition of phenylphosphoryl dichloride is completed, the temperature of the oil bath is increased to 65°C, and the reaction is continued with nitrogen for 7 hours. The obtained reaction product is filtered to obtain a filter cake, and the filter cake uses deionized water Wash three times, filter, dissolve the filtered solid in 50mL of DMF, filter, add a large amount of deionized water to the obtained filtrate, filter the precipitated solid, dry at 120°C for 5 ...

Embodiment 3

[0030] In a 500mL four-necked flask equipped with mechanical stirring and reflux condenser, 21.6g (0.2mol) m-phenylenediamine, 23.7g under normal temperature, stirring speed of 400 rpm and dry nitrogen (0.3mol) pyridine was dissolved in 100mL of toluene, 15.3g (0.1mol) of phosphorus oxychloride was dissolved in 30mL of toluene, and then slowly dripped into the four-necked flask with a constant pressure dropping funnel, the dripping time was 1.5 hours After the dropwise addition of phosphorus oxychloride is completed, the temperature of the oil bath is increased to 90°C, and the nitrogen gas is continued to react for 6 hours. The resulting reaction product is filtered to obtain a precipitate. The precipitated material is washed with deionized water, filtered, and filtered to obtain The solid was dried at 120°C for 5 hours to obtain 24.3 g of the final white solid product, the yield was about 94%, and the product purity was 99.5%. Infrared spectrum characterization: 3284cm -1 And...

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Abstract

The invention discloses a reaction type phosphorus-nitrogen fire retardant and a synthesizing method of the reaction type phosphorus-nitrogen fire retardant. The synthesizing method comprises the following steps: adding a diamido compound into a reaction container containing solvents, adding an acid-binding agent, then adding phosphorus chlorine compound or phosphorus oxychloride compound, stirring uniformly, adjusting the temperature to 50 DEG C-90 DEG C, and reacting for 5-15h at constant temperature; filtering, washing a filter cake with water repeatedly and filtering or dissolving the filter cake with a strong-polarity solvent, and drying to obtain the reaction type phosphorus-nitrogen fire retardant. According to the reaction type phosphorus-nitrogen fire retardant and the synthesizing method of the fire retardant, the synthesizing method is simple, is free of complicated aftertreatment and is easy to implement; and the reaction type phosphorus-nitrogen fire retardant is high in thermal stability, active amido functional groups contained in molecules of the fire retardant have chemical bonding with polymer or polymer raw materials, so that the reaction type phosphorus-nitrogen fiber retardant can be mixed with substrate materials, and can be applied to polymers with various substrate materials.

Description

Technical field [0001] The invention relates to a reactive flame retardant, in particular to a reactive phosphorus-nitrogen flame retardant and a synthesis method thereof. The flame retardant can be applied to the needs of coatings, adhesives, plastics, rubber, electronic products, etc. Flame retardant field. Background technique [0002] Commonly used polymer materials generally have a low oxygen index and are flammable materials. However, polymer materials are inseparable in people's daily life. Therefore, once a fire occurs, polymer materials will have the danger of supporting combustion. How to reduce the combustion performance of polymer materials has become a technical and social issue of increasing concern. In recent years, frequent fires caused by flammable polymer materials have brought great threats to people's lives and property safety. At present, various countries in the world have put forward high standards for the flame retardant requirements of polymer materials...

Claims

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Application Information

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IPC IPC(8): C08K5/5399C07F9/46C07F9/36C09D7/12C09J11/06
Inventor 李玲玉何燕岭陈勇军刘岚贾志欣贾德民李斌
Owner GUANGDONG JUSHI CHEM CO LTD
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