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Reaction type phosphorus/nitrogen flame retardant, and preparation method and application thereof

A phosphorus-nitrogen-based flame retardant and reactive technology, which is applied in the field of flame retardants and their preparation, can solve the problems of toxic smoke, environmental pollution, secondary hazards, etc., and achieves reduced usage, good flame retardant effect and low cost Effect

Active Publication Date: 2014-01-08
浙江通力新材料科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Halogenated flame retardants tend to produce toxic and corrosive gases and a lot of smoke during the combustion process, which can easily cause "secondary hazards" and pollute the environment during use

Method used

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  • Reaction type phosphorus/nitrogen flame retardant, and preparation method and application thereof
  • Reaction type phosphorus/nitrogen flame retardant, and preparation method and application thereof
  • Reaction type phosphorus/nitrogen flame retardant, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: Synthesis of N-ethyl-acrylamido-2-oxo-5,5-dimethyl-1,3,2-dioxaphosphorinane

[0033] Add 15.4g (0.1mol) of phosphorus oxychloride and 50mL of chloroform into a four-necked flask, stir the reaction temperature to 35°C, slowly add dropwise a mixture of 10.4g (0.1mol) of neopentyl glycol and 80mL of chloroform, After the addition, the reaction was maintained at 40°C for 3 hours, the chloroform was recovered by distillation under reduced pressure, washed with 25 mL of anhydrous ether, and filtered to obtain a colorless crystalline solid of 2-oxo-2-chloro-5,5-dimethyl -1,3,2-Dioxaphosphorinane, the yield is 86.1%, the purity is 97.1%, and the melting point is 109-110°C.

[0034] Add 9.0g (0.15mol) of ethylenediamine and 40mL of chloroform into the three-necked flask, stir, and the temperature of the reaction solution is 0°C, slowly add 18.4g (0.1mol) of the solid (2-oxo-2 -Chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane) and 100mL chloroform mixture, after the addit...

Embodiment 2

[0037] The synthesis operation of N-ethyl-acrylamido-2-oxo-5,5-dimethyl-1,3,2-dioxaphosphorinane is the same as in Example 1. In the reaction of the formula (II) compound and the formula (III) compound, the amount ratio of the feeding material of the formula (II) compound and the formula (III) compound is 1.0: 1.2, and the feeding material of the acid-binding agent pyridine and the formula (II) compound The molar ratio is 2.5:1.0, the solvent is acetonitrile, the reaction temperature is 30° C., the reaction time is 6 hours, and the yield is 55.4%.

Embodiment 3

[0039] The synthetic operation of 2-oxo-5,5-dimethyl-1,3,2-dioxaphosphorinane-ethylenediamine is the same as in Example 1, N-ethyl-acrylamido-2-oxo- The synthesis operation of 5,5-dimethyl-1,3,2-dioxaphosphorinane is the same as in Example 1. In the reaction of the formula (II) compound and the formula (III) compound, the amount ratio of the feeding material of the formula (II) compound and the formula (III) compound is 1.0: 1.5, the acid-binding agent sodium bicarbonate and the formula (II) compound The molar ratio of the feed materials is 3.0:1.0, the solvent is ethyl acetate, the reaction temperature is 50° C., the reaction time is 4 hours, and the yield is 37.4%.

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Abstract

The invention discloses a reaction type phosphorus / nitrogen flame retardant, and its preparation method and application. A structure of the reaction type phosphorus / nitrogen flame retardant is shown in the formula (I). The preparation method of the reaction type phosphorus / nitrogen flame retardant comprises the following steps that: a phosphaspiro-containing amine compound shown in the formula (II) and a carboxylic acid halide shown in the formula (III) undergo a reaction or the phosphaspiro-containing amine compound shown in the formula (II) and a carboxylic acid shown in the formula (IV) undergo a reaction to obtain the reaction type phosphorus / nitrogen flame retardant. In the invention, a copolymer is produced from a reaction type phosphorus / nitrogen flame retardant and monomers and is utilized for modifying high-molecular materials in a fire retardant characteristic, and through synergistic effects of nitrogen and phosphorus elements in the phosphorus / nitrogen flame retardant, flame retardant effects of high-molecular materials adopting the phosphorus / nitrogen flame retardant can be improved, thus a usage amount of the phosphorus / nitrogen flame retardant in the high-molecular materials is decreased and a cost of the high-molecular materials with a flame retardant characteristic is reduced.

Description

technical field [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to a reactive phosphorus-nitrogen series flame retardant and its preparation method and application, especially its application in the preparation of flame-retardant polymer materials. Background technique [0002] Halogenated flame retardants are prone to produce toxic and corrosive gases and a large amount of smoke during combustion, and are likely to cause "secondary hazards" and pollute the environment during use. With the improvement of human requirements for environmental protection and health and the introduction of restrictions and bans on the use of halogen flame retardants (2005 WEEE, 2006 RoHS, 2007 EuP and other directives), halogenated flame retardants are facing great challenges. Halogen-free flame retardants - organophosphorus nitrogen intumescent flame retardants are used in flame retardant polymers with the rise of flame retardant technology. Whe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/6571C08F212/08C08F220/10C08F218/08C08F220/56C08F220/44C08F230/02
Inventor 黄国波梁华定葛昌华
Owner 浙江通力新材料科技股份有限公司
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