Preparation method of high-efficiency flame retardant containing DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) and aminopyrazine structures and application of flame retardant

An aminopyrazine and flame retardant technology, applied in the field of flame retardants, can solve the problems of large amount of flame retardants, toxic gas emission, personal safety threats, etc., and achieves high flame retardant efficiency, delayed combustion, and simple reaction method. Effect

Active Publication Date: 2019-07-23
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the secondary damage such as smoke and toxic gas emissions when traditional halogen-based flame retardants are burned, they pose a seriou...

Method used

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  • Preparation method of high-efficiency flame retardant containing DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) and aminopyrazine structures and application of flame retardant
  • Preparation method of high-efficiency flame retardant containing DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) and aminopyrazine structures and application of flame retardant
  • Preparation method of high-efficiency flame retardant containing DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) and aminopyrazine structures and application of flame retardant

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Embodiment 1

[0023] The invention is a preparation method of a high-efficiency flame retardant containing DOPO and an aminopyrazine structure, comprising the following steps;

[0024] (1) Add 54mmol of aminopyrazine, 30mmol of terephthalaldehyde, and an appropriate amount of solvent into a 500mL three-neck flask equipped with a condensing reflux tube, magnetic stirring, and heating device. Dissolving, the Schiff base reaction is carried out at about 65°C, and the reaction equation is shown in the formula;

[0025]

[0026] (2) Add 60mmol of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to make 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10- Addition reaction between oxide and Schiff base at 60°C produces flame retardant DTPA containing aminopyrazine structure, the reaction equation is shown in the following formula, cool to room temperature, and then filter to obtain a white solid, which is used to remove Washed two to three times with deionized water, then washed twice with ethanol...

Embodiment 2

[0032] The invention is a preparation method of a high-efficiency flame retardant containing DOPO and an aminopyrazine structure, comprising the following steps;

[0033] (1) Add 66mmol of aminopyrazine, 30mmol of terephthalaldehyde, and an appropriate amount of solvent into a 500mL three-necked flask equipped with a condensing reflux tube, magnetic stirring, and heating device. The solvent can be ethanol, and the temperature is raised to 65°C. Dissolving, the Schiff base reaction is carried out at about 65°C, and the reaction equation is shown in the formula;

[0034]

[0035] (2) Add 69mmol of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to make 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10- Addition reaction between oxide and Schiff base occurs at 68°C to generate flame retardant DTPA containing aminopyrazine structure. Washed two to three times with deionized water, then washed twice with ethanol, and dried in a vacuum oven at 60° C. for 14 hours to obtain a pure ...

Embodiment 3

[0039] The invention is a preparation method of a high-efficiency flame retardant containing DOPO and an aminopyrazine structure, comprising the following steps;

[0040] (1) Add 60mmol of aminopyrazine, 30mmol of terephthalaldehyde, and an appropriate amount of solvent into a 500mL three-neck flask equipped with a condensing reflux tube, magnetic stirring, and heating device. Dissolving, the Schiff base reaction is carried out at about 65°C, and the reaction equation is shown in the formula;

[0041]

[0042] (2) Add 60mmol of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to make 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10- Addition reaction between oxide and Schiff base occurs at 65°C to generate flame retardant DTPA containing aminopyrazine structure. The reaction equation is shown in the following formula. Cool to room temperature, and then obtain a white solid by suction filtration. Use the obtained white solid to remove Washed two to three times with deionized ...

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Abstract

The invention provides a preparation method of a high-efficiency flame retardant containing DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) and aminopyrazine structures and application of the flame retardant and relates to the technical field of flame retardants. The preparation method of the high-efficiency flame retardant containing the DOPO and aminopyrazine structures comprises the following steps: (1) mixing aminopyrazine and p-phthalaldehyde in solvent, and carrying out a Schiff base reaction, wherein a reaction equation is shown in a formula of the description; (2) adding 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide to generate a addition reaction with Schiff base so as to generate the flame retardant DTPA (Diethylenetriamine pentaacetic acid) containing an aminopyrazine structure, wherein a reaction equation is shown in the following formula of the description. According to the aminopyrazine-type flame retardant prepared by the invention, the flame-retarding efficiency is higher, the phosphorus content is 0.09-0.34%, the flame-retarding property of materials is improved, the oxygen index of cured epoxy resin can be increased to 32.5%, the vertical burning can reach UL-94 V-0 grade, and the use amount of the flame retardant under the same flame-retarding effect is less.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to a preparation method and application of a high-efficiency flame retardant containing DOPO and aminopyrazine structures. Background technique [0002] Epoxy resin (EP) has become a widely used thermosetting polymer material because of its excellent electrical insulation, dimensional stability, high thermal stability, low shrinkage, strong adhesion and mechanical durability, etc., for Electronic appliances, automobiles, packaging, printed circuit boards, adhesives and surface coatings and other fields. However, its application in many fields is limited due to its flammability. Therefore, it is crucial to endow EP with good flame retardancy. [0003] A common way to improve the flame retardant properties of epoxy resins is to add flame retardants. Due to secondary damage such as smoke and toxic gas emissions when traditional halogen-based flame retardants are burned, the...

Claims

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Application Information

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IPC IPC(8): C07F9/6574C08K5/5313C08L63/00
CPCC07F9/657172C08K5/5313C08L2201/02C08L63/00
Inventor 周红汤浩潘志权程清蓉
Owner WUHAN INSTITUTE OF TECHNOLOGY
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