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Synthesis and application of nitrogen-phosphorus series efficient flame retardant containing benzimidazole structure

A benzimidazole and aminobenzimidazole technology, applied in the field of flame retardants, can solve the problems of affecting the mechanical properties of the substrate, easy migration of volatility, poor compatibility, etc. High flame retardant efficiency

Inactive Publication Date: 2020-01-31
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Inorganic flame retardants are added in a large amount due to their poor compatibility with organic polymer materials, which affects the mechanical properties of the substrate; halogenated flame retardants release toxic gas hydrogen halide when burned, which is harmful to the environment and human body. Cause secondary hazards; phosphorus-based flame retardants have the advantages of non-toxic, halogen-free, and good compatibility with polymer materials, and are substitutes for halogen-based flame retardants, but most single-component phosphorus-based flame retardants are liquids. There are some problems such as volatility and easy migration

Method used

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  • Synthesis and application of nitrogen-phosphorus series efficient flame retardant containing benzimidazole structure
  • Synthesis and application of nitrogen-phosphorus series efficient flame retardant containing benzimidazole structure
  • Synthesis and application of nitrogen-phosphorus series efficient flame retardant containing benzimidazole structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A kind of synthesis of nitrogen-phosphorus high-efficiency flame retardant containing benzimidazole structure, comprising the following steps:

[0029] (1) Add 2-aminobenzimidazole and m-nitrobenzaldehyde to a tube equipped with a reflux condenser and magnetic stirring

[0030] Then use a graduated cylinder to measure a certain amount of absolute ethanol, add it to a straight-mouthed three-necked flask to obtain a mixed solution 1, feed nitrogen, turn on the microwave reactor and magnetic stirring, and continue stirring under the microwave-assisted condition. The power is 250W, the Schiff base reaction is carried out, the reaction temperature is 65°C, and the reaction time is 40min;

[0031] (2) When there is an orange precipitate in the mixed solution 1, filter the mixed solution 1 and wash it with absolute ethanol

[0032] Washing the precipitate, drying the precipitate at 60° C. under vacuum for 6 hours to obtain an intermediate product, the structural formula of th...

Embodiment 2

[0040] An application based on the nitrogen-phosphorus high-efficiency flame retardant containing benzimidazole structure prepared in this example 1, comprising the following steps: after stirring 70 parts of epoxy resin in vacuum at 80 °C in parts by weight, Raise the temperature to 120°C, add 0.8 parts of flame retardant; after vacuum stirring evenly, cool to 90°C, add 1.5 parts of curing agent, pour into the mold, and cure at 100°C and 150°C for 2 hours, after curing, the ring Cured epoxy resin.

Embodiment 3

[0042] A kind of synthesis of nitrogen-phosphorus high-efficiency flame retardant containing benzimidazole structure, comprising the following steps:

[0043] (1) Add 2-aminobenzimidazole and m-nitrobenzaldehyde to a tube equipped with a reflux condenser and magnetic stirring

[0044] Then use a graduated cylinder to measure a certain amount of absolute ethanol, add it to a straight-mouthed three-necked flask to obtain a mixed solution 1, feed nitrogen, turn on the microwave reactor and magnetic stirring, and continue stirring under the microwave-assisted condition. The power is 300W, the Schiff base reaction is carried out, the reaction temperature is 60°C, and the reaction time is 35min;

[0045] (2) When there is an orange precipitate in the mixed solution 1, filter the mixed solution 1 and wash it with absolute ethanol

[0046] Wash the precipitate, and dry the precipitate at 60° C. under vacuum for 6 hours to obtain an intermediate product;

[0047] (3) Put the intermed...

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Abstract

The invention provides synthesis and an application of a nitrogen-phosphorus series efficient flame retardant containing a benzimidazole structure, relates to the technical field of flame retardants,and in particular, relates to synthesis of the nitrogen-phosphorus series efficient flame retardant containing the benzimidazole structure, wherein the synthesis comprises the following steps: (1) adding 2-aminobenzimidazole and m-nitrobenzaldehyde into a solvent to obtain a mixed solution I, introducing nitrogen, and continuously stirring under a microwave-assisted condition, and carrying out a Schiff base reaction; (2) when a precipitate is separated out, filtering the mixed solution I to obtain the precipitate, and drying the precipitate to obtain an intermediate product; and (3) putting the intermediate product and 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide in a solvent, dissolving to obtain a mixed solution II, carrying out an addition reaction, and drying to obtain the flameretardant. After the flame retardant is added, the phosphorus content is 0.13-0.52 wt%, the addition amount of the flame retardant is small, and the oxygen index of an epoxy resin cured product can beincreased to 34.5%. With the introduction of the benzimidazole structure, the curing capacity of the resin is enhanced, the addition amount of the flame retardant is small, and the flame retardant effect is good.

Description

technical field [0001] The invention relates to the technical field of flame retardants, in particular to the synthesis and application of a nitrogen-phosphorus high-efficiency flame retardant containing a benzimidazole structure. Background technique [0002] Most polymer materials are flammable, which makes them a great safety hazard during use, which may cause huge losses of life and property. Therefore, flame retardancy of polymer materials and improvement of their flame retardancy have become an urgent problem to be solved. Epoxy resin (EP) is widely used in electronic appliances, national defense and daily life because of its excellent electrical insulation, high mechanical properties, high thermal stability, excellent bonding performance, small curing shrinkage, and good stability. Many fields. However, the limiting oxygen index (LOI) of most epoxy resins is lower than 22%. The fire hazard characteristics of flammability in air and heated molten dripping limit the a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08K5/3475C08L63/00
CPCC07F9/657172C08K5/3475C08L63/00
Inventor 周红王俊杰潘志权
Owner WUHAN INSTITUTE OF TECHNOLOGY
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