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Polymer flame-retardant material containing pyrazole flame retardant and preparation method thereof

A technology of flame retardant materials and flame retardants, applied in the field of organic flame retardants, can solve problems such as harmful harmful gases, and achieve the effects of good compatibility, excellent thermal stability, and transparent comprehensive performance.

Inactive Publication Date: 2020-07-14
WEST ANHUI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Phosphorus-based flame retardants are currently considered to be a class of more efficient and environmentally friendly flame retardants, but most of the existing phosphorus-based flame retardants contain fluorine, which will produce extremely harmful harmful gases when burned

Method used

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  • Polymer flame-retardant material containing pyrazole flame retardant and preparation method thereof
  • Polymer flame-retardant material containing pyrazole flame retardant and preparation method thereof
  • Polymer flame-retardant material containing pyrazole flame retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] The polymer flame retardant material containing pyrazole flame retardant proposed by the present invention comprises the following raw materials in parts by weight: 20 parts of epoxy resin prepolymer, 1.5 parts of pyrazole flame retardant, 4,4'-diaminobis 5 parts of benzene methane.

[0032] The method steps of pyrazole flame retardant preparation are as follows:

[0033] S1: Add 5-amino-3-methyl-1-phenylpyrazole, p-benzaldehyde, and the first solvent to the reaction vessel in sequence, and stir at 30°C for 4 hours;

[0034] S2: Add DOPO to the reaction vessel of S1, and react at 30°C for 4 hours;

[0035] S3: Filter the solution after the reaction in S2, dissolve the filtered crude product in a second solvent to remove impurities in the crude product, and dry the solid product after filtration to obtain a pyrazole-rich flame retardant.

[0036] The molar volume ratio of 5-amino-3-methyl-1-phenylpyrazole, p-benzaldehyde, DOPO, and the first solvent is 1mol:0.1mol:0.1m...

Embodiment 2

[0043] The polymer flame retardant material containing pyrazole flame retardant proposed by the present invention includes the following raw materials in parts by weight: 30 parts of epoxy resin prepolymer, 1.8 parts of pyrazole flame retardant, 4,4'-diaminobis 8 parts of benzene methane.

[0044] The method steps of pyrazole flame retardant preparation are as follows:

[0045] S1: Add 5-amino-3-methyl-1-phenylpyrazole, p-benzaldehyde, and the first solvent to the reaction vessel in sequence, and stir at 180°C for 24 hours;

[0046] S2: Add DOPO to the reaction vessel of S1, and react at 180°C for 24 hours;

[0047] S3: Filter the solution after the reaction in S2, dissolve the filtered crude product in a second solvent to remove impurities in the crude product, and dry the solid product after filtration to obtain a pyrazole-rich flame retardant.

[0048] The molar ratio of 5-amino-3-methyl-1-phenylpyrazole, p-benzaldehyde, DOPO, the first solvent, and the second solvent is ...

Embodiment 3

[0055] The polymer flame retardant material containing pyrazole flame retardant proposed by the present invention includes the following raw materials in parts by weight: 25 parts of epoxy resin prepolymer, 1.65 parts of pyrazole flame retardant, 4,4'-diaminobis 6.5 parts of benzene methane.

[0056] The method steps of pyrazole flame retardant preparation are as follows:

[0057] S1: Add 5-amino-3-methyl-1-phenylpyrazole, p-benzaldehyde, and the first solvent to the reaction vessel in sequence, and stir at 105°C for 14 hours;

[0058] S2: Add DOPO to the reaction vessel of S1, and react at 105°C for 14 hours;

[0059] S3: Filter the solution after the reaction in S2, dissolve the filtered crude product in a second solvent to remove impurities in the crude product, and dry the solid product after filtration to obtain a pyrazole-rich flame retardant.

[0060]The molar volume ratio of 5-amino-3-methyl-1-phenylpyrazole, p-benzaldehyde, DOPO, and the first solvent is 1mol:5mol:5...

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Abstract

The invention discloses a polymer flame-retardant material containing a pyrazole flame retardant and a preparation method thereof. The polymer flame-retardant material is prepared from the following raw materials in parts by weight: an epoxy resin prepolymer, a pyrazole flame retardant and a curing agent. The preparation method comprises the following steps: heating the epoxy resin prepolymer to 60-150 DEG C, adding the pyrazole flame retardant, performing stirring in vacuum until the mixture is in a uniform and transparent state, adding the curing agent, completely dissolving, and curing to obtain the flame-retardant high polymer material. The pyrazole flame retardant prepared by the invention has the characteristics of good thermal stability, low smoke, low toxicity, good mechanical properties and the like, also has good flame retardance, is used for modifying epoxy resin, not only improves the flame retardance of the epoxy resin, but also can improve the thermal stability, transparency and the like of the epoxy resin, and enables a composite material to have the characteristic of multifunctionalization.

Description

technical field [0001] The invention relates to the technical field of organic flame retardants, in particular to polymer flame retardant materials containing pyrazole flame retardants and a preparation method thereof. Background technique [0002] Epoxy resin has the characteristics of excellent mechanical properties, corrosion resistance, good compactness and stable chemical properties, and is widely used in various aspects of life such as coatings, composite materials, casting materials, adhesives, molding materials and injection molding materials. However, due to the flammability of epoxy resin, once a fire breaks out, most of it will spread, which poses a great threat to the national economy and life. Therefore, flame retardant modification of epoxy resin is a very important work. [0003] Phosphorus-based flame retardants are currently considered to be a class of more efficient and environmentally friendly flame retardants, but most of the existing phosphorus-based fl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/00C08K5/5313C07F9/6574
CPCC07F9/657172C08K5/5313C08L2201/02C08L63/00
Inventor 杨梅陈瑞孙传伯王寅嵩张珍林
Owner WEST ANHUI UNIV
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