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Silsesquioxane-modified melamine fire retardant and preparation method thereof

A technology of silsesquioxane and melamine, which is applied in the field of polymer materials and flame retardant chemistry, can solve the problems of complex preparation process of melamine flame retardant, influence of flame retardant performance, and inability to uniformly disperse, so as to achieve good development prospects and improve Good compatibility, mechanical properties and thermal stability

Active Publication Date: 2019-11-05
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But as the research found, common melamine-based flame retardants also have some disadvantages
Melamine flame retardants are often combined with polymer materials, but due to poor compatibility between the two, they cannot be uniformly dispersed, and the flame retardant performance is affected to a certain extent
For example, nylon 6 itself has poor heat resistance, and its bonding properties are similar to melamine cyanurate (MCA). The two can be combined to improve flame retardancy, but due to the poor compatibility between MCA and nylon materials, resulting in low flame retardant efficiency
At the same time, the melamine flame retardant also has problems such as complicated preparation process and difficult access to raw materials.
It can be seen that ordinary melamine-based flame retardants still limit their better development

Method used

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  • Silsesquioxane-modified melamine fire retardant and preparation method thereof
  • Silsesquioxane-modified melamine fire retardant and preparation method thereof
  • Silsesquioxane-modified melamine fire retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 1) Dissolve 1.3g of cyanuric chloride, 2.9g of p-aminobenzoic acid, and 1.4g of sodium hydroxide in 280mL of water, stir and react at 70°C for 24 hours, lower the reaction solution to room temperature, add concentrated hydrochloric acid to acidify, and filter the precipitate ,, 2.5 g of white powdery 4,4',4"-(1,3,5-triazine-2,4,6-triazine)tribenzoic acid was obtained after vacuum spin-drying.

[0027] 2) 2.3g of 4,4',4"-(1,3,5-triazine-2,4,6-triazol)tribenzoic acid and 4.7g of 2-ethoxy-1-ethoxy Carbonyl-1,2-dihydroquinoline was reacted at 65°C for 10 minutes in a mixed solvent of 640mL dioxane and 330mL methanol, then 12.4g of monoaminosilsesquioxane was added, and the reaction was continued for 24 hours Afterwards, it was lowered to room temperature, spin-dried in vacuo, and recrystallized twice with n-hexane to obtain 10.4 g of the target product.

Embodiment 2

[0029] 1) Dissolve 1.5g of cyanuric chloride, 3.3g of p-aminobenzoic acid, and 1.6g of sodium hydroxide in 320mL of water, stir and react at 80°C for 36 hours, lower the reaction solution to room temperature, add concentrated hydrochloric acid to acidify, and filter the precipitate , 2.8 g of white powdery 4,4',4"-(1,3,5-triazine-2,4,6-triazine)tribenzoic acid was obtained after vacuum spin-drying.

[0030] 2) 2.4g of 4,4',4"-(1,3,5-triazine-2,4,6-triazol)tribenzoic acid and 4.9g of 2-ethoxy-1-ethoxy Carbonyl-1,2-dihydroquinoline was reacted at 75°C for 20 minutes in a mixed solvent of 670mL dioxane and 340mL methanol, then 12.9g of monoaminosilsesquioxane was added, and the reaction was continued for 36 hours Afterwards, it was lowered to room temperature, spin-dried in vacuum, and recrystallized twice with n-hexane to obtain 10.9 g of the target product.

Embodiment 3

[0032] 1) Dissolve 1.8g of cyanuric chloride, 4.0g of p-aminobenzoic acid, and 2.0g of sodium hydroxide in 390mL of water, stir and react at 90°C for 48 hours, lower the reaction solution to room temperature, add concentrated hydrochloric acid to acidify, and filter the precipitate ,, 4.7 g of white powdery 4,4',4"-(1,3,5-triazine-2,4,6-triazine)tribenzoic acid was obtained after vacuum spin-drying.

[0033]2) 3.2g of 4,4',4"-(1,3,5-triazine-2,4,6-triazol)tribenzoic acid and 6.5g of 2-ethoxy-1-ethoxy Carbonyl-1,2-dihydroquinoline was reacted at 85°C for 30 minutes in a mixed solvent of 890mL dioxane and 460mL methanol, then 17.2g of monoaminosilsesquioxane was added, and the reaction was continued for 48 hours Afterwards, it was lowered to room temperature, spin-dried in vacuum, and recrystallized twice with n-hexane to obtain 14.5 g of the target product.

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Abstract

The invention discloses a silsesquioxane-modified melamine compound, and a preparation method and an application thereof. The method comprises the following steps: reacting raw materials which are cyanuric chloride, p-aminobenzoic acid and sodium hydroxide in an aqueous solvent system to prepare 4,4',4''-(1,3,5-triazine-2,4,6-trinitro)tribenzoic acid, and then reacting the 4,4',4''-(1,3,5-triazine-2,4,6-trinitro)tribenzoic acid with 2-ethoxy-1-ethoxycarbonyl-1,2-dihydroquinoline and monoaminosilsesquioxane in a dioxane and methanol mixed solvent system to prepare the target product. A result of test shows that the silsesquioxane-modified melamine compound prepared in the invention can significantly improve the compatibility with high-molecular materials in order to effectively improve thefire retardant efficiency. The preparation method of the compound has the advantages of simplicity, easy availability of the raw materials, low cost, realization of large-scale production, and very strong practical values.

Description

technical field [0001] The invention belongs to the field of polymer materials and flame-retardant chemistry, and specifically relates to a silsesquioxane-modified melamine compound and a preparation method and application thereof. Background technique [0002] With the development of polymer materials, the production of a large number of flammable substances has brought more and more harm to society. According to the survey, at least 4,000 people are killed by fires in the United States every year, and more than 5,000 people in Europe, and the economic losses caused are hundreds of millions. Therefore, as an additive that can make flammable materials have flame retardant properties, the importance of flame retardants is self-evident. At the beginning of the last century, researchers began to conduct in-depth research on flame retardant technology, and devoted themselves to the research of highly efficient flame retardants. Compared with intrinsic flame retardant materials...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/388
CPCC08G77/045
Inventor 杨海宽王宏艳詹婷婷
Owner ZHONGBEI UNIV
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