Phosphor-rich graphene flame-retardant agent and preparation method thereof

A technology of flame retardant and graphene, which is applied in coatings, fireproof coatings, polyurea/polyurethane coatings, etc., can solve the problems of limited improvement of polymer flame retardancy and cannot be independently used as a flame retardant, and achieves an improvement Barrier effect, improvement of overall strength and compactness, improvement of flame retardant effect

Active Publication Date: 2017-06-23
宿迁聚萃功能复合材料研究所有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, graphene cannot be used independently as a flame retardant because it can only improve the flame retardant performance of polymers to a limited extent when it is added alone.

Method used

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  • Phosphor-rich graphene flame-retardant agent and preparation method thereof
  • Phosphor-rich graphene flame-retardant agent and preparation method thereof
  • Phosphor-rich graphene flame-retardant agent and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1 Preparation of rich phosphorized graphene flame retardant of the present invention

[0032]Under a nitrogen atmosphere, 4.28g CEPPA and 4.42kg KH560 (molar ratio 1:1) were heated, melted and mixed uniformly, and stirred and reacted at 120°C for 6h to obtain a CEPPA-linked silane coupling agent intermediate compound; 0.9ml deionized Add water (10wt%) to the intermediate compound, stir and hydrolyze at room temperature for 12 hours to remove excess water; disperse 1g of graphene oxide in 100ml of thionyl chloride for surface activation to obtain graphene acid chloride (GO-COCl), drop a few drops DMF was used as a catalyst, and after 24 hours of reaction, the excess thionyl chloride was removed by rotary evaporation, and the powder was dispersed in tetrahydrofuran to obtain a GO-COCl dispersion. The dried intermediate hydrolyzate was completely dissolved in tetrahydrofuran and added dropwise to GO-COCl The dispersion liquid was heated, stirred and refluxed for...

Embodiment 2

[0034] Embodiment 2 Preparation of rich phosphorized graphene flame retardant of the present invention

[0035] Under the atmosphere of helium, 4.32g DOPO and 4.73kg KH550 (molar ratio 1:1) were heated, melted and mixed uniformly, and stirred and reacted at 160°C for 8h to obtain the intermediate compound of DOPO-linked silane coupling agent; Ionized water (5wt%) was added to the intermediate compound, stirred and hydrolyzed at room temperature for 24h to remove excess water; 1.5g graphene oxide was dispersed in 200ml thionyl chloride for surface activation to obtain graphene acid chloride (GO-COCl), dropwise A few drops of dimethylacetamide was used as a catalyst, and after 12 hours of reaction, the excess thionyl chloride was removed by rotary evaporation, and the powder was dispersed in dichloromethane to obtain a GO-COCl dispersion, and the dried intermediate hydrolyzate was completely dissolved in di Add the GO-COCl dispersion dropwise into the methyl chloride, heat, stir...

Embodiment 3

[0040] Embodiment 3 Preparation of rich phosphorized graphene flame retardant of the present invention

[0041] Under a nitrogen atmosphere, 4.28g of CEPPA and 3.94kg of aminopropyltrimethoxysilane (molar ratio 1:1.1) were heated, melted and mixed uniformly, and stirred and reacted at 120°C for 6 hours to obtain a CEPPA-linked silane coupling agent intermediate compound; 0.6ml of deionized water (7wt%) was added to the intermediate compound, stirred and hydrolyzed at room temperature for 8h to remove excess water; 1.5g of graphene oxide was dispersed in 200ml of thionyl chloride for surface activation to obtain graphene acyl chloride (GO-COCl ), drop a few drops of lutidine as a catalyst, and remove excess thionyl chloride by rotary evaporation after 24 hours of reaction, and disperse the powder in ethyl acetate to obtain a GO-COCl dispersion, and completely dry the intermediate hydrolyzate Dissolve in ethyl acetate and add GO-COCl dispersion drop by drop, heat, stir and reflu...

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Abstract

The invention provides a phosphor-rich graphene flame-retardant agent with a structural formula shown in the description. The invention also provides a preparation method of the phosphor-rich graphene flame-retardant agent. The preparation method is characterized in that graphene oxide is used as a basic raw material, reactive groups at both ends of a silane coupler containing a silicon carbon layer improving agent are fully utilized, one end of the silane coupler is connected with acid source components, such as CEPPA (carboxyethyl phenyl phosphinic acid), DOPO or derivatives, and the other end of the silane coupler is connected with the graphene oxide, so as to obtain a macromolecular flame retardant integrating a physical carbon layer, an acid source and the carbon layer improving agent. The phosphor-rich graphene flame-retardant agent has the advantages that the flame-retardant efficiency is high, the polarity is low, the moisture absorbing property is little, and the mechanical property of the material can be well maintained; by not containing halogen, the flame-retardant agent is friendly to the human body and environment, and meets the green development direction of future flame-retardant agents.

Description

technical field [0001] The invention relates to a flame retardant rich in phosphorized graphene. Background technique [0002] Polymer materials are widely used in important fields of the national economy such as automobiles, construction, packaging, aerospace, and military. However, due to their chemical composition (mainly composed of carbon and hydrogen), polymer materials are extremely flammable, and in the combustion process A large amount of toxic and harmful gases are released in the air, which has brought great safety hazards to people's lives and property safety. Therefore, it is very important for polymer materials to be flame retardant, and flame retardants are the second largest additives for polymer materials. And with the increasing pressure of environmental protection, new green and environmentally friendly flame retardants will surely become a hot spot in future research and development. [0003] Phosphorus-based flame retardants are a very important class ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K3/04C08K9/04C08K9/06C08K9/02C08K7/14C09D175/04C09D7/12C08L63/00C08L77/06C08L85/02C08L29/04
CPCC08J5/18C08J2329/04C08K3/04C08K7/14C08K9/02C08K9/04C08K9/06C08L77/06C08L2201/02C08L2203/16C09D5/18C09D7/61C09D175/04C08L85/02C08L63/00C08L29/04
Inventor 刘渊包建军陈文华
Owner 宿迁聚萃功能复合材料研究所有限公司
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