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Graphene grafted nitrogen, phosphorus and silicon synergistic halogen-free flame retardant and preparation method thereof

A technology of grafted graphite and flame retardants, applied in the field of flame retardants, can solve the problems of affecting material processing performance and mechanical properties, secondary pollution, low flame retardant efficiency, etc., achieve good application prospects, less smoke production, Inexpensive effect

Active Publication Date: 2019-01-11
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The main technical problems to be solved by the present invention are: the current halogen flame retardants will produce a large amount of smoke and release toxic and corrosive hydrogen halide gas when burning, causing secondary pollution; halogen-free flame retardant systems such as aluminum hydroxide, magnesium hydroxide Although it does not produce toxic hydrogen halide gas, its flame retardant efficiency is low, and a large amount of filling is required to have flame retardancy, which affects the processing performance and mechanical properties of the material; on the other hand, general flame retardant nanocomposites exist Dispersion and compatibility problems with polymer matrix limit its use

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Place a 500ml three-necked flask in constant temperature water at 50°C, then add 40ml of distilled water, 10ml of isopropanol, 2ml of acetonitrile, 10ml of triethylamine and 2ml of tetraethylammonium hydroxide into the three-necked flask in sequence, stir at a medium speed, and mix uniform. 80 g of 3-aminopropyltriethoxysilane was added dropwise to the mixture, and the mixture was reacted under constant temperature reflux at 50° C. for 12 h. After the reaction was completed, the above reaction solution was distilled under reduced pressure, and a large amount of white solids were precipitated upon standing still. It was filtered under reduced pressure, washed with acetone, and finally extracted with methanol. Vacuum drying finally gave the yellow solid product octaaminopropyl cage silsesquioxane, namely the reaction intermediate product 1.

[0027] Take 500 mg of graphene oxide and add it into 500 ml of tetrahydrofuran, and ultrasonically disperse for 1 h. The dispers...

Embodiment 2

[0030]Place a 500ml three-necked flask in constant temperature water at 60°C, then add 60ml of distilled water, 20ml of isopropanol, 2ml of acetonitrile, 10ml of triethylamine and 2ml of tetraethylammonium hydroxide into the three-necked flask in sequence, stir at a medium speed, and mix uniform. 100 g of 3-aminopropyltriethoxysilane was added dropwise to the mixture, and the mixture was reacted under constant temperature reflux at 60° C. for 24 h. After the reaction was completed, the above reaction solution was distilled under reduced pressure, and a large amount of white solids were precipitated upon standing still. It was filtered under reduced pressure, washed with acetone, and finally extracted with methanol. Vacuum drying finally gave the yellow solid product octaaminopropyl cage silsesquioxane, namely the reaction intermediate product 1.

[0031] Take 500 mg of graphene oxide and add it into 500 ml of tetrahydrofuran, and ultrasonically disperse for 1 h. The dispers...

Embodiment 3

[0034] Place a 500ml three-necked flask in constant temperature water at 65°C, then add 80ml of distilled water, 30ml of isopropanol, 2ml of acetonitrile, 10ml of triethylamine and 2ml of tetraethylammonium hydroxide into the three-necked flask in sequence, stir at a medium speed, and mix uniform. 120 g of 3-aminopropyltriethoxysilane was added dropwise to the mixture, and the mixture was reacted under constant temperature reflux at 65° C. for 36 h. After the reaction was completed, the above reaction solution was distilled under reduced pressure, and a large amount of white solids were precipitated upon standing still. It was filtered under reduced pressure, washed with acetone, and finally extracted with methanol. Vacuum drying finally gave the yellow solid product octaaminopropyl cage silsesquioxane, namely the reaction intermediate product 1.

[0035] Add 1 g of graphene oxide into 500 ml of tetrahydrofuran, and ultrasonically disperse for 1 h. The dispersion was transf...

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Abstract

The invention belongs to the technical field of fire retardants and mainly relates to a graphene grafted nitrogen, phosphorus and silicon synergistic halogen-free flame retardant and a preparation method thereof. The preparation method comprises the following steps: compounding 3-aminopropyl-triethoxysilane into octa-aminopropyl caged silsesquioxane through a hydrolytic condensation polymerizationprocess; preparing graphene oxide after chemically oxidizing and peeling graphene through an improved hummers process; compounding 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and graphene oxide into a grafted product 1 with an reactivity functional group through an in situ polymerization process; grafting the octa-aminopropyl caged silsesquioxane and the grafted product 1 into the graphenegrafted nitrogen, phosphorus and silicon synergistic halogen-free flame retardant through the in situ polymerization process. The preparation method for the graphene grafted nitrogen, phosphorus andsilicon synergistic halogen-free flame retardant provided by the invention has the advantages of simple preparation process, safety, environmental friendliness, and the like; the graphene grafted nitrogen, phosphorus and silicon synergistic halogen-free flame retardant can be widely used for inflaming retarding in the fields of electronics, automobiles, cables, packaging, aviation, and the like; the graphene grafted nitrogen, phosphorus and silicon synergistic halogen-free flame retardant has a bright application prospect.

Description

technical field [0001] The invention belongs to the technical field of flame retardants, and mainly relates to a nitrogen-phosphorus-silicon synergistic halogen-free flame retardant grafted with graphene and a preparation method thereof. Background technique [0002] Cage oligomeric silsesquioxane (POSS) is a nano-organic silicon material with a unique polyhedral cage structure. The cage skeleton is composed of Si—O—Si bonds. The Si atoms at the corners of the polyhedron can connect different organic functional group. This special structure makes POSS have unique physical and chemical properties, that is, the organic-inorganic hybrid structure composed of inorganic core and organic functional groups endows cage-type oligomeric silsesquioxane with excellent heat resistance and high reactivity; The nanoscale size endows it with special thermodynamic, magnetic and optical properties; through molecular design, various functionalized cage oligomeric silsesquioxanes can be prepar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00
CPCC08G83/001
Inventor 陈英红袁高炜杨冰王琪
Owner SICHUAN UNIV
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