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A nitrogen-phosphorus-silicon synergistic halogen-free flame retardant grafted with graphene and its preparation method

A technology of grafted graphite and flame retardant, applied in the field of flame retardants, can solve the problems of low flame retardant efficiency, secondary pollution, affecting material processing performance and mechanical properties, etc., and achieves less smoke production, low price, good The effect of applying the foreground

Active Publication Date: 2020-08-04
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 a constant temperature water area of ​​50°C, and 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, stirring at medium speed, and mixing Evenly. 80g of 3-aminopropyltriethoxysilane was added dropwise to the mixed solution, and the mixture was refluxed for 12 hours at a constant temperature of 50°C. After the completion of the reaction, the reaction liquid was distilled under reduced pressure, and a large amount of white solid was deposited on standing. After vacuum filtration, acetone washing, and finally methanol extraction. Vacuum drying finally obtains the yellow solid product octaaminopropyl cage silsesquioxane, which is the reaction intermediate product 1.

[0027] Take 500 mg of graphene oxide and add it to 500 ml of tetrahydrofuran, and ultrasonically disperse for 1 hour. The dispersion was transferred to a three-...

Embodiment 2

[0030] Place a 500ml three-necked flask in a constant temperature water area of ​​60°C, then add 60ml distilled water, 20ml isopropanol, 2ml acetonitrile, 10ml triethylamine and 2ml tetraethylammonium hydroxide into the three-necked flask, stir at medium speed, and mix Evenly. 100g of 3-aminopropyltriethoxysilane was added dropwise to the mixed solution, and the mixture was refluxed for 24 hours at a constant temperature of 60°C. After the completion of the reaction, the reaction liquid was distilled under reduced pressure, and a large amount of white solid was deposited on standing. After vacuum filtration, acetone washing, and finally methanol extraction. Vacuum drying finally obtains the yellow solid product octaaminopropyl cage silsesquioxane, which is the reaction intermediate product 1.

[0031] Take 500 mg of graphene oxide and add it to 500 ml of tetrahydrofuran, and ultrasonically disperse for 1 hour. The dispersion was transferred to a three-necked flask filled with ...

Embodiment 3

[0034] Place a 500ml three-necked flask in a constant temperature water area of ​​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, stir at medium speed, and mix Evenly. 120 g of 3-aminopropyltriethoxysilane was added dropwise to the mixed solution, and the mixture was refluxed for 36 hours at a constant temperature of 65°C. After the completion of the reaction, the reaction liquid was distilled under reduced pressure, and a large amount of white solid was deposited on standing. After vacuum filtration, acetone washing, and finally methanol extraction. Vacuum drying finally obtains the yellow solid product octaaminopropyl cage silsesquioxane, which is the reaction intermediate product 1.

[0035] Take 1g of graphene oxide and add it to 500ml of tetrahydrofuran, and ultrasonically disperse for 1h. The dispersion was transferred to a three-necked flask fille...

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Abstract

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. Synthesis of octaaminopropyl cage silsesquioxane; preparing graphene oxide through chemical oxidation and exfoliation of graphene through improved hummers method; 9,10-dihydro-9-oxa-10-phosphaphenanthrene Synthesis of grafted product 1 with reactive functional groups by in-situ polymerization of ‑10‑oxide and graphene oxide; grafted graphite synthesized by in-situ polymerization of octaaminopropyl cage silsesquioxane and grafted product 1 Nitrogen-phosphorus-silicon synergistic halogen-free flame retardant. The preparation method of the nitrogen-phosphorus-silicon synergistic halogen-free flame retardant of grafted graphene prepared by the present invention has the advantages of simple preparation process, safety and environmental protection, and can be widely used in flame retardants in the fields of electronic appliances, automobiles, cables, packaging, aviation, etc. Combustion, has broad development prospects.

Description

Technical field [0001] The invention belongs to the technical field of flame retardants, and mainly relates to a nitrogen, phosphorus and 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 frame is composed of Si—O—Si bonds. The Si atoms at the top corners of the polyhedron can connect different organic Functional group. This special structure gives POSS unique physical and chemical properties, that is, the organic-inorganic hybrid structure composed of inorganic core and organic functional groups endows cage oligomeric silsesquioxane with excellent heat resistance and higher reactivity; Nano-scale size gives it special thermodynamic, magnetic and optical properties; through molecular design, various functionalized cage oligomeric silsesquioxanes can be prepared, which can gi...

Claims

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Application Information

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Patent Type & Authority Patents(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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