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Phosphazene fire retardant graft modification carbon nano tube and preparation method thereof

A phosphazene flame retardant, carbon nanotube technology, applied in the direction of fibrous filler, dyed low-molecular-weight organic compounds, etc., can solve the problems of high cost, complicated reaction process, etc., achieve high conversion rate, large preparation amount, improve dispersive effect

Inactive Publication Date: 2013-06-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the preparation method of the above-mentioned modified carbon nanotubes has more or less complicated reaction process, involves thionyl chloride chlorination, and has disadvantages such as high cost, and there are certain limitations in practical application.

Method used

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  • Phosphazene fire retardant graft modification carbon nano tube and preparation method thereof
  • Phosphazene fire retardant graft modification carbon nano tube and preparation method thereof
  • Phosphazene fire retardant graft modification carbon nano tube and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Add 2 g of purified carbon nanotubes into a conical flask filled with 45 ml of concentrated sulfuric acid and concentrated nitric acid (volume ratio 3:1), and ultrasonicate at 50°C for 3 hours. After sonication, pour a large amount of deionized water to dilute, vacuum filter and continuously wash with deionized water until neutral. The solid was dried in a vacuum oven at 80° C. for 12 h to constant weight to obtain acidified carbon nanotubes.

[0026] (2) Take 2g of acidified carbon nanotubes, 2g of hexachlorocyclotriphosphazene, 0.7g of sodium hydroxide, and 80ml of tetrahydrofuran, pour them into a three-necked flask and mix them thoroughly, and ultrasonicate for 30 minutes to fully dissolve and disperse them. After purging nitrogen for 20 minutes to remove oxygen, the reaction was refluxed for 36 hours at 65° C. under strong magnetic stirring. After the reaction, the obtained product was vacuum filtered, washed with tetrahydrofuran and acetone several times, and...

Embodiment 2

[0030] (1) Add 2 g of purified carbon nanotubes into a conical flask filled with 45 ml of concentrated sulfuric acid and concentrated nitric acid (volume ratio 3:1), and sonicate at 50°C for 4 hours. After sonication, pour a large amount of deionized water to dilute, vacuum filter and continuously wash with deionized water until neutral. The solid was dried in a vacuum oven at 80° C. for 12 h to constant weight to obtain acidified carbon nanotubes.

[0031] (2) Take 2g of acidified carbon nanotubes, 2g of hexachlorocyclotriphosphazene, 0.7g of sodium hydroxide, and 80ml of tetrahydrofuran, pour them into a three-necked flask and mix them thoroughly, and ultrasonicate for 30 minutes to fully dissolve and disperse them. After purging nitrogen for 20 minutes to remove oxygen, the reaction was refluxed for 36 hours at 65° C. under strong magnetic stirring. After the reaction, the obtained product was vacuum filtered, washed with tetrahydrofuran and acetone several times, and drie...

Embodiment 3

[0033] (1) Add 2 g of purified carbon nanotubes into a conical flask filled with 45 ml of concentrated sulfuric acid and concentrated nitric acid (volume ratio 3:1), and ultrasonicate at 50°C for 5 hours. After sonication, pour a large amount of deionized water to dilute, vacuum filter and continuously wash with deionized water until neutral. The solid was dried in a vacuum oven at 80° C. for 12 h to constant weight to obtain acidified carbon nanotubes.

[0034] (2) Take 2g of acidified carbon nanotubes, 2g of hexachlorocyclotriphosphazene, 0.7g of sodium hydroxide, and 80ml of tetrahydrofuran, pour them into a three-necked flask and mix them thoroughly, and ultrasonicate for 30 minutes to fully dissolve and disperse them. After purging nitrogen for 20 minutes to remove oxygen, the reaction was refluxed for 48 hours at 65° C. under strong magnetic stirring. After the reaction, the obtained product was vacuum filtered, washed with tetrahydrofuran and acetone several times, and...

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Abstract

The invention relates to a phosphazene fire retardant graft modification carbon nano tube and a preparation method thereof and belongs to the field of carbon nano tube modification. After acidizing is performed to the purified carbon nano tube firstly, active carboxyl is introduced to a surface of the carbon nano tube; and under catalysis of metal hydroxide or metal hydride, the carboxyl reacts with phosphazene fire retardant phosphonitrilic chloride trimer so that the phosphazene fire retardant is grafted to the surface of the carbon nano tube through a chemical bond. The phosphazene fire retardant graft modification carbon nano tube and the preparation method thereof aim at grafting the fire retardant rich in inflaming retarding elements such as phosphorus, nitrogen, chlorine and the like to the surface of the carbon nano tube through the chemical bond so that a novel carbon nano tube with fire retardant surface graft modification is obtained and can be mixed with various resin matrixes. Fire retardant property of the carbon nano tube can be completely improved and meanwhile dispersity and compatibility of the carbon nano tube in the resin matrix are improved.

Description

technical field [0001] The invention relates to the field of modification of carbon nanotubes, in particular to a surface grafted modified carbon nanotube of a phosphazene flame retardant and a preparation method thereof. Background technique [0002] Since Professor S. Lijima of NEC discovered carbon nanotubes in 1991, because of their high strength, high aspect ratio, high specific surface area, high thermal stability, excellent electrical conductivity, excellent thermal conductivity and unique one-dimensional The tubular structure makes carbon nanotubes widely used in the research of drug carriers, catalysts, and biosensors. [0003] The Japanese scholar Fujiwara first applied for a patent on nano-clay flame-retardant nylon in 1976, which opened up another research hotspot of nano-flame retardant materials. Studies have found that adding a very small amount (<5%) of carbon nanotubes to the resin matrix will not only improve the mechanical properties of the composite m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/04C08K7/00C08K3/04C09C1/44C09C3/08
Inventor 张胜孙军谷晓昱邹欢
Owner BEIJING UNIV OF CHEM TECH
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