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Carbon nano tube containing 9,10-Dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) base group and preparation method thereof

A technology of carbon nanotubes and groups, applied in the field of materials, can solve the problems of poor mechanical properties of polymers, and achieve the effects of improving flame retardancy, improving mechanical properties, and mild process conditions

Inactive Publication Date: 2012-07-25
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the addition of the flame retardant DOPO to the polymer can improve its flame retardant performance, it will also deteriorate the mechanical properties of the polymer to a certain extent.

Method used

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  • Carbon nano tube containing 9,10-Dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) base group and preparation method thereof
  • Carbon nano tube containing 9,10-Dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) base group and preparation method thereof
  • Carbon nano tube containing 9,10-Dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) base group and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 1. Mix 100 g of H 2 SO 4 with HNO 3 mixed solution (98%H 2 SO 4 : 68% HNO 3 = 3:1) mixed with 5 g of carbon nanotubes, and refluxed for 4 hours at 100°C under ultrasonic vibration. Then wash with water repeatedly until the pH is neutral. The product was obtained by vacuum drying. With 150 g H 2 SO 4 with H 2 o 2 mixed solution (98%H 2 SO 4 : 30%H 2 o 2 = 4:1) was mixed with 5 g of the above-mentioned one-step acidification product, and refluxed at 70°C for 2.5 hours. Then wash with water repeatedly until the pH is neutral.

[0030] 2. Take 5 grams of the above-mentioned acidified carbon nanotubes and 250 grams of thionyl chloride, and stir and reflux at 70 ° C for 24 hours. Filter and wash with tetrahydrofuran (THF) until neutral.

[0031] 3. Add 100 grams of DOPO to 500 grams of ethanol, heat up to 80°C, slowly add 200 grams of formaldehyde solution dropwise under stirring, and heat up and reflux for 12 hours. After the reaction was completed, it was...

Embodiment 2

[0035] 1. Mix 70 g of H 2 SO 4 with HNO 3 mixed solution (98%H 2 SO 4 : 68% HNO 3 = 3:1) mixed with 5 g of carbon nanotubes, and refluxed for 4 hours at 80°C under ultrasonic vibration. Then wash with water repeatedly until the pH is neutral. The product was obtained by vacuum drying. With 100 g H 2 SO 4 with H 2 o 2 mixed solution (98%H 2 SO 4 : 30%H 2 o 2 = 4:1) was mixed with 5 grams of the above-mentioned one-step acidification product, and refluxed at 70°C for 2 hours. Then wash with water repeatedly until the pH is neutral.

[0036]2. Take 5 grams of the above-mentioned acidified carbon nanotubes and 200 grams of thionyl chloride, and stir and reflux at 70 ° C for 24 hours. Filter and wash with tetrahydrofuran (THF) until neutral.

[0037] 3. Add 80 grams of DOPO into 1000 grams of toluene, heat up to 70°C, slowly add 100 grams of acetaldehyde aqueous solution dropwise under stirring, and heat up and reflux for 8 hours. After the reaction was completed...

Embodiment 3

[0040] 1. Mix 450 g of H 2 SO 4 with HNO 3 mixed solution (98%H 2 SO 4 : 68% HNO 3 = 3:1) were mixed with 3 g of carbon nanotubes, and refluxed for 4 hours at 200°C under ultrasonic vibration. Then wash with water repeatedly until the pH is neutral. The product was obtained by vacuum drying. With 450 g H 2 SO 4 with H 2 o 2 mixed solution (98%H 2 SO 4 : 30%H 2 o 2 = 4:1) was mixed with 3 g of the above-mentioned one-step acidification product, and refluxed at 70°C for 4 hours. Then wash with water repeatedly until the pH is neutral.

[0041] 2. Take 3 grams of the above-mentioned acidified carbon nanotubes and 300 grams of thionyl chloride, and stir and reflux at 70 ° C for 24 hours. Filter and wash with tetrahydrofuran (THF) until neutral.

[0042] 3. Add 10 grams of DOPO into 1500 grams of ethanol, heat up to 140°C, slowly add 200 grams of propionaldehyde aqueous solution dropwise under stirring, and heat up and reflux for 1 hour. After the reaction was co...

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Abstract

The invention belongs to the technical field of materials and particularly relates to a carbon nano tube containing a 9,10-Dihydro-9-oxa-10-phosphaphenanthrene 10-oxide (DOPO) base group and a preparation method thereof. The preparation method specifically comprises the following steps of: performing chemical reaction on a carbon nano tube and POPO respectively to ensure that the carbon nano tubeand the DOPO have a certain chemical base group respectively so as to obtain the DOPO with a hydroxyl and a chlorinated carbon nano tube; and reacting the DOPO with the hydroxyl and the chlorinated carbon nano tube to obtain the carbon nano tube with the DOPO base group. The carbon nano tube with the DOPO base group can be used for flame resistance of a high polymer and a composite material of the high polymer, and can improve the flame resistance of the material and keep or improve the mechanical property of the material. The preparation method of the carbon nano tube with the DOPO base group is simple and effective and is suitable for batch production, and the process conditions are mild.

Description

technical field [0001] The invention belongs to the field of material technology, and in particular relates to a carbon nanotube containing a phosphorus-based flame retardant 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) and a preparation method thereof. It can be used to improve the flame retardancy and mechanical properties of high polymers and their composite materials. Background technique [0002] Carbon nanotubes are seamless nanoscale tubes formed by single-layer or multi-layer graphite sheets curled around the central axis at a certain helical angle. Since Lijima discovered carbon nanotubes in 1991, carbon nanotubes have been used due to their unique structure. Good electrical and mechanical properties are the research hotspots in recent years. At the same time, carbon nanotubes can be a flame retardant additive due to their high tensile shape and high specific surface area, and some studies have proved their flame retardant effect. Adding carbon nanotu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/04C08K7/00C08K3/04
Inventor 于涛李岩罗业董闽沈
Owner TONGJI UNIV
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