Preparation method of modified graphene oxide and preparation method of composite material containing modified graphene oxide

Abstract

The invention provides a preparation method of a modified graphene oxide, comprising the following steps of: (a) reacting a phosphorus oxychloride compound, cyanuric chloride or diisocyanate with glycidol to obtain an intermediate product; and (b) dispersing graphite oxide in an organic solvent, dropwise adding to the intermediate product obtained through reaction, and reacting to obtain the modified graphene oxide. The invention also provides a preparation method of a composite material containing the modified graphene oxide, comprising the following steps of: dispersing the modified graphene oxide obtained through the preparation method in the technical scheme in an organic solvent, mixing the modified graphene oxide containing epoxide groups with epoxy resin oligomers and a polyamide curing agent, and curing to obtain the composite material containing the modified graphene oxide. In the composite material provided by the invention, the modified graphene oxide reacts with a resin substrate, is more uniform to disperse in the obtained composite material, and has better flame-retarding performance.

Description

technical field

[0001] The invention belongs to the technical field of graphene, and in particular relates to a method for preparing modified graphene oxide and a method for preparing a composite material containing modified graphene oxide. Background technique

[0002] Graphene is a new type of carbonaceous material with a thickness of a single layer of carbon atoms and is composed of carbon atoms arranged in a two-dimensional honeycomb lattice structure. It is considered to be the basic unit of all other dimensional carbonaceous materials. Zero-dimensional fullerenes, one-dimensional carbon nanotubes, and three-dimensional graphite. Graphene is composed of carbon atoms with sp 2 The single-atom carbon layer formed by hybridization has a very stable structure, excellent mechanical properties, peculiar electrical properties and good thermal properties. The study found that the Young's modulus of graphene can reach 11000GPa, the fracture strength can reach 125GPa, and the th...

Examples

preparation example Construction

[0037] The invention provides a preparation method of modified graphene oxide, comprising the following steps:

[0038] a) phosphorous oxychloride compound, cyanuric chloride or diisocyanate react with glycidol to obtain an intermediate product;

[0039] b) dispersing graphite oxide in an organic solvent, adding dropwise to the intermediate product, and obtaining modified graphene oxide after the reaction.

[0040] N and P are flame retardant elements. Adding N and / or P to the polymer can improve the flame retardant performance of the polymer. Therefore, after modifying graphene oxide with N and / or P, the resistance of graphene oxide can be improved. The flame retardancy of the polymer can also be improved after the modified graphene oxide is blended into the polymer. However, when the modified graphene oxide is added to the polymer by blending, the flame retardant performance of the polymer is limited due to uneven dispersion. Therefore, the inventors used a compound contain...

Embodiment 1

[0085] Add 46mL of concentrated sulfuric acid and 1g of sodium nitrate to a 250mL three-neck flask equipped with a mechanical stirrer, reflux condenser, constant pressure dropping funnel, and nitrogen inlet, and mix evenly under pressure, then add 2g of expandable graphite with a particle size of 325 mesh , Stir the reaction in an ice bath for 15 minutes, keep the temperature of the reaction solution below 5°C, slowly add 15g of potassium permanganate within 10 minutes, keep the temperature of the reaction solution below 10°C during the addition of potassium permanganate, and finish adding the potassium permanganate dropwise Finally, react in an ice bath for 30 minutes, then transfer to an oil bath, the temperature of the oil bath is 35°C, and react for 1 hour, then add 92 mL of deionized water dropwise to the reaction solution, and raise the temperature of the reaction solution to 98°C, and react for 15 minutes. , pour the obtained reaction solution into a beaker, dilute with ...

Embodiment 2

[0089] Add 6.33g (0.03mol) of phenyl phosphate dichloride and 6.06g (0.06mol) of trichloride into a 250mL three-necked flask equipped with a mechanical stirrer, a reflux condenser, a constant pressure dropping funnel, and a nitrogen inlet under stirring in an ice bath. Ethylamine; 3.48g (0.03mol) glycidol was dissolved in 20mL acetone, and slowly added dropwise to a three-necked flask within 2 hours, and after 4 hours of reaction, glycidyl alcohol-chlorinated phenyl phosphate was obtained; 0.5g was implemented The graphite oxide prepared in Example 1 was dispersed in 100 mL of acetone. After ultrasonication for 1 h, it was added dropwise to the glycidyl alcohol-chlorinated phenyl phosphate through a constant pressure dropping funnel within 1 h, stirred at room temperature for 12 h, and the obtained reaction Liquid was filtered, and the filter cake was washed three times with deionized water to obtain a yellow-brown product.

[0090] Infrared analysis is carried out to describe...

technical field

[0001] The invention belongs to the technical field of graphene, and in particular relates to a method for preparing modified graphene oxide and a method for preparing a composite material containing modified graphene oxide. Background technique

[0002] Graphene is a new type of carbonaceous material with a thickness of a single layer of carbon atoms and is composed of carbon atoms arranged in a two-dimensional honeycomb lattice structure. It is considered to be the basic unit of all other dimensional carbonaceous materials. Zero-dimensional fullerenes, one-dimensional carbon nanotubes, and three-dimensional graphite. Graphene is composed of carbon atoms with sp 2 The single-atom carbon layer formed by hybridization has a very stable structure, excellent mechanical properties, peculiar electrical properties and good thermal properties. The study found that the Young's modulus of graphene can reach 11000GPa, the fracture strength can reach 125GPa, and the th...

Examples

preparation example Construction

[0037] The invention provides a preparation method of modified graphene oxide, comprising the following steps:

[0038] a) phosphorous oxychloride compound, cyanuric chloride or diisocyanate react with glycidol to obtain an intermediate product;

[0039] b) dispersing graphite oxide in an organic solvent, adding dropwise to the intermediate product, and obtaining modified graphene oxide after the reaction.

[0040] N and P are flame retardant elements. Adding N and / or P to the polymer can improve the flame retardant performance of the polymer. Therefore, after modifying graphene oxide with N and / or P, the resistance of graphene oxide can be improved. The flame retardancy of the polymer can also be improved after the modified graphene oxide is blended into the polymer. However, when the modified graphene oxide is added to the polymer by blending, the flame retardant performance of the polymer is limited due to uneven dispersion. Therefore, the inventors used a compound contain...

Embodiment 1

[0085] Add 46mL of concentrated sulfuric acid and 1g of sodium nitrate to a 250mL three-neck flask equipped with a mechanical stirrer, reflux condenser, constant pressure dropping funnel, and nitrogen inlet, and mix evenly under pressure, then add 2g of expandable graphite with a particle size of 325 mesh , Stir the reaction in an ice bath for 15 minutes, keep the temperature of the reaction solution below 5°C, slowly add 15g of potassium permanganate within 10 minutes, keep the temperature of the reaction solution below 10°C during the addition of potassium permanganate, and finish adding the potassium permanganate dropwise Finally, react in an ice bath for 30 minutes, then transfer to an oil bath, the temperature of the oil bath is 35°C, and react for 1 hour, then add 92 mL of deionized water dropwise to the reaction solution, and raise the temperature of the reaction solution to 98°C, and react for 15 minutes. , pour the obtained reaction solution into a beaker, dilute with ...

Embodiment 2

[0089] Add 6.33g (0.03mol) of phenyl phosphate dichloride and 6.06g (0.06mol) of trichloride into a 250mL three-necked flask equipped with a mechanical stirrer, a reflux condenser, a constant pressure dropping funnel, and a nitrogen inlet under stirring in an ice bath. Ethylamine; 3.48g (0.03mol) glycidol was dissolved in 20mL acetone, and slowly added dropwise to a three-necked flask within 2 hours, and after 4 hours of reaction, glycidyl alcohol-chlorinated phenyl phosphate was obtained; 0.5g was implemented The graphite oxide prepared in Example 1 was dispersed in 100 mL of acetone. After ultrasonication for 1 h, it was added dropwise to the glycidyl alcohol-chlorinated phenyl phosphate through a constant pressure dropping funnel within 1 h, stirred at room temperature for 12 h, and the obtained reaction Liquid was filtered, and the filter cake was washed three times with deionized water to obtain a yellow-brown product.

[0090] Infrared analysis is carried out to describe...

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