Preparing method of phosphorus nitrogen high load graphene flame retardant

A graphene and high-load technology, which is applied in the field of preparation of graphene flame retardants with high phosphorus and nitrogen loads, can solve the problems that graphene and flame retardants are difficult to disperse evenly and affect the synergistic flame retardant effect, and achieve a wide range of applications , improve the mechanical properties, the effect of stable performance

Active Publication Date: 2016-03-23
浙江迪恩新材料有限公司
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Problems solved by technology

However, this system is only obtained through simple physical blending of the two. It is difficult to achieve uniform dispersion of graphene and flame

Method used

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  • Preparing method of phosphorus nitrogen high load graphene flame retardant
  • Preparing method of phosphorus nitrogen high load graphene flame retardant

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[0021] Example 1

[0022] 1. Synthesis of isocyanate functionalized graphene: add 1.0g of graphene oxide powder particles to 200mL of chloroform, ultrasonically disperse for 120 minutes, then transfer to drying equipped with mechanical stirring, thermometer, reflux condenser and dropping funnel Add 0.05g of isophorone diisocyanate to a 250mL four-neck flask at room temperature, heat to 45°C, continue to stir and react for 5 hours, then filter the slurry obtained from the reaction, wash it repeatedly with chloroform, and dry it to obtain the isocyanate function Graphene.

[0023] 2. Synthesis of dendrimer functionalized graphene: Disperse 1.0g of isocyanate functionalized graphene obtained above into 80mL of acetonitrile, then add 0.5g of PAMAM, react at 20℃ for 10 hours, and then react to obtain The slurry is filtered to obtain a black solid powder, which is dried to obtain dendritic macromolecule functionalized graphene.

[0024] 3. Synthesis of phosphorus-nitrogen high-load graph...

Example Embodiment

[0025] Example 2

[0026] 1. Synthesis of isocyanate-functionalized graphene: the synthesis operation is the same as in Example 1, except that the isocyanate is diphenylmethane diisocyanate, the reaction temperature of graphene oxide and diphenylmethane diisocyanate is 90°C, and the reaction time For 2 hours, the feed mass ratio of graphene oxide to diphenylmethane diisocyanate is 1.0:0.3, and ethyl acetate is used as the solvent.

[0027] 2. Synthesis of dendrimer functionalized graphene: Disperse 1.0g of isocyanate functionalized graphene obtained by the above reaction into 80mL N,N-dimethylformamide, and then add the second generation polyamide-amine PAMAM to make the isocyanate The feed mass ratio of functionalized graphene to second-generation polyamide-amine is 1.0:2.0, and the mixture is reacted at 50°C for 3.5 hours, and then the slurry obtained by the reaction is filtered to obtain black solid powder, which is dried to obtain functionalized dendrimer Graphene.

[0028] 3. ...

Example Embodiment

[0030] Example 3

[0031] 1. Synthesis of isocyanate functionalized graphene:

[0032] The synthesis operation is the same as in Example 1, except that the isocyanate is hexamethylene diisocyanate, the reaction temperature of graphene oxide and hexamethylene diisocyanate is 35°C, and the reaction time is 4 hours. The feed mass ratio of methyl diisocyanate is 1.0:0.01, and the solvent is toluene.

[0033] 2. Synthesis of dendrimer functionalized graphene:

[0034] The synthesis operation is the same as in Example 1, the difference is: the reaction temperature of isocyanate functionalized graphene and polyamide-amine is 90°C, the reaction time is 3 hours, and the feed mass ratio of isocyanate functionalized graphene to first-generation polyamide-amine It is 1.0:1.0, and the solvent is chloroform.

[0035] 3. Synthesis of graphene flame retardant with high phosphorus and nitrogen loading:

[0036] The synthesis operation is the same as in Example 1. The difference is: the reaction tempera...

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Abstract

The invention relates to a preparing method of a flame retardant, in particular to a preparing method of a phosphorus nitrogen high load graphene flame retardant. The method comprises the following steps: (1) performing a surface grafting reaction on isocyanate and graphene oxide to prepare isocyanate functionalized graphene; (2) reacting the isocyanate functionalized graphene with dendrimer polyamide-amine (PAMAM) to prepare dendrimer functionalized graphene; (3) reacting the dendrimer functionalized graphene with a phosphoryl chloride compound to prepare the phosphorus nitrogen high load graphene flame retardant. The phosphorus nitrogen high load graphene flame retardant can retard flaming of a modified high polymer material and can improve mechanical properties of the high polymer material.

Description

technical field [0001] The invention relates to a preparation method of a flame retardant, in particular to a preparation method of a phosphorus-nitrogen high-loaded graphene flame retardant. Background technique [0002] With the deepening of research on polymer / graphene nanocomposites, the flame retardancy of polymer / graphene nanocomposites has attracted widespread attention from scholars at home and abroad. As a new type of flame retardant material, compared with traditional filled polymers, it has the advantages of high flame retardant efficiency, environmental protection, low toxicity, and excellent comprehensive performance. Compared with traditional filled polymers, polymer / graphene nanocomposites have the advantages of less addition amount and high flame retardant efficiency, but their application range is severely limited due to the lower flame retardant level. In order to further improve the flame retardant properties of polymer / graphene nanocomposites, graphene a...

Claims

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Application Information

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IPC IPC(8): C08K9/04C08K3/04
CPCC08K3/04C08K9/04
Inventor 黄国波方国忠吴鸿飞
Owner 浙江迪恩新材料有限公司
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