A preparation method of flame-retardant modified graphene and its modified thermoplastic elastomer

A thermoplastic elastomer and graphene technology, which is applied in the field of flame retardant material preparation, can solve the problems of difficulty in achieving the flame retardant level of composite materials, restricting the popularization and application of graphene, and poor dispersion of graphene, so as to reduce secondary pollution and the scope of application Broadening and reducing the effect of reunion tendency

Active Publication Date: 2022-05-13
TAIZHOU UNIV
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Problems solved by technology

[0004] The purpose of the present invention is to provide a preparation method of flame-retardant modified graphene and its modified thermoplastic elastomer, so as to solve the problem of poor graphene dispersion, high price, and difficulty in the flame-retardant grade of the prepared composite material proposed in the above-mentioned background technology. Reaching the flame retardant standard of the industry seriously restricts the popularization and application of graphene in polymer flame retardant modification

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  • A preparation method of flame-retardant modified graphene and its modified thermoplastic elastomer
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  • A preparation method of flame-retardant modified graphene and its modified thermoplastic elastomer

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preparation example Construction

[0025] The invention provides a preparation method of flame-retardant modified graphene and its modified thermoplastic elastomer, which improves the expansion and flame-retardant efficiency of phosphorus-nitrogen flame-retardant modified graphene, and helps to improve the mechanical properties, electrical conductivity and resistance of substrate materials. Combustibility, solve the dispersion problem of graphene in the process of processing, give full play to its nano-enhanced effect, please refer to figure 1 ,

[0026] The preparation method of this flame-retardant modified graphene comprises the steps:

[0027] S1: Graphene oxide nitrogen doping reaction: Graphene oxide, 1,3,5-triazine and dimethylformamide are mixed in a certain mass ratio, and the above mixture is transferred to a reactor lined with polytetrafluoroethylene, Under nitrogen protection, heat to 80°C-150°C, stir for 2-10 hours, add distilled water to filter after the reaction, and then vacuum filter and dry t...

Embodiment 1

[0035]Add 1 gram of GO, 5 grams of 1,3,5-triazine and 20 grams of DMF into a beaker and stir evenly, then transfer to a reaction kettle with a Teflon liner, protect with nitrogen, heat to 80°C, and stir for 10 hours ; Add distilled water to filter after the reaction, and then vacuum filter and dry to obtain the product nitrogen-doped GO with a yield of 92.6%;

[0036] Add 1 gram of nitrogen-doped GO, 0.5 gram of dimethyl chlorophosphate and 20 grams of ethyl acetate into a three-necked flask with a magnetic stirring device, stir and react at 10°C for 6 hours, filter after the reaction, and use methanol After washing for several times, and then vacuum drying at 60°C for 12 hours, the product organophosphorus-grafted nitrogen-doped GO was obtained with a yield of 90.7%;

[0037] Add 1 g of PN-GO powder, 3 g of Ni(NO3)3·6H2O and 2 g of La(NO3)3·6H2O to 150 g of methanol, and ultrasonically disperse at room temperature for 1 hour to obtain a suspension. Add 6 grams of 2-methylimi...

Embodiment 2

[0039] 1 gram of GO, 1 gram of 1,3,5-triazine and 10 grams of DMF were added into a beaker and stirred evenly, then transferred to a reaction kettle with a Teflon liner, protected by nitrogen, heated to 150°C, and stirred for 2 hours ; Add distilled water to filter after the reaction, and then vacuum filter and dry to obtain the product nitrogen-doped GO with a yield of 78.7%;

[0040] Add 1 gram of nitrogen-doped GO, 0.1 gram of dimethyl chlorophosphate and 10 grams of acetonitrile into a three-necked flask with a magnetic stirring device, stir and react at 80°C for 2 hours, filter after the reaction, and wash with methanol times, and then vacuum-dried at 60°C for 12 hours to obtain the product organophosphorus-grafted nitrogen-doped GO with a yield of 84.3%;

[0041] Add 1 g of PN-GO powder, 10 g of Ni(NO3)3·6H2O and 5 g of La(NO3)3·6H2O to 2000 g of methanol, and ultrasonically disperse at room temperature for 1 hour to obtain a suspension, in the above suspension Add 50 g...

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Abstract

The invention discloses a method for preparing flame-retardant modified graphene and its modified thermoplastic elastomer in the technical field of preparation of flame-retardant materials. The method for preparing flame-retardant modified graphene includes the following steps: graphene oxide nitrogen doping reaction: Graphene oxide, 1,3,5-triazine and dimethylformamide are mixed according to a certain mass ratio, and the above mixture is transferred to a reaction kettle with a polytetrafluoroethylene lining, protected by nitrogen, and heated to 80°C-150°C ℃, stirred and reacted for 2-10 hours, added distilled water to filter after the reaction, and then vacuum filtered and dried to obtain the product nitrogen-doped graphene oxide. The present invention improves the expansion and flame-retardant efficiency of phosphorus-nitrogen flame-retardant modified graphene, and helps It is used to improve the mechanical properties, electrical conductivity and flame retardancy of the matrix material, solve the dispersion problem of graphene in the processing process, and give full play to its nano-enhanced effect.

Description

technical field [0001] The invention relates to the technical field of preparation of flame-retardant materials, in particular to a preparation method of flame-retardant modified graphene and a modified thermoplastic elastomer thereof. Background technique [0002] Flame-retardant materials are materials that can inhibit or delay combustion but are not easy to burn. They are widely used in clothing, petroleum, chemical industry, metallurgy, shipbuilding, fire protection, national defense and other fields. [0003] Graphene has excellent properties such as high conductivity, high modulus, high strength, and large specific surface area, and is easy to form a good conductive network in the polymer matrix. It has been widely used in the preparation of various modified polymer materials. In recent years, studies in the field of flame retardant have found that graphene has excellent flame retardant effect on many polymers. Although it has the advantages of high flame retardant eff...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08K9/12C08K9/04C08K3/04C08L23/16C08L23/12C08K13/06
CPCC08L23/16C08L2207/04C08L2201/02C08L2201/22C08K2201/001C08L23/12C08K13/06C08K9/12C08K9/04C08K3/042
Inventor 黄国波郭海昌王天乐闫瑞强张斌孙志茵
Owner TAIZHOU UNIV
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