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Preparation method and application of modified graphene nano filling material

A nano-filling, graphene technology, applied in fibrous fillers, chemical instruments and methods, inorganic pigment processing and other directions, can solve the problems of poor graphene conductivity, difficult to meet application requirements, reduce graphene application value, etc. The effect of burning and improving compatibility

Inactive Publication Date: 2015-07-29
苏州安鸿泰新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the fact that a large number of defects have been formed on the graphene sheet during oxidation, and due to the steric hindrance of the graft compound, it is difficult to remove the large The bond is restored, resulting in poor conductivity of graphene, which is difficult to meet application requirements and reduces the application value of graphene

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  • Preparation method and application of modified graphene nano filling material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The modified graphene nano-fill material of the present embodiment is prepared as follows:

[0026] (1) Preparation of graphite oxide: take 2g graphite powder, 1g NaNO 3 , 46ml concentrated H 2 SO 4 Place in a flask and stir in an ice bath; add 6g KMnO to the above system 4 , continue to stir for 30 minutes; then raise the temperature to 35°C, and after stirring for 1 hour, add 92ml of distilled water dropwise to the reaction system; then raise the reaction temperature to 98°C, continue to stir for 15 minutes, and then use warm water to dissolve the reaction solution To dilute, add 5ml H to the reaction solution 2 O 2 and stirred, the obtained product was filtered by suction, washed with water until neutral, and dried in a vacuum oven at 60°C to obtain graphite oxide; the conductivity of the obtained graphite oxide was tested to be 1.34×10 -8 S / m.

[0027] (2) Preparation of reduced graphene: Take 1g of graphite oxide prepared in s...

Embodiment 2

[0033] The modified graphene nano-fill material of the present embodiment is prepared as follows:

[0034] (1) The preparation method of graphite oxide is the same as in Example 1;

[0035] (2) the preparation method of reduced graphene is identical with embodiment 1;

[0036] (3) Preparation of modified graphene: Take 0.5g of the reduced graphene prepared in step (2) and ultrasonically disperse it in 80ml of anhydrous NMP (N-methylpyrrolidone), take 8g of 4,4'-dicyclohexyl Dissolve methane diisocyanate in NMP, under the protection of nitrogen, add 4,4'-dicyclohexylmethane diisocyanate solution dropwise to the reduced graphene dispersion, react at 70°C for 5 hours, and the obtained product is centrifuged , NMP was washed several times, and then dispersed in anhydrous NMP; 7.6g DOPO was dissolved in NMP, and under nitrogen protection, the DOPO solution was added dropwise to the above-mentioned graphene dispersion grafted with isocyanate groups, and then Add 0.3g of tr...

Embodiment 3

[0040] The modified graphene nano-fill material of the present embodiment is prepared as follows:

[0041] (1) The preparation method of graphite oxide is the same as in Example 1;

[0042] (2) the preparation method of reduced graphene is identical with embodiment 1;

[0043] (3) Preparation of modified graphene: take 0.5g of the reduced graphene prepared in step (2) and ultrasonically disperse it in 80ml of anhydrous DMF, take 9g of 4,4'-diphenylmethane diisocyanate and dissolve it in DMF , under the protection of nitrogen, 4,4'-diphenylmethane diisocyanate solution was added dropwise to the reduced graphene dispersion, and reacted at 70°C for 5 hours. The obtained product was centrifuged, washed with DMF several times, and then Disperse in anhydrous DMF; get 6.5g dimethyl phosphite and dissolve in DMF, under the protection of nitrogen, add the dimethyl phosphite solution dropwise in the above-mentioned graphene dispersion liquid grafted with isocyanate groups, Add...

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Abstract

The invention relates to a preparation method of a modified graphene nano filling material and an application of the modified graphene nano filling material in a nylon 6 material. According to the preparation method, through selection of a reducer and a modifier, optimization of process conditions and the like, graphite oxide is partially reduced, electrical conductivity of the graphite oxide is recovered, and then, residual oxygen-containing groups on the surface of a graphene sheet layer are modified, grafted and endowed with special performance. By comparison with a method adopting first grafting and second reduction in the prior art, compatibility of graphene and polymers can be improved while the graphene conductivity is not damaged, and the modified graphene nano filling material has certain inflaming retarding synergy. When the modified graphene nano filling material is applied to nylon 6, the thermal stability of the nylon 6 material can be improved to a certain extent, the conductivity of a graphene / nylon 6 nanocomposite material is improved by about 4 orders of magnitudes by comparison with that of graphite oxide. Therefore, compared with an existing graphene filling material, the modified graphene nano filling material can improve the conductivity of a polymer substrate, and the anti-static function of the polymer material is improved.

Description

Technical field [0001] The present invention is the field of graphene material technology, which involves a method of preparation method with conductive and flame -retardant modified graphene nano -filling materials, and its application in nylon 6 materials. Background technique [0002] Graphene is SP 2 The two -dimensional layered structure formed by the hybolized carbon atom has very good thermal conductivity and sheet layer barrier effects. Add graphene as a nano -filled material to the polymer matrix.Passing the heat faster outside the system; at the same time, the graphene has a large ratio area. When the material is burned, it can also block the release and diffusion of volatile gas gas to a certain extent.Therefore, graphene can usually be applied to the flame retardant system to play a certain effect of combustible flame retardant.In addition, the unique coexistence structure of graphene can provide a path for electronic transmission. When graphene is filled in a polym...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/46C09C3/06C09C3/08C08K9/04C08K3/04C08L77/02
Inventor 程园朱长江台启龙
Owner 苏州安鸿泰新材料有限公司
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