Preparation method of functionalized graphene oxide containing phosphorus and silicon

A graphene and functionalization technology, applied in the field of preparation of phosphorus-containing silicon-functionalized graphene oxide, can solve the problems of reduced total heat release, increased initial thermal degradation temperature, unsuitable for industrial applications, etc., and achieves improved thermal stability. properties, mild reaction conditions, and the effect of improving dispersibility

Active Publication Date: 2018-08-24
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Wang et al. directly used OapPOSS to form covalent bonds with graphene oxide and applied it to epoxy resin. The results showed that when the addition of OapPOSS-rGO was 2wt%, the initial thermal degradation temperature of epoxy resin composites increased significantly. The total heat release is also 58% lower than that of pure epoxy, but OapPOSS is expensive and not suitable for industrial applications.

Method used

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  • Preparation method of functionalized graphene oxide containing phosphorus and silicon
  • Preparation method of functionalized graphene oxide containing phosphorus and silicon
  • Preparation method of functionalized graphene oxide containing phosphorus and silicon

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Synthesis of phosphorus-containing silicon element compounds In a 50mL reaction vessel, add 2.27g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 1.11g of γ-aminopropyl tris Ethoxysilane and 0.32 g of paraformaldehyde were dissolved in 30 mL of chloroform, and stirred and reacted at a reaction temperature of 60° C. for 24 h under nitrogen protection. After the reaction, the reaction solution was precipitated and purified in n-hexane to obtain the following figure 1 The phosphorus-containing silicon element compound shown.

[0027] (2) Synthesis of phosphorus-containing silicon functionalized graphene oxide

[0028] Dissolve 20 mg of graphene oxide in a mixed solution of 10 mL of deionized water and 40 mL of absolute ethanol. After ultrasonication for 60 min, add 0.34 g of phosphorus-containing silicon element compound diluted with 10 mL of toluene drop by drop, and react with stirring at 78°C for 24 h. After the reaction is finished, the product is washed w...

Embodiment 2

[0030] (1) Synthesis of phosphorus-containing silicon compound

[0031] In a 50 mL reaction vessel, add 2.27 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 1.11 g of γ-aminopropyltriethoxysilane, and 0.56 g of paraformaldehyde Dissolve in 30mL of carbon tetrachloride, and stir for 24h at a reaction temperature of 60°C under nitrogen protection. After the reaction, the reaction liquid was precipitated and purified in n-hexane.

[0032] (2) Synthesis of phosphorus-containing silicon functionalized graphene oxide

[0033] Dissolve 50mg of graphene oxide in 10mL of deionized water and 40mL of N,N-dimethylformamide mixed solution, after ultrasonication for 60min, add 0.25g of phosphorus-containing silicon element compound diluted with 10mL of toluene drop by drop, at 78°C , Stir the reaction for 24h. After the reaction, the product was washed with absolute ethanol and deionized water several times, and then purified by centrifugation and lyophilization to obtain the fo...

Embodiment 3

[0035] (1) Synthesis of phosphorus-containing silicon compound

[0036] In a 50 mL reaction vessel, add 3.14 g of 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide, 1.52 g of γ-aminopropyltriethoxysilane, and 0.65 g of paraformaldehyde Dissolve it in 30 mL of chloroform, and stir for 24 h at a reaction temperature of 60° C. under nitrogen protection. After the reaction, the reaction liquid was precipitated and purified in n-hexane.

[0037] (2) Synthesis of phosphorus-containing silicon functionalized graphene oxide

[0038] Dissolve 80 mg of graphene oxide in a mixed solution of 10 mL of deionized water and 80 mL of absolute ethanol. After ultrasonication for 60 min, 0.25 g of phosphorus-containing silicon element compound diluted with 10 mL of toluene is added dropwise, and the reaction is stirred at 80°C for 24 h. After the reaction is finished, the product is washed with absolute ethanol and deionized water several times, and then purified by centrifugation and freeze-d...

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Abstract

The invention discloses a preparation method of functionalized graphene oxide containing phosphorus and silicon. According to the method disclosed by the invention, two N-H bonds on gamma-aminopropyltriethoxysilane are simultaneously connected with DOPO by utilizing a simple and convenient experiment method to synthesize a compound containing phosphorus and silicon elements in one step. Accordingto the preparation method disclosed by the invention, graphene is modified through utilizing the compound containing the phosphorus and silicon elements, so that the dispersity of the graphene in an organic solvent and the compatibility of the graphene in epoxy resin are hopefully improved. According to the preparation method, the phosphorus and silicon flame-retarding elements are introduced intothe graphene oxide to synthesize a small-molecular flame retardant and formation of a coke layer is facilitated through a cooperative effect of the phosphorus and silicon flame-retarding elements andthe graphene oxide; the thermal stability of the epoxy resin is hopefully improved. The preparation method has moderate reaction conditions and the functionalized graphene oxide does not contain halogen elements and is an environment-friendly type novel flame retardant.

Description

technical field [0001] The invention belongs to the technical field of graphene modification, and specifically relates to a preparation method of phosphorus-containing silicon functionalized graphene oxide. Background technique [0002] Because of its unique two-dimensional sheet structure, high thermal stability, Young's modulus of up to 1000GPa and breaking strength of 125GPa, graphene has good flame retardant and toughening effects. Therefore, it is widely used in the field of fire retardant materials Attractive application prospects. However, the interaction between graphene sheets is strong, and the dispersion in organic solvents is poor, which makes it easy to agglomerate when preparing polymer nanocomposites, and the compatibility with epoxy resin is naturally not high. Therefore, it is necessary to modify graphene, which can not only effectively inhibit the interlayer agglomeration, but also exert a certain synergistic flame retardant effect. [0003] Phosphorus-co...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K9/06C08K3/04C08L63/00
CPCC08K3/04C08K9/06C08L63/00
Inventor 戴李宗吴雯倩许一婷王秀陈国荣袁丛辉曾碧榕罗伟昂王瑞攀何凯斌
Owner XIAMEN UNIV
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