A kind of graphene-based antioxidant and its preparation method and application

Abstract

The invention relates to the field of polymer composite materials, in particular to a graphene-based antioxidant and its preparation method and application. The invention provides a preparation method of a graphene-based antioxidant. The preparation method is as follows: firstly, graphene oxide is subjected to the action of a solvent and a carboxyl activator to obtain carboxyl-activated graphene oxide, and then the antioxidant is grafted to the obtained carboxyl-activated graphene oxide, and finally filtered, washed and dried to obtain a graphene-based antioxidant. The polyolefin-based composite material obtained by adding the graphene-based antioxidant obtained in the present invention to the polyolefin matrix has the characteristics of long oxidation induction period, high initial degradation temperature and resistance to solvent extraction.

Description

technical field

[0001] The invention relates to the field of polymer composite materials, in particular to a graphene-based antioxidant and its preparation method and application. Background technique

[0002] Polyolefin materials are often affected by light, oxygen, and heat during processing and use, causing aging and degradation, which affects the use effect and service life. Therefore, stabilizing additives are often added in the processing and production of polyolefin materials to delay its aging and increase its thermal oxygen and light oxygen stability. Stabilizing additives are mainly divided into three categories: light stabilizers, heat stabilizers and antioxidants. Among them, the most effective and widely used method in industry is to add antioxidants to polyolefin materials. Among them, the primary antioxidant can terminate the transmission and growth of free radical chains in the oxidation process, and the secondary antioxidant can delay the generation of free...

Examples

Embodiment 1

[0059] Prepare graphene-based antioxidant, the specific preparation process is as follows figure 1 shown, prepared by the following steps:

[0060] A, preparation of graphite oxide: prepare graphite oxide according to the method reported in the document "DC, M., et al., Acs Nano, 2010.4 (8): p.4806";

[0061] B. Activation of carboxyl groups: disperse graphite oxide ultrasonically (probe ultrasonic in ice-water bath) in N,N-dimethylformamide, then add thionyl chloride for reaction to obtain graphene oxide with activated carboxyl groups; ultrasonic The dispersion power is 500W; the ultrasonic dispersion time is 30min; the solid-liquid ratio of graphite oxide to N,N-dimethylformamide is 0.65:1 (mg / ml); the solid-liquid ratio of graphene oxide to thionyl chloride ( g / ml) was 1:100; the reaction was specifically stirred at 70°C for 24h under an argon atmosphere;

[0062] C, remove excess reactant: adopt underpressure distillation to remove remaining thionyl chloride in the react...

Embodiment 2

[0072] Prepare graphene-based antioxidant, the specific preparation process is as follows figure 1 shown, prepared by the following steps:

[0073] A, preparation of graphite oxide: prepare graphite oxide according to the method reported in the document "DC, M., et al., Acs Nano, 2010.4 (8): p.4806";

[0074] B. Activation of carboxyl groups: disperse graphite oxide ultrasonically (probe ultrasonic in ice-water bath) in toluene, then add thionyl chloride to react to obtain graphene oxide with activated carboxyl groups; ultrasonic dispersion power is 600W; ultrasonic dispersion time For 20min; the solid-to-liquid ratio of graphite oxide and toluene is 0.38:1 (mg / ml); the solid-to-liquid ratio (g / ml) of graphene oxide and thionyl chloride is 1:100; Described reaction is specifically adopted in nitrogen gas Stir at 70°C for 24h under atmosphere;

[0075] C, remove excess reactant: adopt underpressure distillation to remove remaining thionyl chloride in the reaction;

[0076]D,...

Embodiment 3

[0085] Prepare graphene-based antioxidant, the specific preparation process is as follows figure 1 shown, prepared by the following steps:

[0086] A, preparation of graphite oxide: prepare graphite oxide according to the method reported in the document "DC, M., et al., Acs Nano, 2010.4 (8): p.4806";

[0087] B. Activation of carboxyl groups: disperse graphite oxide ultrasonically (probe ultrasonic in ice-water bath) in N,N-dimethylformamide, then add thionyl chloride for reaction to obtain graphene oxide with activated carboxyl groups; ultrasonic The dispersion power is 500W; the ultrasonic dispersion time is 30min; the solid-liquid ratio of graphite oxide to N,N-dimethylformamide is 0.5:1 (mg / ml); the solid-liquid ratio of graphene oxide to thionyl chloride ( g / ml) was 1:100; the reaction was specifically stirred at 70°C for 24h under an argon atmosphere;

[0088] C, remove excess reactant: adopt underpressure distillation to remove remaining thionyl chloride in the reacti...

technical field

[0001] The invention relates to the field of polymer composite materials, in particular to a graphene-based antioxidant and its preparation method and application. Background technique

[0002] Polyolefin materials are often affected by light, oxygen, and heat during processing and use, causing aging and degradation, which affects the use effect and service life. Therefore, stabilizing additives are often added in the processing and production of polyolefin materials to delay its aging and increase its thermal oxygen and light oxygen stability. Stabilizing additives are mainly divided into three categories: light stabilizers, heat stabilizers and antioxidants. Among them, the most effective and widely used method in industry is to add antioxidants to polyolefin materials. Among them, the primary antioxidant can terminate the transmission and growth of free radical chains in the oxidation process, and the secondary antioxidant can delay the generation of free...

Examples

Embodiment 1

[0059] Prepare graphene-based antioxidant, the specific preparation process is as follows figure 1 shown, prepared by the following steps:

[0060] A, preparation of graphite oxide: prepare graphite oxide according to the method reported in the document "DC, M., et al., Acs Nano, 2010.4 (8): p.4806";

[0061] B. Activation of carboxyl groups: disperse graphite oxide ultrasonically (probe ultrasonic in ice-water bath) in N,N-dimethylformamide, then add thionyl chloride for reaction to obtain graphene oxide with activated carboxyl groups; ultrasonic The dispersion power is 500W; the ultrasonic dispersion time is 30min; the solid-liquid ratio of graphite oxide to N,N-dimethylformamide is 0.65:1 (mg / ml); the solid-liquid ratio of graphene oxide to thionyl chloride ( g / ml) was 1:100; the reaction was specifically stirred at 70°C for 24h under an argon atmosphere;

[0062] C, remove excess reactant: adopt underpressure distillation to remove remaining thionyl chloride in the react...

Embodiment 2

[0072] Prepare graphene-based antioxidant, the specific preparation process is as follows figure 1 shown, prepared by the following steps:

[0073] A, preparation of graphite oxide: prepare graphite oxide according to the method reported in the document "DC, M., et al., Acs Nano, 2010.4 (8): p.4806";

[0074] B. Activation of carboxyl groups: disperse graphite oxide ultrasonically (probe ultrasonic in ice-water bath) in toluene, then add thionyl chloride to react to obtain graphene oxide with activated carboxyl groups; ultrasonic dispersion power is 600W; ultrasonic dispersion time For 20min; the solid-to-liquid ratio of graphite oxide and toluene is 0.38:1 (mg / ml); the solid-to-liquid ratio (g / ml) of graphene oxide and thionyl chloride is 1:100; Described reaction is specifically adopted in nitrogen gas Stir at 70°C for 24h under atmosphere;

[0075] C, remove excess reactant: adopt underpressure distillation to remove remaining thionyl chloride in the reaction;

[0076]D,...

Embodiment 3

[0085] Prepare graphene-based antioxidant, the specific preparation process is as follows figure 1 shown, prepared by the following steps:

[0086] A, preparation of graphite oxide: prepare graphite oxide according to the method reported in the document "DC, M., et al., Acs Nano, 2010.4 (8): p.4806";

[0087] B. Activation of carboxyl groups: disperse graphite oxide ultrasonically (probe ultrasonic in ice-water bath) in N,N-dimethylformamide, then add thionyl chloride for reaction to obtain graphene oxide with activated carboxyl groups; ultrasonic The dispersion power is 500W; the ultrasonic dispersion time is 30min; the solid-liquid ratio of graphite oxide to N,N-dimethylformamide is 0.5:1 (mg / ml); the solid-liquid ratio of graphene oxide to thionyl chloride ( g / ml) was 1:100; the reaction was specifically stirred at 70°C for 24h under an argon atmosphere;

[0088] C, remove excess reactant: adopt underpressure distillation to remove remaining thionyl chloride in the reacti...

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