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Non-mobility graphene oxide grafted anti-aging agent and preparation method thereof

An oxide stone, non-migration technology, applied in the field of rubber anti-aging, can solve problems such as affecting the performance of rubber products, reducing the anti-aging efficiency of antioxidants, endangering health and other problems, achieving good thermal oxidation resistance and anti-extraction performance. , the effect of high specific surface area

Inactive Publication Date: 2018-09-07
SICHUAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The existence of carbon-carbon double bonds in the structural unit of diene rubber makes it easy to age in the presence of thermal oxygen, light and ozone, causing the parameters of rubber materials and components to deviate from the initial design values, resulting in safety hazards or loss of performance
[0004] Traditional small molecule amine anti-aging agents are easy to migrate, volatilize and extract from the inside of rubber products, and the migration speed will be significantly accelerated with the increase of temperature, aging time and air flow. This phenomenon is greatly reduced. The anti-aging efficiency of the anti-aging agent is not conducive to the long-term protection of rubber products from aging
At the same time, the anti-aging agent migrated from rubber products not only pollutes the environment, but also endangers human health.
When the amount of anti-aging agent is too large, the anti-aging agent will also "frost" on the rubber product, thus affecting the performance of the rubber product

Method used

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  • Non-mobility graphene oxide grafted anti-aging agent and preparation method thereof
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  • Non-mobility graphene oxide grafted anti-aging agent and preparation method thereof

Examples

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Embodiment 1

[0026] In this example, the schematic diagram of the synthesis of non-migrating graphene oxide grafted antioxidant is shown in figure 1 The preparation method of the non-migrating graphene oxide graft antioxidant is as follows:

[0027] (1) Dissolve graphene oxide (GO) in thionyl chloride, sonicate it for 1h, and then reflux for 2h at 85°C, then spin steam, wash and filter to remove thionyl chloride to obtain thionyl chloride modified Graphene oxide.

[0028] (2) Add 0.2g of thionyl chloride modified graphene oxide to 200mL of dimethylformamide (DMF), and ultrasonically dissolve thionyl chloride modified graphene oxide to obtain thionyl chloride modified Graphene oxide solution. Dissolve 4 g of 4-aminodiphenylamine (anti-aging agent intermediate RT Peis, RT for short) in DMF to form an RT solution. The amount of DMF should be such that RT can just dissolve. Mix the aforementioned two solutions, control the mass ratio of thionyl chloride modified graphene oxide to RT in the mixed ...

Embodiment 2

[0033] In this embodiment, the preparation method of the non-migrating graphene oxide grafted antioxidant is as follows:

[0034] (1) Dissolve GO in thionyl chloride, sonicate for 1.5h, and then reflux for 1h at 85°C, then spin steam, wash and filter to remove thionyl chloride to obtain thionyl chloride modified graphene oxide.

[0035] (2) Add 0.1 g of thionyl chloride-modified graphene oxide to 200 mL of DMF, and ultrasonically dissolve the thionyl chloride-modified graphene oxide to obtain a thionyl chloride-modified graphene oxide solution. Dissolve 3g of RT in DMF to form an RT solution. The amount of DMF should be such that RT just dissolves. Mix the aforementioned two solutions, control the mass ratio of thionyl chloride modified graphene oxide to RT in the mixed solution to be 1:30, reflux for 60 hours, and filter the reaction solution obtained by the reflux reaction to remove Part of the solvent DMF and RT that has not completed the grafting reaction, the solid product ob...

Embodiment 3

[0037] In this embodiment, the preparation method of the non-migrating graphene oxide grafted antioxidant is as follows:

[0038] (1) Dissolve GO in thionyl chloride, sonicate for 2h, and then reflux for 3h at 85°C, then spin steam, wash and filter to remove thionyl chloride to obtain thionyl chloride modified graphene oxide.

[0039] (2) Add 0.16 g of thionyl chloride-modified graphene oxide to 200 mL of DMF, and ultrasonically dissolve the thionyl chloride-modified graphene oxide to obtain a thionyl chloride-modified graphene oxide solution. Dissolve 2.4 g of RT in DMF to form an RT solution. The amount of DMF should be such that RT just dissolves. Mix the aforementioned two solutions, control the mass ratio of thionyl chloride modified graphene oxide to RT in the mixed solution to be 1:15, reflux for 50 hours, and filter the reaction solution obtained by the reflux reaction to remove Part of the solvent DMF and RT that did not complete the grafting reaction, the solid product o...

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Abstract

The invention provides a non-mobility graphene oxide grafted anti-aging agent and preparation method thereof. 4-aminodiphenylamine is used for carrying out grafting modification on graphene oxide by so as to enable a hydroxyl group in the carboxyl group of graphene oxide to be replaced with an R group, wherein the structural formula of the R group is described in the description; the grafting rateof the R group is 7-15wt%. The preparation method comprises the following steps: (1) dissolving graphene oxide into thionyl chloride, carrying out a refluxing reaction, separating out a reaction product, and washing to remove thionyl chloride so as to obtain thionyl chloride modified graphene oxide; (2) adding the thionyl chloride modified graphene oxide into dimethylformamide, carrying out ultrasonic treatment to enable the thionyl chloride modified graphene oxide to be fully dissolved, and dissolving 4-aminodiphenylamine into dimethylformamide; then, mixing the thionyl chloride modified graphene oxide solution with the 4-aminodiphenylamine solution, carrying out a refluxing reaction and solid-liquid separation, and fully soaking the obtained solid phase in absolute ethanol, separating out the soaked solid product, and drying to obtain the non-mobility graphene oxide grafted anti-aging agent.

Description

Technical field [0001] The invention belongs to the technical field of rubber anti-aging, and relates to a graphene oxide grafted anti-aging agent and a preparation method thereof. Background technique [0002] The existence of carbon-carbon double bonds in the structural unit of diene rubber makes it prone to aging in the presence of hot oxygen, light and ozone, which causes the parameters of rubber materials and components to deviate from the initial design values, causing safety hazards or loss of performance . Therefore, it is of great significance to study rubber aging protection methods. Rubber aging is an irreversible chemical reaction process, which cannot be absolutely prevented. The only way to slow down its aging speed is to extend the service life of rubber products, or to maintain relatively more stable and superior performance during the use of rubber products. [0003] At present, the most convenient and widely used anti-aging method is to add substances that can i...

Claims

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Application Information

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IPC IPC(8): C08K9/04C08K9/02C08K3/04C08L7/00
Inventor 黄光速郑静周军军魏来蕴魏海涛朱勇
Owner SICHUAN UNIV
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